Relazione-ScientificaAprile2013
Transcript
Relazione-ScientificaAprile2013
Scuola di dottorato di ricerca in Nanotecnologie Resoconto dell’attività 2012 Sommario 1. Relazione scientifica riassuntiva .................................................................................................. 3 2. Elenco dottorandi, supervisori e titolo delle tesi .......................................................................... 6 3. Matrice delal attività di Ricerca della scuola di nanotecnologie ............................................... 11 4. Schede attività dottorandi........................................................................................................... 14 Dottorandi del 24 e 25 ciclo: • ............................................................................................................ 15 Dottorandi del 26 ciclo:....................................................................................................................... 52 Dottorandi del 27 ciclo ........................................................................................................................ 87 Progetti Dottorandi del 28 ciclo: ......................................................................................................... 88 5. Elenco dei componenti del collegio docenti ............................................................................ 164 6. Produzione scientifica del collegio docenti 2007-2012 ........................................................... 167 Personale di ruolo nelle università italiane e INAF .......................................................................... 167 Personale non di ruolo nelle università o dipendenti di altri enti...................................................... 197 7. Criteri di valuatazione delle scuole di dottorato ...................................................................... 204 8. Giudizi dei referee esterni per dottorandi ammessi all’esame finale aprile 2013 .................... 207 9. Presentazioni dei dottorandi al congesso del gennaio 2013 ..................................................... 209 Attività della scuola: situazione ad aprile 2013. Questo documento contiene il dettaglio dell’attività didattico scientifica della scuola di dottorato in nanotecnologie svolto durante l’anno 2011 fino ad aprile del 2012. Il documento si compone delle seguenti parti: 1. Relazione scientifica riassuntiva (Executive summary) 2. Elenco dei dottorandi, supervisori e titolo tesi in corso. 3. Schede di attività dei dottorandi che hanno svolto attività continuativa nell’anno 2011. Questa attività è stata presentata nel congresso di gennaio 2012 (vedi slides su CD allegato) ed è riassunto per ogni dottorando nelle schede riportate di seguito. Le schede si riferiscono ai dottorandi in corso dei cicli 24, 25 e 26, non esssendoci dottorandi in proroga da cicli precedenti. 4. Progetti dei dottorandi nuovi entrati nella scuola (27 ciclo). Questa attività non è stata presentata in gennaio 2012 poiché non ancora definiti gli accoppiamenti dottorando – tema di ricerca. 5. Riassuntivo delle pubblicazioni dei dottorandi. 6. Giudizi della commissione d’esame finale 2012. 7. Elenco dei componenti collegio docenti. 8. Pubblicazioni rappresentative del collegio docenti. 9. Criteri di valutazione delle scuole di dottorato. 10. Valutazione della scuola da parte del nucleo di valutazione riassunta in una tabella e rimandi ad allegati. 11. Giudizi dei reviewer esterni per i dottorandi ammessi all’esame finale (allegati). 12. Presentazioni dei dottorandi al congresso gennaio 2012 (allegati). 1. Relazione scientifica riassuntiva La missione della scuola di dottorato è di migliorare le conoscenze ed educare studenti nel campo delle nanotecnologie al fine di formare scienziati e tecnici per il 21° secolo. La caratteristica della Scuola è l’interdisciplinarità: sugli argomenti di ricerca attivi lavorano in sinergia fisici, chimici, biologi, ingegneri, medici, farmacologi, odontoiatri, biotecnologi e laureati in Agraria, mantenendo e rafforzando la specificità della cultura di provenienza ed acquisendo la capacità di sviluppare la propria ricerca in un quadro più ampio. L’obiettivo principale della Scuola è di formare Ricercatori che sappiano progettare, costruire, utilizzare e sottoporre a prove di funzionalità strumenti e dispositivi nano tecnologici, in grado di rispondere alle crescenti e diversificate esigenze delle applicazioni. L'allievo “dottorato” di questa Scuola sarà un professionista della ricerca e dello sviluppo tecnologico che sappia applicare le proprie conoscenze, con capacità di valutazione critica, allo sviluppo di metodi di progettazione, produzione e valutazione di nuovi materiali e al miglioramento di quelli esistenti. Questo anche mirato ad una produzione industriale più efficace, economica e sostenibile dal punto di vista delle risorse e dell'ambiente. La scuola è stata fondata nel 2006 a partire da un dottorato in nanotecnologie. Gli obiettivi delle ricerche sono i seguenti: •Sviluppo di nuove tecniche sperimentali per lo studio, la lavorazione, la manipolazione e la visualizzazione su scala nanometrica di materiali nanostrutturati. •Sviluppo di tecniche spettroscopiche di rivelazione di singola molecola su substrati nanostrutturati. •Studio delle relazioni tra la microstruttura e le proprietà dei materiali e ingegnerizzazione di materiali nanostrutturati. •Sintesi di nanostrutture. •Applicazioni delle nanotecniche e nanostrutture a ricerche di interesse biomedico ed energetico. •Modellizzazione molecolare multiscala di materiali e di fenomeni di interesse attraverso tecniche di simulazione computazionale. •Salute umana con particolare attenzione allo studio ed al trattamento di tumori e malattie degenerative. •Applicazione delle nanotecnologie nei settori medico, farmacologico, biomedico ed agroalimentare. Questi obiettivi sono perseguiti avvalendosi delle attrezzature d'avanguardia disponibili nei laboratori dell'Università di Trieste e degli Enti di ricerca pubblici e privati convenzionati con l’Università di Trieste, come da seguente tabella: n. 1. 2. 3. 4. 5. 6. 7. 8. Tipologia del soggetto Istituto/Ente di Ricerca non (compreso IRCCS) Istituto/Ente di Ricerca non (compreso IRCCS) Istituto/Ente di Ricerca non (compreso IRCCS) Istituto/Ente di Ricerca non (compreso IRCCS) Istituto/Ente di Ricerca non (compreso IRCCS) Istituto/Ente di Ricerca non (compreso IRCCS) Privato non di ricerca Istituto/Ente di Ricerca non (compreso IRCCS) accademici Pubblico/Privato PUBBLICO Denominazione del soggetto Sincrotrone Trieste S.C.p.A. accademici PUBBLICO Laboratorio Nazionale TASC-IOM CNR accademici PUBBLICO accademici PUBBLICO CNR - Institute of Chemistry of OrganoMetallic Compounds IRCSS Burlo Garofolo - Trieste accademici PUBBLICO CRO Aviano accademici PUBBLICO accademici PRIVATO PUBBLICO Istituto Nazionale dei tumori di Milano Fondazione IRCSS Indistrie Bracco Fondazione Callerio - Trieste Gli studenti di dottorato nel periodo in esame hanno svolto stage presso aziende ed enti di ricerca. I più significativi sono i segnueti: STAGE IN ITALIA n. 1. 2. 3. 4. 5. 6. Pubblico/Privato PUBBLICO PUBBLICO PUBBLICO PUBBLICO MISTO PUBBLICO Denominazione del soggetto CNR-IOM TASC Laboratorio Trieste Elettra Sincrotrone Trieste IRCCS Burlo Garofalo CRO Aviano Centro Biomedicina Molecolare (CBM) Università di Udine STAGE ALL'ESTERO n. 1. 2. 3. 4. 5. 6. 7. 8. 9. Denominazione del soggetto Max Plank Institute - Halle CNRS - Marsiglia University Poznan - Center for nanotechnology Ohio University, Athens (OH) Technische Universität di Monaco di Baviera Soft Matter Physics Division - Leipzig Università di San Pietroburgo Technische Universitaet - Institut fuer Chemie Max-Volmer-Laboratorium für Biophysikalische Chemie Università della Svizzera Italiana Paese Germania Francia Polonia Stati Uniti d'America Germania Germania Russai Germania Svizzera Di seguito alcuni numeri rappresentativi dell’attività della scuola: • Numero di studenti (ad aprile 2013): 70 • Numero di diplomati nel 2013: 10 • Numero di diplomati nel 2012: 12 • Numero di diplomati nel 2011: 8 • Numero di diplomati nel 2010: 7 • Numero di diplomati nel 2009: 6 • Numero di diplomati nel 2008: 9 • Numero di diplomati nel 2007: 14 • Membri del collegio docenti: 44 • Enti di ricerca coinvolti nel dottorato: oDipartimenti dell’Università di Trieste: 5 (in diminuzione per accorpamenti) oEnti di ricerca esterni: 10 oAltre Università: 4 • Numero di pubblicazioni degli studenti: oAnno 2007: 67 oAnno 2008: 68 oAnno 2009: 72 oAnno 2010: 105 oAnno 2011: 95 oAnno 2012: 98 • Numero di pubblicazioni di supervisori e tutors (2007-12): oltre 1000 • Risorse finanziarie (per anno): 700.000 euro • Ultima valutazione complessiva del nucleo dell’Università di Trieste: A+ (Ottimo) I criteri usati per la valutazione interna sono stati quelli suggeriti dal Ministero, accompagnati da criteri interni all’Ateneo. Questi criteri sono descritti di seguito in questo documento in modo dettagliato. I principali indicatori utilizzati dal nucleo che hanno permesso la valutazione in classe A+ sono (vedi capitolo 10 per maggiori dettagli): • produzione scientifica del Collegio Docenti; • congruo numero di docenti dell’Ateneo coinvolti nel collegio; • rapporto del dottorato con il mondo del lavoro; • attrattività del dottorato nelle precedenti edizioni; • livello di soddisfazione dei dottorandi; • produzione scientifica dei dottorandi ed iniziative esistenti di pubblicizzazione e referaggio delle tesi di dottorato; • adeguata formulazione delle tematiche scientifiche e degli obiettivi formativi, • riduzione della frammentazione dei corsi di dottorato; • accuratezza delle informazioni fornite per la valutazione; • presenza di iscritti stranieri; • sito web del dottorato. 2.Elenco dottorandi, supervisori e titolo delle tesi La situazione riportata in tabella è quella ad aprile 2013, quindi include i dottorandi del 28 ciclo e non quelli del 25 ciclo diplomati ad aprile. Dottorando Ciclo Supervisore ABDOLLAHZADEH Iman AMODIO Alessia 27 SCOLES Giacinto 28 TOFFOLI Giuseppe ANGELONI Valeria 27 BRESCHI Lorenzo BORIN Daniele 27 LAZZARINO Marco 28 PASCOLO Lorella CAMMISULI Francesca SSD NomeDip FIS/03 Department of Physics ‐ DF Department of Physics ‐ DF Nanotechnology approaches for the detection of circulating tumor cells BIO/14 Quantitative analysis of tumor suppressor and ancogene proteins in tumor micro‐sample MED/28 Clinical Department Role of collagen cross‐linkers on the of Medical Science, stability of bonded interface Surgery and Health ‐ DCSMCS FIS/03 Department of Micro mechanical oscillators for Physics ‐ DF biochemical applications BIO/14 Clinical Department Effetti dei nano materiali sulle of Medical Science, barriere biologiche fetali e post‐natali Surgery and Health ‐ e valutazioni della tossicità epigenica DCSMCS FIS/03 Department of Capacitance immunosensors for the Physics ‐ DF early detection of circulating cancer biomarkers CAPALDO Pietro 28 CASALIS Loredana CAPOLLA Sara 27 MACOR Paolo MED/04 Department of Life Science ‐ DLS CASSESE Damiano 26 LAZZARINO Marco CECCHINI Paolo 27 TOGNETTO Daniele COCEANO Giovanna CORAL Lucia 27 COJOC Dan CORVAGLIA Stefania DAGOSTINO Ilenia 28 TOFFOLI Giuseppe 26 CASALIS Loredana 28 GAMINI Amelia Titolo Tesi Use of chemotherapic‐loaded nanoparticles in the treatment of cancer FIS/03 Department of Design and realization of Physics ‐ DF nanoelectromechanical and plasmonic devices for Raman spectro‐ microscopy MED/30 Clinical Department Bio‐Materials in oculist micro surgery of Medical Science, Surgery and Health ‐ DCSMCS FIS/03 Department of Physics ‐ DF BIO/14 Department of Physics ‐ DF FIS/03 Department of Physics ‐ DF CHIM/04 Department of Life Science ‐ DLS Characterization of the mechanical properties of cancer cells Detection of tumor cell surface biomarkers in microsamples Nanoscale platform to study unstructured proteins interactions Valorizzazione di matrici alimentari della dieta mediterranea con l’arricchimento di nutrienti Dottorando Ciclo Supervisore SSD DAL COL Valentina 26 PRICL Sabrina ING‐ IND/24 DE BIASI Matteo 28 ANGERAME Daniele DEL BEN Fabio 28 SCOLES Giacinto DIOLOSA‘ Marina 27 CADENARO Milena ELISEI Elena FORNASARO Stefano NomeDip Department of Engineering and Architecture ‐ DIA MED/28 Clinical Department of Medical Science, Surgery and Health ‐ DCSMCS FIS/01 Department of Physics ‐ DF MED/28 Clinical Department of Medical Science, Surgery and Health ‐ DCSMCS 27 CESARO CHIM/04 Department of Life Attilio Science ‐ DLS 27 PASSAMONTI BIO/10 Department of Life Sabina Science ‐ DLS Titolo Tesi In silicio prediction of drug resistance: from cancer targeted therapy to cancer targeted prevention Materiali nano‐strutturati per l’odontoiatria Development of nanodevice to explore cell network in cancer Development of a new nano‐ engineered biopolymer‐based dental adhesive system Nanostructured biomolecular glasses Targeting natural antioxidant compounds to the brain: a metabolomic assessment. MED/28 Clinical Department Nanostructural analysis of the of Medical Science, adhesive interface in dentistry Surgery and Health ‐ DCSMCS FIS/03 Department of Development of quantum well Physics ‐ DF structures for multi band photon detection FIS/03 Department of Syntesis of ordered semiconductor Physics ‐ DF nanostructures by directed self‐ assembly for photonic applications MED/28 Clinical Department The influence of resin‐based dental of Medical Science, materials upon oral biofilms Surgery and Health ‐ development. DCSMCS FRASSETTO Andrea 26 CADENARO Milena GANBOLD Tamiraa 27 BIASIOL Giorgio HUSSAIN Sajid 26 BIASIOL Giorgio IONESCU Andrei Cristian 27 CADENARO Milena LOVAT Giacomo 27 MORGANTE Alberto MARSON Domenico 27 PRICL Sabrina ING‐ IND/24 MINIUSSI Elisa 26 BARALDI Alessandro FIS/03 MITRI Elisa 26 TORMEN Massimo FIS/03 FIS/03 Department of Physics ‐ DF Study of charge transfer processes at interfaces for photovoltaic applications Department of Engineering and Architecture ‐ DIA Department of Physics ‐ DF Computer‐assisted design of nanovectors for gene therapy Department of Physics ‐ DF Interaction of metal nanoclusters with graphene and low dimensional systems Fabrication of microfluidic devices for studying living cells, responding to external stimuli, by vibration spectroscopies Dottorando MOHAMMED Khalid Amna Ciclo Supervisore SSD 28 ONESTI Silvia FIS/03 NomeDip Department of Physics ‐ DF Titolo Tesi Atomic force microscopy investigation of the structural properties of DNA replication origins in tumor cells High sensitivity detection of DNA/miRNA targets in AFM nanografted arrays NKOUA NGAVOUKA Maryse Dadina 27 CASALIS Loredana FIS/03 Department of Physics ‐ DF OMICIUOLO Luca 28 BARALDI Alessandro FIS/03 Department of Physics ‐ DF OTTAVIANI Giulia 27 ZACCHIGNA Serena MED/28 Clinical Department of Medical Science, Surgery and Health ‐ DCSMCS Use of nanotechnology for the evaluation of the effect of laser therapy on neo‐angiogenesis tumor in vivo and in vitro PALMA Giuseppina 26 FRALEONI Alessandro FIS/03 Department of Physics ‐ DF Nanostructured dye‐sensitized solar cells PANIGHEL Mirco 27 MORGANTE Alberto FIS/03 Department of Physics ‐ DF Organic Molecules and Carbon Nanotubes Assembled on Metal Surfaces:Properties and Applications in Molecular Electronics and Photovoltaics PATERA Laerte Luigi PELLIZZONI Elena 28 AFRICH Cristina 28 TOFFOLI Giuseppe 27 LAZZARINO Marco FIS/03 Department of Physics ‐ DF Department of Physics ‐ DF Department of Physics ‐ DF Studio in situ e inoperando di processi catalitici su superfici metalliche Interactomics in tumor cells studied with a nanotechnology approach Plasmonic ruler and the applications to the DNA origami 27 CESARO Attilio 28 PAOLETTI Sergio CHIM/04 Department of Life Science ‐ DLS BIO/10 Department of Life Science ‐ DLS RADIVO Andrea 26 TORMEN Massimo FIS/03 ROMEO Michele 26 FRONZONI Giovanna PIANTANIDA Luca PITTIA Paola PORRELLI Davide ROMERO Ocana Ismael SACCO Pasquale BIO/14 FIS/03 Department of Physics ‐ DF CHIM/02 Department of Chemical and Pharmaceutical Science ‐ DSCF 28 FORNASIERO CHIM/03 Department of Paolo Chemical and Pharmaceutical Science ‐ DSCF 28 PAOLETTI BIO/10 Department of Life Study of the growth processes and of the physical and chemical properties of graphene‐based low dimensional systems Nanotecnology for food science Nanocostruttori polimerici a matrice polisaccaridica quali biomateriali bioattivi per impieghi in chirurgia Experimental study of the physics of nanostructured organic photovoltaic devices. Development and applications of methodologies TDDFT for the simulation of core spectrum for condensed matter. Combustibili solari Nuovi biomateriali per terapie Dottorando Ciclo Supervisore Sergio SANTESE Francesca 26 FERMEGLIA Maurizio SCOGNAMIGLIO Francesca SSD NomeDip Science ‐ DLS Titolo Tesi innovative nel trattamento delle ferite difficili ING‐ IND/24 Department of Engineering and Architecture ‐ DIA Multiscale molecular modeling for nanostructured multifunctional materials and coatings 28 PAOLETTI Sergio BIO/10 Department of Life Science ‐ DLS Sviluppo di un sistema adesivo per applicazioni odontoiatriche in grado di formare legami chimici sia con il collagene della dentina che con la resina riparativa SCOTTI Nicola 27 BRESCHI Lorenzo MED/28 Clinical Department Laboratory evaluation of several of Medical Science, nanofilled dental resin composites Surgery and Health ‐ mechanical and chemical properties DCSMCS STOPAR Alex 27 TOFFOLI Giuseppe FIS/03 SVETINA Cristian 28 ZANGRANDO FIS/03 Marco Department of Physics ‐ DF TARUSHA Lorena 27 PAOLETTI Sergio BIO/10 Department of Life Science ‐ DLS TAVAGNACCO Letizia 26 CESARO Attilio CHIM/04 Department of Life Science ‐ DLS VAIDYA Shital 26 GOTTER Roberto FIS/03 VEGA Marienette 27 SERGO Valter ING‐ IND/22 VELARI Simone 28 DE VITA Alessandro ING‐ IND/22 VENTURELLI Leonardo 27 SCOLES Giacinto FIS/03 Department of Physics ‐ DF VIRGILIO Francesca 26 TORMEN Massimo FIS/03 Department of Physics ‐ DF WANG Lianqin 27 FORNASIERO CHIM/03 Department of Department of Life Science ‐ DLS Department of Physics ‐ DF Department of Engineering and Architecture ‐ DIA Department of Engineering and Architecture ‐ DIA Innovative Tools for Pharmacogenetics and Pharmacogenomics: Protein‐Nucleic Acid Interactions Within Self‐ Assembled Nanosystems Photon beam studies and characterization for EUV/Soft X‐ray coherent imaging of nano‐structures using coherent FEL radiation Novel nanostructured biomaterials for biomedical applications How do water molecules probe and control bionanostructures and food functionalities Low‐dimensional magnetic materials: the electronic structure and correlation effects Raman and fluorescence spectroscopy of biomedical nanomaterials Modelling the atomic scale properties of simple biomolecules at surfaces: from the role of solvent to small structured peptides. Microfluidic Devices for Circulating Tumor Cells Counting Development of electrochemical sensors by nanofabrication techniques for biological and medical diagnostics Design, synthesis and characterization Dottorando Ciclo Supervisore Paolo SSD YOUSAFZAI Muhammad Sulaiman 28 COJOC Dan FIS/03 ZANNIER Valentina 27 RUBINI Silvia FIS/03 NomeDip Chemical and Pharmaceutical Science ‐ DSCF Department of Physics ‐ DF Titolo Tesi of nanostructured materials for electrocatalysis Department of Physics ‐ DF Synthesis and characterization of semiconductor nanowires Study of mechanotransduction signaling in tumoral and metastatic cells 3.Matrice della attività di Ricerca della scuola di nanotecnologie N. Ph.D. student N. Ph.D. student 1 ABDOLLAHZADEH Iman 29 PERONIO Angelo 2 ANGELONI Valeria 30 SAMMITO Davide 3 BORIN Daniele 31 TARUSHA Lorena 4 CAPOLLA Sara 32 ZANNIER Valentina 5 CECCHINI Paolo 33 VENTURELLI Leonardo 6 GANBOLD Tamiraa 34 WANG Lianqin 7 DIOLOSA‘ Marina 35 VEGA Marienette 8 ELISEI Elena 36 PITTIA Paola 9 FORNASARO Stefano 37 STOKELJ Tina 10 COCEANO Giovanna 38 PALMA Giuseppina 11 IONESCU Andrei Cristian 39 CORVAGLIA Stefania 12 LOVAT Giacomo 40 HUSSAIN Sajid 13 MARSON Domenico 41 MINIUSSI Elisa 14 NKOUA NGAVOUKA Maryse Dadina 42 MITRI Elisa 15 OTTAVIANI Giulia 43 CASSESE Damiano 16 PANIGHEL Mirco 44 VAIDYA Shital 17 PIANTANIDA Luca 45 ROMEO Michele 18 SALGADO 46 GANAU Mario Simâo Pedro 47 ZANUSSO Chiara 19 SCOTTI Nicola 48 MARSICH Lucia 20 STOPAR Alex 49 LUCAFO’ Marianna 21 VIRGILIO Francesca 50 CHEN Yan Xin 22 SANTESE Francesca 51 FRASSETTO Andrea 23 TAVAGNACCO Letizia 24 RADIVO Andrea 25 DAL COL Valentina 26 AMBROSINI Stefano 27 BIDOGGIA Silvia 28 GIORGIS Valentina BERNARDES PEREIRA Applications of Nanotechnology Nano character ization Nano fabrication Methods and Techniques Micro, Nano Advanced Pharmaceutics Medicine & Agro Food (E) and Opto Materials & drug Life Sciences electronics (A) biomaterials development (D) (B) and drug delivery (C) 1.1.Nanofabrication bottom 16,26,32,38,40 up ,41,43 1.2.Nanofabrication top 6,28,30,40,43 down 1.3.Nanoparticles fabrication and characterization 1.4.Self assembly 3, 16,40,41 1.5.Development of MEMS and NEMS 1.6.Development of new nanofabrication techniques / instruments 1.7.Templated growth/deposition 2.1.Single molecules detection 2.2.Living cells characterization 11, 20, 14 26,31,38,41 20, 17,31,42,46 Energy & Environment (F) 16,24,26,32,38 ,50 24,30,50 7, 17, 27,49 27,31,35,41,51 4, 9,27,31,35,48 17, 20, 27,41 20, 27,39,46 14, 27 3 36 34 5, 43 36 38,50 2,3, 17 23 29 3, 43 6,38 38 16,28,40 41 3 2 14 11,31 42 12 1,4,9,10,11,15, 31,33,42 Nano modelingtheory and 2.3.Characterization techniques/ instruments 3,38 11,19,31,35,38 47 1,3,9,11,17,19, 31,33,35,39,43 2.4.Imaging & diagnostics 3,40 8,2,11 8 2,3,4,5,8,10,11 ,15,17,20,21,4 2,46,47 2.5.Toxicity 11,31 9,42,47,49 11, 15,31 2.6.Investigations of dynamical processes 2.7.Novel characterization techniques 2.8.Nano characterization of materials 2.9.Low-dimensional systems 2.10.Electronic and geometric structure of solid surfaces 3.1.Multiscale molecular modeling 3.2.Ab initio molecular modeling 3.3.Development of new theory / methods 41 42,47 9, 17 34 20,39,43 38 38,44 27,38,44 12,32,40,41 8,27,35,41 16,32,40,41,44 41,44 16,41 41 28,30 18,22 12,45 45 45 45 8,27 8 9 29 34,38 37 20 12,29,34 29,34 29,34 13, 25 25 23,37 18 12,29 47 Number refers to the Ph.D. students. In Red the main them (one per student). 13 4.Schede attività dottorandi Questo allegato contiene le schede dei dottorandi della scuola di nanotecnologia così come sono pervenute al 31 gennaio 2013. Sono quindi incluse le schede dei dottorandi dei cicli 25, 26 e 27. • Dottorandi del 24 cilco: ZANUSSO Chiara (estensione di un anno) • Dottorandi del 25 ciclo: AMBROSINI Stefano, BIDOGGIA Silvia, CHEN Yan Xin, GANAU Mario, GIORGIS Valentina, LUCAFO' Marianna, MARSICH Lucia, PERONIO Angelo, SAMMITO Davide • Dottorandi del 26 ciclo: CASSESE Damiano, CORVAGLIA Stefania, DAL COL Valentina. FRASSETTO Andrea, MINIUSSI Elisa, MITRI Elisa, PALMA Giuseppina, RADIVO Andrea, ROMEO Michele, SAJID Hussain, SANTESE Francesca, TAVAGNACCO Letizia, VAIDYA Shital, VIRGILIO Francesca. • Dottorandi del 27 ciclo: ABDOLLAHZADEH Iman, ANGELONI Valeria, BORIN Daniele, CAPOLLA Sara, CECCHINI Paolo, COCEANO Giovanna, DIOLOSA‘ Marina, ELISEI Elena, FORNASARO Stefano, GANBOLD Tamiraa, IONESCU Andrei Cristian, LOVAT Giacomo, MARSON Domenico, NKOUA Ngavouka Maryse Dadina, OTTAVIANI Giulia, PANIGHEL Mirco, PIANTANIDA Luca, PITTIA Paola, SALGADO Bernardes Pereira Simâo Pedro, SCOTTI Nicola, STOKELJ Tina, STOPAR Alex, TARUSHA Lorena, VEGA Marienette, VENTURELLI Leonardo, WANG Lianqui, ZANNIER Valentina. 14 Dottorandi del 24 e 25 ciclo: • STEFANO AMBROSINI Title of the thesis: Growth and characterization of nanostructures Supervisor: Silvia Rubini RESEARCH ACTIVITY The aim of my Ph.D. was the synthesis and characterization of nanostructures. One of the most sought after topics of the nanoscience in the recent years are semiconductor nanowires, of which the host research group had experience, especially regarding GaAs. Bearing this aim in mind and given the rising interest into non-Au-related protocols to synthesize semiconductor nanowires (accounting the well known incompatibility of Au with Si-based technology), the first period of my Ph.D. was spent on the study and engineering of a suitable substrate to obtain the self catalyzed (Au free) nanowire growth. We found that by depositing Si onto epiready GaAs wafers, or onto thermally deoxidized wafers afterwards exposed to air, a thin silicon oxide layer was formed. Exposing such substrates (Si-treated substrates) at Ga and As fluxes resulted in epitaxially oriented, full zincblende, Ga catalyzed GaAs nanowires. We eventually found the dependences of the nanowire yield on the growth temperature, material fluxes, Si layer thickness and substrate crystal orientation. GaAs material suffers from crystal polytypism given by the hexagonal wurtzite structure and the cubic zincblende, the cohesive energy difference among them being few tens of meV. Such polytypism was a crucial problem affecting both Au- and self catalyzed GaAs nanowires. Therefore a big part of my Ph.D. was dedicated to the study of the dependence of such polytypism on growth conditions and post growth processes (more on this later). The dependence on the growth conditions were investigated and found by means of MBE in Trieste. In particular we found that when the material ratio leans towards As-rich conditions, the Ga catalyst nanoparticle shrinks and consequently the most favoured crystal structure becomes hexagonal, over the default cubic stacking. Eventually, this study led to hints of GaAs nanowire growth in absence of any catalyst at all. Deeper studies though resulted into bizarre and not fully understandable results, the main problem being a too wide dispersion of the experimental data, that made any trend not reilable. In collaboration with dott. Giacomo Priante at TASC IOM CNR (Trieste, Italy), self catalyzed GaAs nanowire were later on found to resume the catalyzed growth after the Ga catalyst consumption in As flux, in the correct (Ga rich) conditions. Electron microscopy studies (performed in Saint Petersburg State university) unveiled details of the Ga catalyst renucleation, gave the trends for the axial re-growth and the lateral over-growth and helped the formulation of a theory model to explain such a behaviour, not previosly remarked in 15 literature, the last point thanks to the collaboration with prof. Vladimir Dubrovskii from Saint Petersburg Accademic University. In particular, such growth model states that GaAs nanowires under our conditions grow in net Ga-rich conditions with negligible adatom diffusion on the nanowire sidewalls. Post growth annealing step were thought to be a solution to the GaAs polytypism. By giving thermal energy to the structures, the metastable hexagonal structure, (common in Au catalyzed nanowires ), was thought to change to the default bulk cubic structure, whose energy is lower also for nanowires with diameter on the scale of interest – 100 nm). This thesis was checked by means of TEM at DTU Nanotech and DTU CEN (Copenhagen, Denmark). Some of the experiments confirmed the theses but a too low statistics led to the conclusion that TEM was not the best technique to assess such physics. Therefore, in collaboration with dott. Damiano Cassese at TASC IOM CNR (Trieste, Italy) we approached the same task by means of Raman spectroscopy. In particular we compared the intensity of the optical phonons of the hexagonal and cubic structure, that exhibit a different and clearly distinguishable energy and found that after 100 hours at 600 °C in As atmosphere bundles of Au catalyzed hexagonal nanowires were nearly completely transformed to cubic structure. This demonstrated the hypotheses, although only on nanowire bundles measurements. In single nanowire analyses, in fact, no such a clear result was found, and the same data dispersion found by means of TEM was encountered. The last part of my Ph.D. was spent in Russia, at Saint Petersburg State and Academic Universities, studying nanowire applications and devices, MBE growth and TEM microscopy. The main results so far have been the synthesis of Au catalyzed GaAs nanowires on Si (111) capable of intense THz emission when stimulated by a femtosecond pulsed green laser, and the synthesis of self catalyzed GaAs/AlGaAs core-shell nanowires, responsible of intense, linearly polarized photoluminescence. Electron microscopy characterization activity covered the study of several types of nanostructures (synthesized in Trieste and or in Saint Petersburg). A brief visit to Durham Science Site at Durham, UK, allowed me to be trained onto FIB usage, in order to pattern by top down means silicon substrates, with the aim of spatially localize the later grown nanowires. No satisfactory result regarding such part of my project are yet available. The collateral, concomitant synchrotron activity along the 3 years has been dedicated to contactless conductivity measurements by means of spatially resolved X-ray photoemission spectroscopy on GaAs nanowires at ELETTRA synchrotron facility, Trieste, Italy. By continuing the research line of the previous Ph.D. student, Fauzia Jabeen, we found that Ga catalyzed nanowires showed a much lower electrical conductivity as opposed to the Au grown 16 wires. We explained this fact invoking the higher purity of the self catalyzed wires. We also compared the conductivity of catalytically grown wires with the non catalyzed: Si doping of these wires resulted in p doped structures in the first case (catalyzed wires) and n type in the second (non catalyzed). We explained this fact observing that the non catalyzed growth occours in As rich conditions, thus forcing the amphoteric Si to occupy the Ga sites in GaAs, resulting then in n doping. Recently, a collaboration with the canadian group of prof. LaPierre started, devoted to model the surface depletion layer of our nanowires, and obtain quantitative information on the doping of the nanostructures form the photoemission data. Publications on scientific journals (printed or in press) - S. Ambrosini, M. Fanetti, V. Grillo, A. Franciosi and S. Rubini, Journal of Applied Physics 109, 094306 (2011) - S. Ambrosini, M. Fanetti, V. Grillo, A. Franciosi and S. Rubini, AIP ADVANCES 1, 042142 (2011), selezionato per la rivista Virtual Journal of Nanoscale Science & Technology. - V.V. Danilov, A.S. Panfutova, A.I. Khrebtov, S.Ambrosini, and D.A. Videnichev, Optics Letters, Vol. 37, Issue 19, pp. 3948-3950 (2012) Publications/abstracts in conferences/congresses (national or international) - Self catalyzed GaAs nanowires on Si-treated epiready (100) GaAs wafers by MBE, S. Ambrosini, M. Fanetti, V. Grillo, A. Franciosi and S. Rubini, III-V Nanowire workshop, Bad Honnef (Germany), 02/2011 VAPOR-LIQUID-SOLID AND VAPOR-SOLID GROWTH PROCESSES: STRUCTURAL IMPLICATIONS OF CATALIST CONSUMPTION DURING SELFCATALYSED GROWTH OF GaAs NANOWIRES, Stefano Ambrosini, Mattia Fanetti, Vincenzo Grillo, Alfonso Franciosi and Silvia Rubini, 40esimo congresso della associazione italiana cristallografia (AIC), Siena, settembre 2011. - “vapor solid nanowire growth”, NGW12 Saint Petersburg Russia - “study of the final stages of GaAs nanowire growth by MBE”, SPFKC November 2012 Yekaterinburg Russia - “Vapor solid and vapor liquid solid growth of GaAs nanowires by MBE”, STRANN October 2012, Saint Petersburg Russia Participation to conferences (as speaker) - Nano2011, Yekaterinburg, 06/11 - NWGW (nanowire growth workshop) June 2012, Saint Petersburg, Russia - STRANN (New research lines in nanotechnology and nanobiotechnology) September 2012, Saint Petersburg, Russia 17 - SPFKC (winter school about problems of solid state physics) November 2012 Yekaterinburg Russia EDUCATIONAL ACTIVITY Periods abroad (date and place) 24/01/11 – 24/05/11: DTU Copenhagen, DK 19/06/11 – 01/07/11: Yekaterinburg, Russia 10/12/11 – 20/12/11: Saint Petersburg, Russia 29/04/2012 – 28/12/2012: Saint Petersburg Accademic and State University, Saint Petersburg, Russia 10/09/2012 – 25/09/2012: Durham Science Site, Durham, UK Classes followed (date, course, professor, type of course) 02/02/11 – 05/05/11, Transmission Electron Microscopy, Marco Beleggia, Ph.D student class, DTU CEN, Copenhagen (DK) Conferences, seminars, advanced courses and other didactic activities Nanotechnology graduate Summer School, Udine, Italia, july 2012. Winter school on problems of solid state physics, SPFKC, Yekaterinburg, Russia, November 2012 Support educational activity and teaching - Atomic Force Microscopy, to nanotechnology master degree students, DTU Nanotech, Copenhagen (DK) with Zachary Davis, ordinary professor at DTU Nanotech, Copenhagen (DK). - 10 hours in russian about semiconductor nanowire growth through molecular beam epitaxy at Saint Petersburg Academic University, october 2012. - 4 hours in russian about transmission electron microscopy and epitaxial growth of semiconductor nanowires at Ural Federal State University, Yekaterinburg, November 2012 18 SILVIA BIDOGGIA Title of the thesis: Mixed-monolayers protected gold nanoparticles for applications in medicine. Supervisor: Prof. L. Pasquato RESEARCH ACTIVITY The object of my research project deals with the design and synthesis of organic monolayer protected gold nanoparticles (AuNPs) with an innovative degree of complexity and functionality and the evaluation of their application in the biomedical field for the transport and release of biomolecules and drugs. During the last two years many efforts has been spent for the design, synthesis and characterization of water soluble NPs coated by hydrogenated charged ligands (H-ligands) and perfluorinated ligands (F-ligands) with the desired composition of the monolayer. Over this year, preliminary confocal fluorescence microscopy studies of uptake in living cells has been performed on these nanoparticles. In particular we are interested to investigate the ability of NPs to pass cell membrane. The behavior of these NPs in cell is compared with that of NPs coated by H- and F-ligands ending with PEG moieties (synthesized during the last two years) that we expect don’t pass cell membrane. All samples of nanoparticles were labeled with FITC as dye. Absorbance and florescence experiments have been carried out to calculate the number of fluorescent chains per nanoparticle. In that contest quenching effect of the gold core and of the fluorinated regions were analyzed. Preliminary experiments on cells have been performed by Dr. F. Sousa from Besta in Milan and have shown that both charged nanoparticles and pegylated ones are taken up by endocytosis. This unexpected behavior seems to be due to -stacking interaction between FITC moieties of different nanoparticles that is responsible of aggregates formation and the consequent cellular uptake by the well-known EPR effect. To avoid aggregates formation, the nature of the fluorescent and the loading have been changed. NPs functionalized with Bodipy, instead of FITC, have been synthesized and cellular experiments are now in progress. The organization of H-and F-ligands on the surface of nanoparticles may influence the ability to pass cellular barrier, beside many other properties. During the first two years we have investigated the morphology of mixed H- and F- ligands with multiscale molecular simulations that has given us information about the size and the shape of hydrogenated and perfluorurated domains present on NPs surface. For this reason in order to investigate the morphology of monolayers formed by H- and F-ligands by STM, mixed monolayer gold NPs coated by different ratios of commercially available dodecanthiol and tridecafluoro-1octanethiol have been synthesized and characterized. STM experiments are still in progress. Publications on scientific journals (printed or in press): • C. Gentilini, A. Pace, S. Bidoggia, P. Posocco, P. Franchi, M. Lucarini, S. Pricl and L. Pasquato “Self-organization of mixtures of fluorocarbon- and hydrocarbon amphiplic thiolates on the surface of gold nanoparticles: a combined experimental and multiscale molecular modeling study”, ACS Nano 2012, 6 (8), 7243–7253. 19 Publications/abstracts in conferences/congresses (national or international): • • • • • S. Bidoggia; L. Pasquato; “European Winter School on Physical Organic Chemistry”; Poster Presentation: “Perfluorinated monolayer-protected Au nanoparticles for membrane permeation”; Bressanone, Italy, January 30 – February 4, 2011. S. Bidoggia, P. Posocco, M. Fermeglia, S. Pricl, and L. Pasquato; “Summer School on Nanotechnology”; Poster presentation: “Control of the morphology of mixed monolayers protecting gold nanoparticles using perfluoro ligands”; Trieste, September 20-23, 2011. S. Bidoggia, M. Boccalon, D. Porrelli, L. Pasquato; “Summer School on Nanotechnology”; Poster presentation: “Perfluorinated monolayer-protected Au nanoparticles for biological applications”; Udine, July 2-5, 2012. S. Bidoggia, L. Pasquato; “Spanish Italian Symposium on Organic Chemistry”; poster presentation: “Self-organization of Mixtures of Fluorocarbon- and Hydrocarbon Thiolates on the Surface of Gold Nanoparticles”; Tenerife, Spain, February 10-14, 2012. L. Pasquato, S. Bidoggia, M. Boccalon, D. Porrelli; “Nanomedicine: from molecules to diagnosis and therapy”; Oral communication: “Toward a new generation of nanoparticles for therapy and diagnosis”; CNR Rome, October 1-3, 2012. Participation to conferences (as speaker): • • • L. Pasquato, S. Bidoggia; Summer workshop on “Supramolecular functional materials”; oral communication: "Morphology of mixed-monolayers protecting gold nanoparticles", Bibione 20 - 22 May 2010. “PhD school of Nanotechnology, Annual Meeting 2011”; University of di Trieste, January 17-19, 2011. “PhD school of Nanotechnology, Annual Meeting 2011”; University of di Trieste, January 16-18, 2012. EDUCATIONAL ACTIVITY Classes followed (date, course, professor, type of course): • Prof. A. Franciosi; “Proprietà fisiche dei materiali” (48 h); Corso di laurea magistrale in Chimica; February-June 2010. • Prof. L. Casalis, prof. A. Morgante, prof. L. Pasquato; “Molecular self-assembling and nanostructures” (16 h);PhD School of Nanotechnology; June-July 2010. • Prof. L. Pasquato; “Materiali organici” (32 h); Corso di laurea magistrale in Chimica; October-December 2010. Conferences, seminars, advanced courses and other didactic activities • • “PhD school of Nanotechnology, Annual Meeting 2010”; University of Trieste, January 18-20, 2010. Prof. Hanna Mamzer, Sociology Department of Adam Mickiewicz University in Poznan (Poland); Seminar “How to present scientific results in public”; University of Trieste, January 22, 2010. 20 • Summer workshop on “Supramolecular functional materials”; Bibione, May 20-22, 2010. • Veneto Nanotech; Seminar “NanoChallenge and PolymerChallenge”; University of Trieste, June 15, 2010. • Prof. Miguel Nobrega of the University of Minho in Portugal; seminar “Development of On-Line Monitoring devices for the extrusion process”; University of Trieste, June 15, 2010. • Prof. Maurizio Fermeglia; seminar “Use of VPN and U-GOV”; University of Trieste, June 15, 2010. • Scientific meeting “I giovani e la chimica in Friuli Venezia Giulia”; Dipartimento di Scienze e Tecnologie Chimiche, Udine, September 24, 2010. • Presentations of the last year students of the PhD school in Nanotechnology; University of Trieste, November 23, 2010. • Dr. Sangeeta Kale, Associate Professor Defence Institute of Advanced Technology (India); seminar “Metal oxide nanomaterials in sensors and biomedicine”; University of Trieste, November 23, 2010. • “PhD school of Nanotechnology, Annual Meeting 2011”; University of di Trieste, January 17-19, 2011. “European Winter School on Physical Organic Chemistry”; Bressanone, January 30 – February 4, 2011. Prof. Maurizio Prato from the University of Trieste; seminar: ”Biomaterials and Nanomedicine”; Savoia Excelsior Palace, Trieste, March 30, 2011. Prof. János Kristóf and Prof. Erzsébet Horváth of the University of Pannonia, Institute of Environmental Engineering in Hungary; seminar: “Synthesis and structure elucidation of kaolinite organo-complexes”; University of Trieste, May 3, 2011. Prof. Maurizio Fermeglia; seminar “Use of VPN and U-GOV”; University of Trieste, May 3, 2011. Dr. Hicham Hamoudi of the Université-Paris Sud; seminar: “ Self assembled monolayers on gold the challenge”; University of Trieste, July 1, 2011. Dr. Matteo Castronovo; seminar “The effect of confinement on enzymes diffusion and reactions inside DNA nanostructures”; University of Trieste, July 29, 2011. “Summer School on Nanotechnology”; Trieste, September 20-23, 2011. Dr. Cristina Gentilini from the Imperial College of London; seminar: “Biomimetic scaffold for tissue engineering”; University of Trieste, September 22, 2011. Presentations of the last year students of the PhD school in Nanotechnology; University of Trieste, November 29, 2011. • • • • • • • • • • • “PhD school of Nanotechnology, Annual Meeting 2011”; University of di Trieste, January 16-18, 2012. Prof. Norberto Masciocchi and Prof Antonietta Guagliardi of Università dell’Insubria, “Spring course on Diffraction Methods for Nanostructured Materials“, University of Trieste, March 15, 2012 21 • “Summer School on Nanotechnology”; Udine, July 2-5, 2012. Support educational activity and teaching • • • • • Support educational activity as tutor of the course Organic Chemistry I with lab, Corso di Laurea di primo livello in Chimica, first year, University of Trieste, 40 hours, April – June 2010. Support educational activity as tutor of the course Organic Chemistry I with lab, Corso di Laurea di primo livello in Chimica, first year, University of Trieste, 40 hours, April – June 2011. Support educational activity as tutor of the course Organic Chemistry I with lab, Corso di Laurea di primo livello in Chimica, first year, University of Trieste, 40 hours, April – June 2012. Tutor of a dissertation degree of Corso di Laurea di primo livello in Chimica, Title: Studi per la sintesi di nanoparticelle di oro perfluorurate solubili in mezzi acquosi. February – May 2011. Tutor of a dissertation degree of Corso di Laurea di primo livello in Chimica, Title: Nanoparticelle di oro protette da un monostrato misto di leganti idrogenati/perfluorurati: sintesi e caratterizzazione. March – July 2012. 22 YAN-XIN CHEN Title of the thesis: Nanostructured Titanium Dioxide Based Materials for Photocatalysis and Photoelectrocatalysis Supervisor: Paolo Fornasiero Tutors:Claudio Bianchini, Alessandro Lavacchi, Francesco Vizza RESEARCH ACTIVITY Titania Nanotubes arrays (TNTAs) are excellent candidates as support materials for engineering metal catalyzed materials, and has been widely used in the Fuel Cells and also in the solar production of hydrogen from aqueous solutions of renewable alcohols, due to its high active surface area; good stability in both acidic and alkaline solutions and cooperative effects between the TiO2 substrate and the support metal-based catalysts (such as Palladium). During the whole 3 years PhD study, 4 parts of works have been done. (1) TiO2 NTs over large flat samples (Ti disk), which with controllable tube length and width, had been synthesized through the anodization method. (2) A novel method, ElectroChemical Milling and Faceting (ECMF), for the modification of Pd Nanoparticles. By which the catalytic activity of supported Pd NPs was huge enhanced by an order of magnitude for the ethanol electrooxidation. (3) In order to overcome those major drawbacks for carbon black based electrodes such as mechanical stability and mass transport limitation, we propose the use of a titanium web with an ordered anatase nanotube array on top (TNTA-web) as a support for nanostructured Pd electrocatalyst for the Direct Ethanol Fuel Cells (DEFCs). And compared to the carbon black based electrodes, TNTA-web based electrodes exhibit much better stability and power density during the high current density discharge process. (4) TNTA-web also is introduced in the solar hydrogen production from water, which shows a significant improvement of H2 photoproduction from suitable aqueous solutions. Publications on scientific journals (printed or in press) (1) “Electrochemical Milling and Faceting: Size Reduction and Catalytic Activation of Palladium Nanoparticles”, Angew. Chem. Int. Ed., Vol. 51, Issue 34, (2012) 8500-8504. Yan-Xin Chen, Alessandro Lavacchi, Sheng-Pei Chen, Francesco di Benedetto, Manuela Bevilacqua, Claudio Bianchini, Paolo Fornasiero, Massimo Innocenti, Marcello Marelli, Werner Oberhauser, Shi-Gang Sun, Francesco Vizza (2) “Energy Efficiency Enhancement of Ethanol Electrooxidation on Pd-CeO2/C in Passive and Active Polymer Electrolyte-Membrane Fuel Cells”, ChemSusChem., Vol. 5, Issue 7, (2012) 1266-1273. Valentina Bambagioni, Claudio Bianchini, YanXin Chen, Jonathan 23 Filippi, Paolo Fornasiero, Massimo Innocenti, Alessandro Lavacchi, Andrea Marchionni, Werner Oberhauser, Francesco Vizza (3) “Electrooxidation in Alkaline Media of Ethylene Glycol and Glycerol on Pd-(Ni-Zn)/C Anodes in Direct Alcohol Fuel Cells”, (submitted to ChemSusChem in October, 2012 ) . Andrea Marchionni, Manuela Bevilacqua, Claudio Bianchini, Yan-Xin Chen, Jonathan Filippi, Paolo Fornasiero, Alessandro Lavacchi, Hamish Miller, Lianqin Wang, Francesco Vizza , (4) “Titania Nanotueb Ordered Arrays Anodes Boost Platinum Free Direct Alcohol Fuel Cell Performance and Stability”, (manuscript in preparation) .YanXin Chen, et.al Publications/abstracts in conferences/congresses (national or international) (1) Y.X. Chen, S.P. Chen, Z.Y. Zhou, P. Fornasiero, C. Bianchini, S.G. Sun, “ShapeControlled Synthesis of Fe Micro flowers and their Catalytic Properties for Nitrite Reduction”, ISE2010, s07-P-063, Nice, France, 2010 (2) Y.X. Chen, P. Fornasiero, A. Lavacchi, C. Bianchini, F. Vizza, S.P. Chen, S.G. Sun, “Electrochemical Milling and Faceting (ECMF): a New Method for Size Reduction and Catalytic Activation of Palladium Nanoparticles”, ISACS9, P-099, Xiamen, China, 2012 Participation to conferences (as speaker) (1) “Electrochemically shape-controlled synthesis of Fe nanoparticles, their structural characterization and properties”, oral presentation, ICCOM-CNR Florence, Sesto Fiorentino, 24 March 2010 EDUCATIONAL ACTIVITY Periods abroad (date and place) 14/08/2012-19/09/2012 xiamen university, xiamen of China Classes followed (date, course, professor, type of course) (1). Nanotechnology Summer School 2011 – September 20-23, 2011, Trieste, Italy. (2). PhD program in “Chemistry” International Course “New Concepts in Catalysis” – 24-29 June, 2012, Pavia, Italy. Conferences, seminars, advanced courses and other didactic activities (1). Annual meeting PhD School in Nanotechnology, 18-20 January 2010, total 25 hours. (2). Annual meeting PhD School in Nanotechnology, 17-19 January 2011, total 25 hours. (3). Annual meeting PhD School in Nanotechnology, 16-18 January 2012, total 25 hours. (4). The 61st Annual Meeting of the International Society of Electrochemistry, September 26th - October 1st, 2010, Nice, France 24 (5). 9° Congresso del Gruppo Interdivisionale di Chimica Organometallica della Società Chimica Italiana ( Co. G.I.C.O), 8-11 June 2010, Firenze, Italy. (6). 9th International Symposium on Carbanion Chemistry, 20-24, July 2010, Firenze, Italy. (7). The China-Italy Regional Cooperation Forum on Technology and Innovation. 10-12 November, 2010, Firenze, Italy (8). “Carbohydrate recognition: Chemistry issues and applications”, Prof. Bing-He Wang. 17/05/ 2011, Firenze, Italy. (9). “Form Metal to Metal-Free Catalysts”, Dr. Cuong Phan- Huu & Dr. Francois Garin, 29/06/2011, Firenze, Italy. (10). “Stability diagram of dipolar Bose Einstein condensate in an optical lattice”, Dr. Alves Emmauel De Lima Henn, 13/10/2011, Firenze, Italy. (11). “High resolution structure and stability of gold nanoparticles/protein complex”, Dr. Luigi Calzolai, 18/10/2011, Firenze, Italy. (12). “Computer simulation of biomolecules”, Draio A. Estrin, 26/10/2011, Firenze, Italy. (13). Challenges in Nanoscience, the International Symposia on Advancing the Chemical Sciences (ISACS9), Xiamen, China, 2012– 31 Auguest - 3 September. Support educational activity and teaching - Read the book《TiO2 Nanotube Arrays-Synthesis, Properties, and ApplicationsSPRINGER 2009》, 10-20 March, 2010, total 40 hours - Read the book《Electrochemical Methods Fundamentals and Applications John Wiley & Sons, Inc,1980》, 5-20 Auguest, 2010, total 60 hours - Read the book《Scanning Microscopy for Nanotechnology》, 2-21 May, 2011, total 30 hours - Read the book《Characterization of Nanophase Materials》, 10-20 Auguest, 2011, total 40 hours - Read the book《Renewable Resources and Renewable Energy: A Global Challenge, Second Edition》, 5-20 October, 2011, total 60 hours - Read the book《Handbook of Electrochemistry by Cynthia G. Zoski》, 1-20 November, 2011, total 80 hours - Read the book《 Solar Hydrogen Generation》, 2-21 June, 2012, total 70 hours - Read the book《Fuel Cell fundamentals》, 1-20 September, 2012, total 80 hours 25 MARIO GANAU Title of the thesis: Nanotechnology applications in quantitative neuroscience: proteomic analyses of malignant gliomas Supervisor: Prof Giacinto Scoles Tutors: Dr Loredana Casalis RESEARCH ACTIVITY The main focus of this PhD thesis is oriented toward the proteomic analyses of astrocytes in neuro-oncogenesis processes. A systematic review of multiple independent proteomic analyses of gliomas has demonstrated alterations of almost 100 different proteins; the current limit of knowledge advancement is related to the high sensitivity required to accurately monitor protein-protein interaction to follow changes in cellular pathways due to different kinds of external perturbations. To address this problem we have chosen to develop a quantitative approach based on nanotechnology to eventually enable precise, high throughput and low cost analysis of few glial cells with potential capability of real-time pathological screening and subtyping of brain tumors. Towards this goal, we decided to develop and characterize micro-fabricated wells capable to sort and host living cells and to optimize immuno nano-arrays to study, at high sensitivity, the cells secretome or proteome. The experimental activity was devoted to the fabrication and optimization of nanostructures for protein arrays. The biomarker chosen was: Glial Fibrillary Acidic Protein (GFAP), which belongs to the family of intermediate filaments and is crucial in cell’s differentiation. For the fabrication of nanoarrays, meant to immobilize antibodies specific for the abovementioned protein, an approach consisting in DNA-directed-immobilization (DDI) of biotinilated antibodies, a nanografting technique based on Atomic Force Microscopy (AFM) has been applied. Nanosized patches of thiol modified single strand DNA (ssDNA) were prepared by AFM-based nanografting inside a matrix of self assembled monolayers (SAM) of alkenthiolmodified gold surfaces. Subsequently a complementary DNA strand (cDNA) conjugated to streptavidine (STV) was allowed to covalently bind to the patch by sequence specific DNA hybridization. Finally the biotin binding sites of STV (4 binding sites per tetramer of STV) was exploited to immobilize biotinilated monoclonal GFAP Ab (alreafy in use for ELISA analyses) on the top of those nanopatches. The efficiency of those nano-immuno arrays was tested by successfully obtaining the immobilization of purified recombinant GFAP protein at a concentration of 40 nM firstly in standard conditions then in a multicells’ proteome. The immobilization was detected by means of AFM measuring step by step the increases in the 26 height of the patches and excluding modification of the signal to noise ratio and of the roughness of both the SAM and the nanopatches after incubation with the proteome. Publications on scientific journals (printed or in press) •Ganau M, Bosco A, Palma A, Beltrami AP, Cesselli D, Casalis L, Scoles G. Label-free nano-immuno-detection of GFAP in multicells’ lysate. In preparation Publications/abstracts in conferences/congresses (national or international) •M.Ganau, P.Parisse, S.Corvaglia, L.Ianeselli, D.Scaini, C.Sanavio, L.Casalis, G.Scoles. Proteomic analyses of malignant gliomas. Regional Summer School of Nanotechnology 2011 •S.Corvaglia, M.Ganau, Fruk L, Sanavio B, Ianeselli L, Cesselli D, Beltrami AP, Scoles G, Scaini D, Casalis L. Combination of novel protein nanoarrays and microwells devices for single cell protein profiling. Gordon Research Conference Proceedings 2011 EDUCATIONAL ACTIVITY Classes followed (date, course, professor, type of course) •April 29, 2010: Toffoli Giuseppe, “Pharmacokinetics and Pharmacogenomics” Facoltà di Medicina UniTs •Fall-Spring 2010: Giacinto Scoles, Lectures of Nanotechnology and Biochemistry •January 11-14, 2011: Statistics Course for Medical Residents c/o UniTs •April 11, 2011: Prof Livesey, Seminar “Stem cell models of human cerebral cortex development and disease” c/o UniTs •June 24, 2011: Prof Legname (SISSA), Prof Zanusso (UniVr), Prof Geschwind (UCSF) Seminar: Molecular Biology and clinical aspects of prion diseases c/o UniTs •July 29, 2011: Dr Castronovo (Temple University): The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA Nanostructures c/o UniTs •October 31-November 01, 2011: Lectures on Quantitative approaches to Biological Problems c/o ICTP •The experimental activity was conducted along the course of the 3 academic years at the NanoInnovation Lab Elettra Sincrotrone Trieste Conferences, seminars, advanced courses and other didactic activities / •Annual Graduate School of Nanotechnology Annual Meeting c/o UniTs •Annual Regional Summer School of Nanotechnology c/o UniT •(2010) Hanna Mamzer, Seminars “Autopresentation and preparing presentations” and “Comunication in cross cultural environment” c/o UniTs 27 •(2010) Giacinto Scoles, Seminar “Sapendo fare “single Cell Proteomics” come la vendiamo a medici e biologi?” c/o UniTs •(2010) Conference “Il ruolo emergente delle Nanotecnologie nelle Scienze della Vita” Area Science Park •(2010) Lucia Pasquato, Alberto Morgante and Loredana Casalis, Seminars “Molecular self-assembling and nanostructures” c/o UniTs •(2010) Sangeeta Kale, Seminar “ Metal oxide nanomaterials in sensors and biomedicine” c/o UniTs •(2011) Seminar BioMol c/o Elettra •(2011) Seminar Brain Awareness Week c/o Centro Interdipartimentale per le Neuroscienze Brain •(2011) Joint ICTP-KFAS conference on Nanotechnology for Biological and Biomedical Applications (Nano-Bio-Med) c/o ICTP •(2011) Conference on System Biology and New Sequencing Techniques c/o ICTP 28 VALENTINA GIORGIS Title of the thesis: Design, fabrication and characterization of metamaterials inspired plasmonic structures for sensing application Supervisor: Filippo Romanato RESEARCH ACTIVITY My research is focused on design, fabrication and characterization of metamaterials inspired plasmonic structures, expecially on Split Ring Resonator (SRR) geometry. The finite element analysis software COMSOL is used to design the metamaterials, with the support of LaNN group theoreticians (Padua). Samples are fabricated with X-Ray Lithography (XRL) technique and Electron Beam Lithography (EBL), then grown in gold using electochemical bath. To support samole fabrication other techniques are used: wet and dry etching (membrane production for X-Ray mask), metal evaporation deposition (base plating for a non-conductive substrate), sputtering deposition (substrate fabrication). Positive and negative resist has been used in order to reply mask pattern on the substrate with XRL. The final goal is the fabrication of structures to study as bio-chemical sensor. During the last year we design and fabricate new X-ray mask geometries and the litographic processes have been optimized. At the moment large area samples for microfluidic analysis have been fabricated on a transparent substrate (ITO on glass) to achieve transmission measurement. Sample characterization has shown a red-shif of the plasmon resonance peack when the structure is functionalized with thiols. Beside the thesis project, I collaborate to various research project in my group, fabricating samples (electochemical growt, evaporation deposition) and designing and building new facilities. I collaborate, also, to external universities and companies projects. • Publications on scientific journals (printed or in press) Sammito, G. Zacco, P. Zilio, V. Giorgis, A. Martucci, J. Janusonis, F. Romanato, “Design and fabrication of a light trapping method for photovoltaic devices based on plasmonic gratings”, Microelectronic Engineering 98 , pp. 440-443 F. Romanato, M. Massari, T. Ongarello, M. Carli, G. Pirruccio, D. Sammito, V. Giorgis, D. Garoli, R. Bozio, R. Pilot, R. Signorini, P. Schiavuta, F. Marinello, “Design, Fabrication and characterization of Plasmonic Gratings for SERS”, Microelectronic Engineering 88 (8), pp. 2717-2720 D. Garoli, M. Natali, G. Parisi, T. Ongarello, E. Sovernigo, M. Massari, V. Giorgis, G. Ruffato, S. De Zuani, F. Romanato “Fabrication of metamaterials in the optical spectral range”, Microelectronic Engineering 88 (8), pp. 1951-1954 29 • Publications/abstracts in conferences/congresses (national or international) V. Giorgis, M. Massari, P. Zilio, G. Parisi, G. Ruffato, G. Grenci, F. Romanato, “Large area array of split ring resonators for sensing applications ”, Metamaterials 2012 V. Giorgis, F. Romanato, M. Massari, G. Parisi, M. Carli, D. Sammito, E. Sovernigo, “Design, Fabrication and Characterization of Split Ring Resonators using X-Ray Lithography”, MNE 2011 G. Bovo, D. Sammito, D. De Salvador, G. Biasiol, M. Gaio, T. Ongarello, V. Giorgis, “Design of a plasmonic structure integrated on a GaAs HEMT photodetector for biosensing applications”, MNE 2011 D. Sammito, G. Zacco, P. Zilio, V. Giorgis, A. Martucci, J. Janusonis, “Design and fabrication of plasmonic gratings for bulk Silicon solar cell light harvesting enhancement”, MNE 2011 S. De Zuani, M. Natali, D. Garoli, V. Giorgis, M. Massari, G. Parisi, “Ferroelectric metamaterials: towards a refractive index control”, Metamaterials 2011 • Other publications Sammito, P. Zilio, G. Zacco, V. Giorgis, F. Romanato, “Nanotrutture plasmoniche per la raccolta della luce, PV Technology, 4/4/2010, p,46 • EDUCATIONAL ACTIVITY Conferences, seminars, advanced courses and other didactic activities Metamaterials 2011, St Petersburb, Russia, 17/09/2012-20/09/2012 Nanotechnology Summer School 2012, Udine, Italia, 2/07/2011-5/07/2011 2012 Winter College on Optics, Trieste, Italia, 6/2/2012-17/2/2012 Nanotechnology Summer School 2011, Trieste, Italia, 20/09/2011-23/09/2011 Metamaterials 2011, Barcellona, Spagna, 10/10/2011-13/10/2011 Metamaterials Doctoral School, Barcellona, Spagna, 14/10/2011-15/10/2011 30 MARIANNA LUCAFÒ Title of the thesis: CARBON NANOSTRUCTURES AS NANOCARRIERS FOR ANTITUMORAL DRUGS Supervisor: Prof. Gianni Sava Tutors: Dr. Sabrina Pacor, Dr. Tatiana Da Ros, Prof. Sonia Zorzet RESEARCH ACTIVITY The study of carbon nanostructures, such as fullerene, is of strong interest in biomedical field also thanks to the possibility of using them as vectors in drug delivery. During these three years, in vitro studies were carried out on two fullerene derivatives (F2 and F3) using different cell lines with the purpose to evaluate whether cytotoxicity of these compounds could change depending on the cell lines used. The studies have allowed to spot one fullerene, which has shown a very limited toxicity (F2) and another with high toxicity (F3). Unfortunately many of these studies show contradictory and ambiguous results, pointing out that the molecular mechanisms underlying the cytotoxicity of these nanomaterials are not yet completely understood. On the basis of this knowledge and with the aim to address the cell toxicity of these compounds, we performed a whole genome expression analysis, by high throughput RNA sequencing, on a human adenocarcinoma cell line exposed to two fullerenes, using the Illumina technology. Our results show that the treatment with the two fullerenes induces similar gene expression changes in a time dependent fashion. These changes include a general depression of processes related to transcription and protein synthesis, determining a slowdown of the cell cycle progression. The intensity of the alterations observed in response to F3 was always higher than for F2, confirming the previously data. Therefore F2 was chosen to continue the study as a suitable nanocarrier. Uptake tests were made on MCF7 cell line up to 72 hours, time in which the fluorescence value of F2 seems to remain stable. Fluorescence microscopy techniques have demonstrated an absence of co-localization both in mitochondria and lysosomes after treatment with F2. Moreover, it was seen that F2 did not co-localized inside the nuclei; these data are important as they exclude the possibility of direct interaction between F2 and DNA. Experiments were made on conjugated F2DOXORUBICIN above all to verify if the activity of the drug is retained or enhanced when linked to the fullerene. Furthermore we studied the cellular uptake of F2-DOXO in both MCF7 and MCF/ADR lines. Cytotoxicity tests have shown that F2-DOXO has an irrelevant activity compared to free drug because doxorubicin cannot get into the nucleus to perform its activity as it remains linked to F2. Nevertheless, the internalization of F2-DOXO is higher in MCF7/ADR compared to the free drug. So F2 could be a suitable vector to avoid the “Multidrug resistance” phenomenon caused by P-gp extrusion pump. 31 Publications on scientific journals (printed or in press) Lucafò M., Gerdol M., Pallavicini A., Pacor S., Zorzet S., Da Ros T., Prato M., Sava G. “Profiling the molecular mechanism of fullerene cytotoxicity on tumor cells by RNA-seq” ACS NANO (Submitted); Lucafò M., Pacor S., Fabbro C., Da Ros T., Zorzet S., Prato M. and Sava G. “Study of a potential drug delivery system based on carbon nanoparticles: effects of fullerene derivatives in MCF7 mammary carcinoma cells” Journal of Nanoparticle Research, vol. 14, pp. 830-842 (ISSN 1388-0764), 2012 Publications/abstracts in conferences/congresses (national or international) 16-19 September 2012, Rimini – 16° Seminario Nazionale SIF Dottorandi ed Assegnisti di Ricerca 02-05 July 2012 -Udine- Nanotechnology Summer School (Poster) 27-30 March 2011, Trieste - 5° Meeting Nuove Prospettive in Chimica Farmaceutica (Abstract and Poster); 14-17 September 2011 – Bologna - 35° Congresso Nazionale Della Società Italiana di Farmacologia (Abstract and poster) 20-23 September 2010 - Certosa di Pontignano (Siena) - “XIV Seminario nazionale per dottorandi in Farmacologia e Scienze affini” (Abstract and Poster) Conference 20-22 October 2010 - Mestre (VE) - NanotechItaly 2010 (Abstract and poster) Congress 24 November 2010 – Milano - Nanotecnologie e veicolazione di Farmaci (AICC) (poster co-author) Participation to conferences (as speaker) 16-19 September 2012, Rimini – 16° Seminario Nazionale SIF Dottorandi ed Assegnisti di Ricerca EDUCATIONAL ACTIVITY Classes followed (date, course, professor, type of course) 27\10\2010 al 29\10\2010, (30 h) Lectures on Pharmacology, given by Prof. Gianni Sava, for the students of the degree in Chemistry and pharmaceutics technology in the Faculty of Pharmacy; Lectures on the use of flow cytometer by Dr. Sabrina Pacor since February 2010 (about 40 hrs). Conferences, seminars, advanced courses and other didactic activities 10-14 September 2012 – Udine- Biology, Computation and Information Summer School 20-23 September 2011 -Trieste- Nanotechnology Summer School 2011 32 20-23 September 2010 -Certosa di Pontignano (Siena)- XIV Seminario nazionale per dottorandi in Farmacologia e Scienze affini Support educational activity and teaching Tutor for the theses in the Faculty of Pharmacy, titled: - “Confronto della citotossicità di fullereni funzionalizzati quali potenziali vettori per farmaci” (Supervisor Dr. Sabrina Pacor) - “Valutazione di biocompatibilità di nanoparticelle (SPION, GNPs) in cellule tumorali” (Supervisor Dr. Sabrina Pacor) - “Nanovettori per farmaci antitumorali: studio di un fullerene funzionalizzato ed analisi preliminare del coniugato con la doxorubicina” (Supervisor Dr. Sabrina Pacor) - “Studio di fullereni funzionalizzati come vettori per farmaci” (Supervisor Dr. Sabrina Pacor) -“Studio pilota su un modello di linfoma umano dell’attività antitumorale di nanoparticelle veicolate specificatamente” (Supervisor Prof. Sonia Zorzet); I worked as a tutor during lessons for high school lab (LLC). LUCIA MARSICH Title of the thesis: “Design and synthesis of functionalized metal nanoparticles for bioanalysis with Surface-Enhanced Raman Scattering (SERS)” Supervisor: Valter Sergo Tutors: Alois Bonifacio RESEARCH ACTIVITY During the first year as a PhD student, I developed a SERS-active substrate made of citrate reduced silver nanoparticles coated with poly-L-lysine (PLL-AgNPs). This substrate was applied for measuring free bilirubin. During my second year a calibration curve was done, confidence bands, limit of quantitation and of detection were calculated with the purpose of quantifying bilirubin in samples with unknown concentration. To apply the PLL-AgNPs for quantifying bilirubin uptake of cellular cultures exposed to nanomolar concentration of bilirubin a new buffer solution, suitable for cell growth and SERS measurement, were prepared. In particular the osmolarity and the pH were chosen considering the cell growth. With this new buffer, the bilirubin spectrum intensity is lower, because of the different protonation state of the PLL. In order to substitute the PLL coating, two polymer with quaternary nitrogen atom were chosen. The coated nanoparticles absorption maximum shown a red shift of the plasmonic frequency indicating that the coating succeeded. The relatively small red shift rules out the formation of large nanoparticles aggregates. The nanoparticles coated with this two polymer were applied to detect nanomolar concentration of bilirubin. 33 The interaction between the PLL-AgNPs and the albumin was studied. TEM images of albumin added to the PLL-AgNPs showed the protein bonded on the PLL layer around NPs. Since the bilirubin is itself hydrophobic, the NPs were coated with an hydrophobic and redisperse in hexane. During the period at the Technical University in Berlin (prof. Hildebrandt’s group) I have developed chitosan coated silver nanoparticles to detect the cytocrome-c attached on a gold surface and silica coated silver nanoparticles to detect cytochrome-b5 attached on a gold surface. Publications on scientific journals (printed or in press) •Marsich, L., Moimas, L., Sergo, V., Schmid, C.; “Raman spectroscopic study of bioactive silica-based glasses: The role of the alkali/alkali earth ratio on the NonBridging Oxygen/Bridging Oxygen (NBO/BO) ratio”; Spectroscopy 23, 2009; pp 227232 •Marsich L, Bonifacio A, Mandal S, Krol S, Beleites C, and Sergo V, “Poly-L-lysine coated silver nanoparticles as positively charged substrates for Surface Enhanced Raman Scattering”, Langmuir, 2012, 28, 13166−13171. •In preparation: Bonifacio A, Barbone M, Marsich L, Lughi V, Sergo V, “SurfaceEnhanced Raman Effect in Hybrid Metal-Semiconductor Nanoparticle Assemblies” Poster •“Polylysine coated silver nanoparticles as sensors for bilirubin quantification using Surface Enhanced Raman Spectroscopy (SERS)”, L. Marsich, A. Bonifacio, V. Sergo; Yellow Retreat; Trieste, 06 – 07 June 2011 (Congress about bilirubin studies organized by Centro Studi Fegato) •“Coated Silver Nanoparticles to Detect Heme Proteins on Gold Electrodes”, L. Marsich, A. Bonifacio, I. Weidinger, P. Hildebrandt, V. Sergo, Regional summer school of Nanotechnology, Udine, 2-5 July 2012 EDUCATIONAL ACTIVITY Periods abroad (date and place) Since the 24th of October 2011 till 19th of Aprile 2012 in Berlin (Germany) at “Technische Universitaet”, in the “Institut fuer Chemie Max-Volmer-Laboratorium für Biophysikalische Chemie”. Classes followed (substituted by personal study) Books: •R. Aroca, “Surface-Enhanced Vibrational Spectroscopy” 2006 John Wiley & Sons, Ltd 34 •“Bile pigments and Jaudice , Edited by J. Donald Ostrow. New York: Marcel Dekker, Inc., 1986. •D. Harvey, “Modern Analytical Chemistry”, 2000 McGraw-Hill Higher Education •F. Siebert and P. Hildebrant, “Vibrational spectroscopy in Life Science”, 2008, WILEYVCH Reviews: •Hyunhyub Ko, Srikanth Singamaneni, and Vladimir V. Tsukruk, ”Nanostructured Surfaces and Assemblies as SERS Media”, Small 2008, 4, No. 10, 1576–1599 •Richard J. C. Brown, Martin J. T. Milton, “Nanostructures and nanostructured substrates for surface-enhanced Raman scattering (SERS)”, J. Raman Spectrosc. 2008; 39: 1313–1326 •Xiu-Mei Lin, Yan Cui, Yan-Hui Xu, Bin Ren, Zhong-Qun Tian, “Surface-enhanced Raman spectroscopy: substrate-related issues”, Anal Bioanal Chem, DOI 10.1007/s00216-009-2761-5 •J. Millstone et al. “Colloidal gold and silver triangular nanoprisms.”, Small, 2009, Vol 5, Issue 6, Pages 646-664 •A. Guerrero Martinez “Nanostars shine bright for you: Colloidal synthesis, properties and applications of branched metallic nanoparticles” Current Opinion in Colloid & Interface Science, April 2011, Volume 16, Issue 2, Pages 118-127. Conferences, seminars, advanced courses and other didactic activities Final Conference 2009 – Trieste,18 - 20 January 2010 (PhD School in Nanotechnology) How to present scientific results, Trieste 22 January 2010 Yellow Retreat – Trieste, 08 – 09 March 2010 Yellow Reatreat – Trieste, 08 – 09 March 2010 (Congress about bilirubin studies organized by Centro Studi Fegato) Intensive course about "Molecular self-assembling and nanostructures” , Trieste 23 June - 13 July 2010 Tour of SENIL laboratories (Elettra) - Trieste, 20 July 2010 XVI Scuola Nazionale di Scienza dei Materiali – Bressanone (BZ), 27 September- 02 October 2010 “High-Resolution Integrated Micro Electrode Arrays (MEAs) for Imaging Neurophysiological Signaling” – Trieste, 25 October 2010 “Introduzione alla tecnologia MEMS”, Dr Ing Cristina Bertoni – Trieste, 12 April “Synthesis and structure elucidation of kaolinite organo-complexes”, János Kristóf and Erzsébet Horváth – Trieste, 3 May 2011 Yellow Retreat – Trieste, 06 – 07 June 2011 (Congress about bilirubin studies organized by Centro Studi Fegato) “Self assembled monolayers on gold the challenge”, Dr. Hicham Hmamoudi - 1 July 2011 35 “The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA Nanostructures”, Matteo Castronovo – 18 July 2011 Regional summer school of Nanotechnology – Trieste, 19 – 23 September 2011 “Functionalized nanoparticles for bioanalysis”, Arumugam Sivanesan, Berlin, 13 January 2012 “Influence of the protein environment on the Raman spectra of cyanobacterial phytochrome” Grazia Daminelli, Berlin, 20 January 2012. “The investigation of rubber by vibrational spectra”, Katharina Haider, Berlin, 9 March 2012 “SERS for protein and estrogen detection”, XiaoXia Han, Berlin, 20 April 2012 Regional summer school of Nanotechnology, Udine, 2-5 July 2012 “Robust Imaging and Delivery Systems: Targeted Nanoparticles”, dr. Luis Nunez, Universtiy of Chicago and BioTarget Inc, Trieste, 17 September 2012 Support educational activity and teaching 20 h following three students in the Raman laboratory. Safety training of undergraduate students in chemical laboratory. Co-advisor of a master thesis in material engineering with the title: “Sintesi e caratterizzazione di nanoparticelle ibride semiconduttore-metallo come marcatori ottici per applicazioni biomediche”. Co-advisor of a bachelor thesis in industrial engineering with the title: “Nanostrutture metalliche per applicazioni SERS (Surface Enhanced Raman Spectroscopy) ottenute per deposizione di oro”. Co-advisor of a bachelor thesis in industrial engineering with the title: “Valutazione dei rischi e pianificazione del sistema di prevenzione e protezione: applicazione ad un laboratorio chimico universitario a scopo didattico e di ricerca”. 36 ANGELO PERONIO Title of the thesis: Single-molecule heterogeneous catalysis Supervisor: prof. Giovanni Comelli Tutors: prof. Carlo Dri RESEARCH ACTIVITY My research topic is the study of model systems for heterogeneous catalysis at the singlemolecule level by means of sub-molecularly resolved imaging and spectroscopy with a lowtemperature scanning tunnelling microscope (LT-STM). In these years I studied a coadsorption complex formed by ammonia and nitrogen monoxide on the (111) surface of platinum. This is a model system to understand the selectivity in the catalytic reduction of nitrogen monoxide by ammonia (SCR). I determined the microscopic structure of the complex and the nature of the interaction between NH3 and NO, using a combined experimental (STM) and theoretical (DFT) approach. A side topic was the hydrogenation of CO2 to methanol catalyzed by nickel and copper alloys. In particular I characterized by STM the structural properties of CO2 chemisorbed on Ni(110). This species is particularly reactive, due to a strong charge transfer from the surface, and has thus a central role in the hydrogenation process. On the instrumental side. I introduced in our laboratory the inelastic electron tunneling spectroscopy (STM-IETS), which allows to measure the vibrational spectrum of single molecules adsorbed on a surface. Since our group lacked previous expertise in STM-based spectroscopies, it was necessary to understand in detail the role of the various experimental parameters. This characterization led to the formulation of a set of protocols to measure the performance of the various components of a STM system, and to an innovative detection scheme, increasing the energy-resolution of the IETS spectra. Publications on scientific journals (printed or in press) •C. Dri, A. Peronio, E. Vesselli, C. Africh, M. Rizzi, A. Baldereschi, M. Peressi, and G. Comelli, Imaging and characterization of activated CO2 species on Ni(110) Phys. Rev. B 82, 165403 (1-6) (2010), doi: 10.1103/PhysRevB.82.165403 •M. Rizzi, S. Furlan, M. Peressi, A. Baldereschi, C. Dri, A. Peronio, C. Africh, P. Lacovig, E. Vesselli, and G. Comelli Tailoring bimetallic alloy surface properties by kinetic control of self-diffusion processes at the nano-scale J. Am. Chem. Soc. 134 (2012) 16827, doi: 10.1021/ja307294p 37 Publications/abstracts in conferences/congresses (national or international) •Poster: CO2 activation and hydrogenation on Ni model catalysts: an atomic-scale investigation by spectroscopy and microscopy measurements and ab-initio calculations; E. Vesselli, M. Rizzi, C. Dri, A. Peronio, C. Africh, X. Ding, A. Baraldi, A.Baldereschi, M. Peressi, and G. Comelli, presented at the workshop of the Istituto Officina dei Materiali del CNR, 30 settembre – Padriciano (TS), October 1, 2010, •Poster STM-based tools for the investigation of chemical processes at the atomic level: FastSTM and single molecule vibrational spectroscopies; C.Dri, A.Peronio, C.Africh, F.Esch and G.Comelli, presented at the workshop of the Istituto Officina dei Materiali del CNR, 30 settembre – Padriciano (TS), October 1, 2010 •Talk Catalysis at the single molecule level at the annual meeting of the School in Nanotechnology, University of Trieste, January 17-19, 2011 •Poster A NH3‒NO coadsorption complex on Pt(111), A. Peronio, A. Cepellotti, S. Marchini, N. Abdurakhmanova, C. Dri, C. Africh, F. Esch, M. Peressi e G. Comelli, presented at the 1st joint Summer School on Nanotechnology, University of Trieste, September 20-23 2011; and at the Slonano 2011 conference, Institut Jožef Stefan, Ljubljana (SLO), October 27, 2011 •Talk Catalysis at the single molecule level at the annual meeting of the School in Nanotechnology, University of Trieste, January 16-18, 2012 •Poster Ideas towards an optimized detection scheme for STM-IETS, A. Peronio, C. Dri e G. Comelli, presented at the 2nd joint summer school on Nanotechnology, Udine, July 2-5 2012 •Talk Optimized detection scheme for STM-IETS at the 14a Vibrations At Surfaces conference, Kobe (JP), September 24-28, 2012 Participation to conferences (as speaker) •Annual meeting of the Graduate school of Nanotechnology, University of Trieste, January 17-19, 2011. Talk Catalysis at the single molecule level •Annual meeting of the Graduate school of Nanotechnology, University of Trieste, January 16-18, 2012. Talk Catalysis at the single molecule level a •14 Vibrations At Surfaces conference, Kobe (JP), September 24-28, 2012. Talk Optimized detection scheme for STM-IETS EDUCATIONAL ACTIVITY Periods abroad (date and place) November 7, 2011 – December 22, 2011: visiting scientist at prof. Saw-Wai Hla group, Ohio University, Athens (OH), USA 38 Classes followed (date, course, professor, type of course) •Heterogeneous catalysis, module of M.Sc. programme in Chemistry at Trieste University, taught by prof. Paolo Fornasiero, 16 hours, March 2010. •Advanced statistics for data analysis, course of M.Sc. programme in Physics at Trieste University, taught by prof. Edoardo Milotti, 48 hours, ottobre-dicembre 2010. •Photoemission spectroscopies and spectromicroscopies, course of PhD programme in Physics at Trieste University, taught by proff. Alessandro Baraldi, Andrea Goldoni and Andrea Locatelli, 25 hours, November-December 2010 •Molecular self-assembling and nanostructures, course of the graduate school in Nanotechnology of the University of Trieste, taught by dr. Loredana Casalis, prof. Alberto Morgante, and prof. Lucia Pasquato, 10 hours followed, June 21, 2011 – July 15, 2011 •Laboratory: almost all of my research activity was performed at the SSR-STM laboratory of IOM-CNR laboratorio Tasc. Conferences, seminars, advanced courses and other didactic activities •School Synchrotron and free-electron-laser sources and their multidisciplinary applications, Abdus Salam International Centre for Theoretical Physics, Trieste, about 70 hours, April 26 – May 7 2010 •Spring college on Computational nanoscience, Abdus Salam International Centre for Theoretical Physics, Trieste, about 70 hours, May 17 - 28 2010. •Workshop of the Istituto Officina dei Materiali of CNR, Padriciano (TS), about 12 ore, September 30 – October 1 2010 •Seminar Synthesis and structure elucidation of kaolinite organo-complexes by prof. János Kristóf and Erzsébet Horváth of the Universiy of Pannonia, University of Trieste, May 3 2011 •Seminar Self assembled monolayers on gold the challenge by dr. Hicham Hamoudi of the Université-Paris Sud, University of Trieste, July 1, 2011 a •1 joint Summer School on Nanotechnology, University of Trieste, September 20-23, 2011 •Slonano 2011 conference, Institut Jožef Stefan, Ljubljana (SLO), October 27, 2011 •Spring course on Diffraction Methods for Nanostructured Materials. Taught by prof. Norberto Masciocchi from Unversity of Insubria and Antonietta Guagliardi from Istituto di Cristallografia of CNR and University of Insubria. University of Trieste, March 15, 2012. •Seminar How to perform a literature search using the resources available at UNITS, and how to connect to the UNITS network form outside the campus, by prof. Maurizio Fermeglia of the University of Trieste. University of Trieste, June 6, 2012. •Seminar Polymer-based nanocomposites, by dr. Galder Kortaberria from Escuela Universitaria Politécnica of Donostia (ES). University of Trieste, June 6, 2012. 39 •2a joint summer school on Nanotechnology, July 2-5 2012, Udine. •14a Vibrations At Surfaces conference, September 24-28 2012, Kobe (JP). Support educational activity and teaching •Tutor for a B.Sc thesis in Physics, Vibrational properties of single molecules of ammonia adsorbed on Pt(111) by low-temperature scanning tunneling microscopy, University of Trieste, defended on September 24, 2010. •April 4 2011, January 23 2012 and February 15 2012: hands-on seminar for high school students “The physics of hydrogen fuel cells” at the department of Physics of the University of Trieste, within the Progetto Lauree Scientifiche of the University of Trieste. 1st place at the Italian national contest “Piano Lauree Scientifiche” for the best popular work in Chemistry for high school students •Tutor for a M.Sc thesis in Physics, Structural and electronic properties of cysteamine adsorbed on gold surface by low-temperature scanning tunneling microscopy, University of Milano, to be defended. 40 DAVIDE SAMMITO Title of the thesis: Integration of plasmonic gratings into optoelectronic devices Supervisor: prof. Filippo Romanato RESEARCH ACTIVITY My research activity is focused on the integration of nanostructured metallic gratings on optoelectronic devices with the aim to exploit plasmonic effects to control light absorption properties. I have been working on three different applications of plasmonic crystals to thin film organic solar cells, to wafer-based conventional silicon solar cells and to phototransistor made of GaAs/AlGaAs. In particular during the last year I have been focusing on the last two applications. For what concerns photovoltaic devices, I wrote three papers. I have compared, in thin film and wafer-based solar cells, the light trapping properties of gratings constituted by silver nanowires. I described the nanofabrication technique developed, that is based on laser interference lithography and is suited to the large surface area of solar cells. I highlighted by simulations that the designed gratings allow a global conversion efficiency enhancement in thin film devices. On the other hand in wafer-based cells only an improvement of internal quantum efficiency can be obtained and it is due to the redistribution of light absorption profile in the semiconductor. These findings are supported by comparison of modeling results with external quantum efficiency and front surface reflectance measurements. For what concerns phototransistors, I have studied the integration of gold plasmonic gratings with V-groove shape on the gate. The aim is to detect, by variations in conductivity of the devices, modulations of light intensity transmitted toward the 2D electron gas due to the coating of the gate surface with a thin layer of bioanalytes. I have optimized the epitaxial multilayer measuring the electro-optical response and fabricated devices by lithographic techniques. In a first batch of samples, the trend of conductivity versus incidence angle curves, before and after functionalization, has shown a good agreement with simulation and it is possible to estimate that a batch integrating optimized nanostructures could give a resolution of the order of 10-5 in terms of effective refractive index. Publications on scientific journals (printed or in press) •Sammito D., Zilio P., Zacco G., Janusonis J., Romanato F., “Light trapping properties of metallic gratings on wafer-based silicon solar cells” (2012) Nano Energy, http://dx.doi.org/10.1016/j.nanoen.2012.10.008 41 • Sammito D. , Zacco G. , Zilio P. ,Giorgis V. , Martucci A. , Janusonis J. , Romanato F., “Design and fabrication of a light trapping method for photovoltaic devices based on plasmonic gratings” (2012) Microelectronic Engineering, 98, pp. 440–443 • Zilio P., Sammito D., Zacco G., Mazzeo M., Gigli G., Romanato F., “Light absorption enhancement in heterostructure organic solar cells through the integration of 1-D plasmonic gratings” (2012) Optics Express, 20(14), pp. A476-A488 • Garoli D., Romanato F., Zilio P., Natali M., Marinello F., Ongarello T., Sammito D., De Salvador D., “Fabrication of "nano-rocket-tips" for plasmonic nanofocusing” (2011) Microelectronic Engineering, 88 (8), pp. 2530-2532. • Romanato F., Pilot R., Massari M., Ongarello T., Pirruccio G., Zilio P., Ruffato G., Carli M., Sammito D., Giorgis V., Garoli D., Signorini R., Schiavuta P., Bozio R., “Design, fabrication and characterization of plasmonic gratings for SERS” (2011) Microelectronic Engineering, 88 (8), pp. 2717-2720. • Zacco G., Romanato F., Sonato A., Sammito D., Ruffato G., Morpurgo M., Silvestri D., Carli M., Schiavuta P., Brusatin G., “Sinusoidal plasmonic crystals for bio-detection sensors” (2011) Microelectronic Engineering, 88 (8), pp. 1898-1901. • Zilio P., Sammito D., Zacco G., Romanato F., “Absorption profile modulation by means of 1D digital plasmonic gratings” (2010) Optics Express, 18 (19), pp. 19558-19565. Publications/abstracts in conferences/congresses (national or international) •Poster: Sammito D., De Salvador D., Biasiol G., Bovo G., Zilio P., Ongarello T., Massari M. and Romanato F., “Design of a AlGaAs/GaAs HEMT photodetector integrating plasmonic nanostructures for biosensing applications”, NanotechItaly 2012, Venice 21-22 November 2012 •Poster: Zilio P., Sammito D., Zacco G., Mazzeo M., Gigli G. and Romanato F., “Analysis of absorption enhancement mechanisms in organic solar cells by means of plasmonic crystals”, NanotechItaly 2012, Venice 21-22 November 2012 •Poster: Sammito D., Zacco G., Zilio P., Sovernigo E., Dai Prè M., Martucci A., Janusonis J. and Romanato F., “Integration of plasmonic gratings on flat wafer-based silicon solar cells for light trapping purpose”, E-MRS spring 2012, Strasbourg 14-18 May 2012 •Poster: D. Sammito, P. Zilio, G. Zacco, A. Martucci, M. Dai Prè, J. Janusonis, J. Ulbikas, S. Padovani, F. Rasello, S. Sinesi and F. Romanato, “The ORION project: nanotechnology applied to bulk Silicon solar cells”, NanotechItaly 2011, Venice 23-25 November 2011 •Poster and Conference Proceedings: G. Zacco, D. Sammito, P. Zilio, G. Melcarne, G. Gigli, M. Mazzeo, F. Romanato, “Light harvesting enhancement in organic solar cells 42 through the integration of plasmonic crystals”, 26th European Photovoltaic Solar Energy Conference and Exhibition, Hamburg 5-9 September 2011 •Poster: G. Bovo, D. Sammito, D. De Salvador, G. Biasiol, M. Gaio, V. Giorgis, P. Zilio, T. Ongarello and F. Romanato, “Design of a plasmonic structure integrated on a GaAs HEMT photodetector for biosensing applications”, 37th International Conference on Micro and Nano Engineering, Berlin 19-23 September 2011 •Poster: V. Giorgis, F. Romanato, M. Massari, G. Parisi, M. Carli, D. Sammito, E. Sovernigo, “Design, Fabrication and Characterization of Split Ring Resonators using X-Ray Lithography”, 37th International Conference on Micro and Nano Engineering, Berlin 19-23 September 2011 • Poster: P. Zilio, D. Sammito, G. Zacco, and F. Romanato, “Role of Resonances of Digital Plasmonic Gratings in Absorption Profile Remodulation in Silicon Solar Cells”, OSA Optical Nanostructures for Photovoltaics, Karlsruhe 2010, and CNRIOM Workshop, Trieste 2010 • Poster e conference proceedings: “Absorption Profile Remodulation in Silicon Solar Cells by Means of Plasmonic Gratings”, D. Sammito, P. Zilio, G. Zacco, and F. Romanato, 25th EUPVSEC - WCPEC-5, Valencia 2010 Other publications •D. Sammito, P. Zilio, G. Zacco, V. Giorgis, F. Romanato, “Nanostrutture plasmoniche per la raccolta della luce”, PV Technology, 4/4 2010, p. 46 Participation to conferences (as speaker) •“Design and fabrication of plasmonic gratings for bulk Silicon solar cell light harvesting enhancement”, 37th International Conference on Micro and Nano Engineering, Berlin 19-23 September 2011 EDUCATIONAL ACTIVITY Classes followed (date, course, professor, type of course) o“Materiali nanostrutturati”, prof. V. Lughi, “corso di laurea specialistica in ingegneria dei materiali”, second semester 2009/2010 o“Laboratorio di materiali elettrici e fotovoltaici”, prof. A. Massi Pavan, “corso di laurea specialistica in ingegneria dei materiali”, second semester 2009/2010 Conferences, seminars, advanced courses and other didactic activities •Nanotechnology summer school, University of Udine, 2-5 July 2012 •Winter College on Optics: Advances in Nano-Optics and Plasmonics, ICTP Trieste, 6-17 February 2012 •Nanotechnology school annual meeting, University of Trieste, 16-18 January 2012 43 •Congress: “Nanotechnology school congress”, Università di Trieste 17-19 January 2011 •Course on Labview programming environment at Sincrotrone Trieste April 2011 •Course: “Molecular self-assembling and nanostructures”, Università di Trieste June-July 2011 •Seminar: “Self assembled monolayers on gold the challenge”, Hicham Hmamoudi at Università di Trieste 1 July 2011 •Seminar: “The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA Nanostructures”, Matteo Castronovo at Università di Trieste 29 July 2011 •Summer school: “International Summer School on Photovoltaics and New Concepts of Quantum Solar Energy Conversion”, organized by Helmholtz Zentrum Berlin at Hirschegg (Austria) 11-18 September 2011 •Workshop of the School of Nanotechnology: January 18th-20th 2010 •Seminar: ‘How to present scientific results in public’, dr. Hanna Mamzer of Adam Mickiewicz University in Poznan (Poland), January 22nd 2010 •Workshop: Electron Beam Lithography with Jeol JBX-6300FS, January 25th-29th 2010 at Nanofab, Venezia – Marghera •Workshop: Comsol Multiphysics, 4/3/10 Trieste •Summer school: International school of quantum electronics, 47th course advances on nanophotonics III: plasmonics and energy efficiency, 11-18/07/10 Erice, Ettore Majorana Foundation and Centre for Scientific Culture •Seminar: “Development of On-line Monitoring devices for the extrusion process”, prof. Miguel Nobrega of the University of Minho, 15/06/10 •Seminar: “Use of VPN and UGOV”, 15/06/10 •Workshop IOM, 30/09 – 1/10/2010 •Course: “Fundamentals of electron microscopy and analytical techniques”, Dr. R. Ciancio, 12-13/10/10 Laboratorio TASC •Seminar: “Metal oxide nanomaterials in sensors and biomedicine”, Dr. Kale of the Defence Institute of Advanced Technology (DIAT) India, 23/11/10 •Books reading: o “Plasmonics – fundamentals and applications”, S. Maier o “Handbook of photovoltaic science and engineering”, A. Luque, S. Hegedus Support educational activity and teaching •Tutor of Gianluca Bovo in his experimental activity finalized with the master thesis in Material Science at University of Padua having as title “Multilayer electro-plasmonic nanostructures for biosensing architectures” 44 CHIARA ZANUSSO Title of the thesis: “Nanotechnologies and oncology: pharmacokinetics and pharmacogenomics to optimize the antitumoral therapies” Supervisor: dr. Giuseppe Toffoli Tutors: prof. Tullio Giraldi RESEARCH ACTIVITY 1° year: This study purpose is to characterize pharmacogenetic markers above all the neurological type involved in the response and toxicity to the pharmacologic treatment with oxaliplatin in patients with colorectal cancer. At first literature search has been done to define the genetic polymorphisms of possible prognostic/predictive significance. Polymorphisms of glutathione S-transferase (GST) has been identified, transmembrane transporters (ATPBinding Cassette) that are responsible for the extrusion of the drug from the cell, and polymorphisms concerning DNA repair genes that codify for proteins involved in the repair of the damage exerted on nucleic acid from mutagens as alkylating drugs. 154 patients were enrolled with colorectal cancer (CCR) treated with adjuvant FOLFOX-4 from the National Cancer Institute of Aviano (CRO) and other centres of Veneto region. At first genomic DNA was extracted from peripheral blood samples and then the development of analytical methods was performed. Specifically an innovative use of nanotechnologies in gene sequencing has been implemented, such as Pyrosequencing, a technique of recent development, that allows to identify simply and quickly mutations of punctiform type (SNP). Finally statistical analysis of data was performed to evaluate the relative risk (OR) of developing colorectal cancer by means of case-control studies and the role of individual gene variations in making prone the patient to the development of toxic reactions after chemotherapy with oxaliplatin. 2° year: The aim of this study is to assess the impact of certain genetic variants (polymorphisms) involved in the process of carcinogenesis and tumor progression. Prostate cancer (CA) is the third most common cause of cancer deaths in men of all ages and is a major health problem worldwide. Incidence and mortality rates of prostate cancer vary substantially worldwide, suggesting the importance of environmental/lifestyle risk factors and perhaps their combination with genetic variants across racial/ethnic populations. The genetic characteristics of the patient are one of the determinants in the inter-subject variation observed in the outcome of anti-tumor therapy, and pharmacogenetics aims to validate and use in clinical practice certain genetic markers in order to customise and optimize therapy. 45 Pharmacogenetics aims to validate and then use some genetic markers in clinical practice in order to customize and optimize therapy. At first literature search has been done to define the genetic polymorphisms of possible prognostic/predictive significance. Polymorphisms of glutathione S-transferase (GST) has been identified, transmembrane transporters (ATPBinding Cassette) that are responsible for the extrusion of the drug from the cell, and polymorphisms concerning DNA repair genes. 917 patients were enrolled with prostate cancer from the National Cancer Institute of Aviano (CRO) and 1342 healthy controls of Friuli Venezia-Giulia region. The analytical methods used for assessing polymorphisms examined are based on amplification of the portion of the gene of interest by PCR and subsequent analysis with TaqMan method, which relies on a direct and quantitative measurement of the amplified DNA using a probe fluorescent, or with the Pyrosequencing technology, a nanotechnology of recent development, that allows to identify simply and quickly mutations of punctiform type (SNP). Finally statistical analysis of data was performed using Fisher's Exact test, has been calculated odds ratios (OR) and corresponding 95% confidence interval (95%CI) to evaluate the relative risk (OR) of developing prostate cancer. 3° year: Radical radiotherapy, employed alone or in combination with chemotherapy, is one of the major modalities used in the treatment of cancer. Although several clinicopathologic indicators, such as prostate-specific antigen level (PSA), Gleason score, pathologic stage, and surgical margin status, are currently used to predict therapy outcome, there is a need to find new biomarkers to improve the prediction of disease recurrence. There is evidence that in addition to patient-related factors such as age and lifestyle, the heterogeneity in response to radiotherapy in prostate cancer is attributable to a genetic basis. The aim of this study is to assess the impact of certain genetic variants (polymorphisms) as genes impacting DNA repair, oxidative stress, phase I and II metabolism and apoptosis, on tumor response (risk to disease recurrence) to radiotherapy in prostate cancer. 924 prostate cancer patients treated with radiation therapy (adjuvant or radical) in association or not with surgery and/or hormone therapy were enrolled at the National Cancer Institute of Aviano (CRO), but only 864 resulted eligible for the evaluation of the risk of biochemical recurrence. Patients with post-radiotherapy PSA level ≥ 0.2 ng/ml (almost 3 months since the end of radiotherapy) have been considered to show biochemical PSA recurrence. Genomic DNA of each patient has been extracted from whole blood. After PCR amplification, genetic tests have been performed by Pyrosequencing, a nanotechnology that allows to identify mutations of punctiform type (SNP), TaqMan allelic discrimination, and automated fragment analysis technologies. Statistical analysis has been done by SAS software (version 9.2) (SAS Institute Inc., Milan, Italy). 46 Publications on scientific journals (printed or in press) 1. “NUCLEOTIDE EXCISION REPAIR GENE VARIANTS AND ASSOCIATION WITH SURVIVAL IN OSTEOSARCOMA PATIENTS TREATED WITH NEOADJUVANT CHEMOTHERAPY” P Biason, CM Hattinger, F Innocenti, R Talamini, M Alberghini, K Scotlandi, C Zanusso, M Serra and G Toffoli The Pharmacogenomics Journal (2011), 1-8 2. “A PROSPECTIVE VALIDATION PHARMACOGENOMIC STUDY IN THE ADJUVANT SETTING OF COLORECTAL CANCER PATIENTS TREATED WITH THE 5-FLUOROURACIL/LEUCOVORIN/OXALIPLATIN (folfox4) REGIMEN” E Cecchin, M D’Andrea, S Lonardi, C Zanusso, N Pella, D Errante, E De Mattia, J Polesel, F Innocenti, G Toffoli The Pharmacogenomics Journal (2012), 1-7 Publications/abstracts in conferences/congresses (national or international) 1. “FARMACOGENETICA DELLA CARDIOTOSSICITÀ DA ANTRACICLINE” C Zanusso and G Toffoli, (long abstract for the conference entitled “Complicanze cardiovascolari in oncologia: ieri ed oggi. La gestione delle problematiche”, Napoli, March 25-26, 2009) 2. “NANOTECHNOLOGIES AND ONCOLOGY: PHARMACOKINETICS AND PHARMACOGENOMICS TO OPTIMIZE THE ANTITUMOR THERAPIES” C Zanusso, E Cecchin, P Biason, E De Mattia, F Sartor and G Toffoli (Poster presented at the 2nd Phd workshop 10th/11 September 2009, Wittenberg) (Abstract presented at the “Congresso Nazionale della Società Italiana di Chemioterapia”, Udine, October 14, 2009) 3. “RADIOGENETICS AND THE OUTCOME OF RADIATION-TREATED PROSTATE CANCER PATIENTS” C Zanusso, E Cecchin, R Bortolus, P Biason, E De Mattia, S Boffo, MG Trovò, and G Toffoli (Abstract presented at “35° Congresso Nazionale della Società Italiana di Farmacologia” Bologna, 14-17 September 2011) 4. “GENETIC POLYMORPHISMS IN THE EARLY ONSET OF OXALIPLATIN NEUROPATHY AFTER ADJUVANT FOLFOX“ E Cecchin, C Zanusso, M D'Andrea, N Pella, D Errante, S Bonura, M Bari, M Medici, A Buonadonna, P Biason, E De Mattia and G Toffoli 47 (Abstract presentato al “35° Congresso Nazionale della Società Italiana di Farmacologia” Bologna , 14-17 September 2011) 5. “PHARMACOGENETICS IN OSTEOSARCOMA: THE ROLE OF NUCLEOTIDE EXCISION REPAIR GENE VARIANTS IN SURVIVAL AFTER NEOADJUVANT CHEMOTHERAPY” P Biason, C Zanusso, S Boffo, E De Mattia, E Cecchin, CM Hattinger, M Serra, G Toffoli (Abstract presentato al III° Convegno monotematico Società Italiana di Farmacologia “Farmacogenomica e cancro: dal laboratorio alla clinica”; Grado (GO), 8 October 2011) 6. “FROM BENCH TO BEDSIDE: A GENOTYPE-GUIDED PHASE I STUDY OF FOLFIRI AND BEVACIZUMAB IN ADVANCED COLON-RECTAL CANCER PATIENTS” S Boffo, E Marangon, E Cecchin, E De Mattia, F Innocenti, S Frustaci, A Buonadonna, GM Miolo, AM Colussi, E Turchet, P Biason, C Zanusso, E Mazzega, P Giusti, G Toffoli (Abstract presentato al III° Convegno monotematico Società Italiana di Farmacologia “Farmacogenomica e cancro: dal laboratorio alla clinica”; Grado (GO), 8 October 2011) Participation to conferences (as speaker) 1. “RUOLO DELLA FARMACOGENETICA NEL CARCINOMA PROSTATICO DELL’ANZIANO” Convegno GUONE “Il tumore della prostata nell’anziano”, Adria (RO), 23 November 2012 EDUCATIONAL ACTIVITY Classes followed (date, course, professor, type of course) • • • • • • 700 hours of study and deepening of the topics covered by books and review-type paper and / or electronic from January 1, 2009; 700 laboratory hours at the "Experimental and Clinical Pharmacology", CRO Aviano from January , 2009 700 hours of study and deepening of the topics covered by books and review-type paper and / or electronic from January 1, 2010; 700 laboratory hours at the "Experimental and Clinical Pharmacology", CRO Aviano from January 1, 2010 400 hours of study and deepening of the topics covered by books and review-type paper and / or electronic from April 16, 2012; 100 laboratory hours at the "Experimental and Clinical Pharmacology", CRO Aviano from April 16, 2012 48 Conferences, seminars, advanced courses and other didactic activities “Congresso annuale delle presentazioni dell’attività scientifica dei dottorandi in corso”, University of Trieste, January 13-14-15, 2009. “Seminario sull'uso della VPN e del Portale”, University of Trieste, March 20, 2009. “Esame Finale 2009”, University of Trieste, April 8, 2009. “Modeling reactions at the nanoparticle scale” (Prof. Phillip R. Westmoreland Dept of Chemical Engineering, University of Massachusetts Amherst), University of Trieste, May 8, 2009. “Chimica fisica delle interfasi in sistemi nanostrutturati” (Dr. Italo Colombo), University of Trieste, May 15, 2009. “Incontri informativi per i dottorandi: orientamento all’utilizzo delle risorse e dei servizi documentali forniti dal Sistema Bibliotecario di Ateneo; panoramicadelle nuove modalità di comunicazione scientifica: l’archivio istituzionale di Ateneo OpenstarTs; l’autoarchiviazione delle tesi di dottorato e cenni sull’accesso aperto alla letteratura di ricerca; procedure di conferimento al sito login miur e all’anagrafe di Ateneo (Saperi), University of Trieste, June 30, 2009. “Joint workshop 10th/11 September”, Wittenberg, 2009. “How to write (and manage) a research project”, (Lecturers: Cecilia Blasetti (Elettra), Valter Sergo (UNITS), Maurizio Fermeglia (UNITS)), University of Trieste, October 16, 2009. “Nanotechnology School Annual Meeting 2010”, University of Trieste, January 18, 19 and 20, 2010. Seminar on 'How to present scientific results' (dr. Hanna Mamzer), University of Trieste, January 22, 2010. “Presentation of Nanochallenge and Polymerchallenge by Veneto Nanotech”, University of Trieste, June 15, 2010. “Development of On-line Monitoring devices for the extrusion process” (prof. Miguel Nobrega of the University of Minho in Portugal), University of Trieste, June 15, 2010.. “Use of VPN and UGOV” (prof. Maurizio Fermeglia), University of Trieste, June 15, 2010. “New Approches in Cancer Therapy” (Prof. Konrad Misiura), University of Trieste, May 12, 2011. Seminars (at CRO Aviano): “Dal Focus 2009: aggiornamenti sul carcinoma mammario”, March 25, 2009. “Roles of small RNAs in genome defense”, May 7, 2009. “Seminari in Oncologia al C.R.O. di Aviano”, May 28 and June 4-11-18, 2009. 49 “Matrix revolutions: Perlecan domain V as a novel cancer and stroke therapy” (G. Bix - Texas A&M College of Medicine- USA), September 14, 2009. “Invasion and Metastasis in Breast Cancer”, November 23, 2009. “Bone marrow modelling: new insights regulation of hemopoiesis”, January 13, 2010. “Young investigators event: la due-giorni dei giovani ricercatori dell’IRCCS CRO”, March 10 and 11, 2010. “Targeting tyrosine kinase receptors in solid tumors: the lesson of GISTs”, March 12, 2010. “Connecting the Dots between Tumor Cell Metabolism and Statins as Anti-Cancer Agents”, May 3, 2010. “Recenti progressi in nanomedicina clinica visti da una prospettiva chimico-fisica”, June 8, 2010. “Mechanisms controlling the integrity of replicating chromosomes” (dr. Foiani), June 11, 2010. “Strutturare un protocollo di ricerca” (dr. Foiani), June 11, 2010. “Multidisciplinarità in UroOncologia”, September 10, 2010. “The future of technologies (an overview on research technology)”, October 6, 2010. “Infertilità, gravidanza e tumori”, October 20, 2010. “Seminari in Oncologia: diagnostica, clinica e ricerca”, October 21, 2010, November 4, 2010, November 11, 2010, November 18, 2010, and November 25, 2010. “Incontri finalizzati all’esposizione e alla discussione dei progressi ottenuti nell’ambito dei progetti di ricerca della SOC di FSC” from January 1, 2010 to December 31, 2010. “Mitocondri, calcio e morte cellulare per apoptosi e autofagia”, January 27, 2011. “Introduzione alle nanotecnologie mediche e le loro possibili applicazioni alla medicina clinica” (prof. G. Scoles), February 2, 2011. “Introduzione alla Nanobiologia” (prof. G. Scoles) on February 2, 2011. “Ruolo del complemento nel controllo dello sviluppo tumorale”, February 4, 2011. “Le associazioni per pazienti oncologici in Europa: il CRO incontra Jan Geissler”, February 16, 2011. “Regulation and dysregulation of the p53 network and its role in breast cancer”, May 31, 2011. “Targeting cancer stem cells the NGAL: MMP9 connection”, June 8, 2011. “Nuovi approcci molecolari farmacogenetici, immunogenetica, proteomici e metabolomici nella ricerca farmacologica”, from January 1, 2011 to June 30, 2011. “Role of the Hippo pathway effectors YAP and TAZ in mechanotransduction, cell polarity and cancer stem cells”, May 15, 2012. 50 “Reversal of glucocorticoid resistance by AKT inhibition in T-ALL”, May 24, 2012. “Aberrant PI3K signalling in lung cancer: from man to mouse and back again”, July 12, 2012. Conferences “Congresso Nazionale della Società Italiana di Chemioterapia”, Udine, October 14, 2009. “Trasferimento Tecnologico. Dinamiche spiegate tramite Case Study, la Brevettazione in Biomedicina e Biotecnologie”, April 19, 2011. “DAL FOCUS 2011 SUL CARCINOMA MAMMARIO: assistenza e ricerca clinica in oncologia”, April 29, 2011. “Young Investigators Event II: la due-giorni dei giovani ricercatori dell'IRCCS CRO”, May 3-4, 2011. “Carcinoma del retto: approccio multidisciplinare, terapie integrate” on May 27, 2011 Courses (at CRO of Aviano): “Corso di lingua inglese” (Shenker Institute), Pordenone, from January to July 2009. “RefWorks: creare DataBase Bibliografici personali”, May 7, 2009. “REFERENCE MANAGER: uno strumento straordinario per ottimizzare la gestione delle bibliografie”, May 19 and 26, 2009. “BLSD - Corso teorico pratico di Basic Life Support and Defibrillation”, September 22, 2009. “L'informazione scientifica in un IRCCS oncologico: formazione all'uso delle risorse informative rese disponibili dalla Biblioteca del CRO, Bibliosan”, September 29, 2009. “L'operatore sanitario e la comunicazione in sanità: Power Point come strumento informatico per presentazioni efficaci”, February 3 and 9, 2010. “Corso di inglese scientifico livello avanzato”, May 6, 13, 20, 27, June 3, 10, 17, 24, September 30, October 7, 14, 21, 28, November 4, 11, 2010. “L’operatore sanitario e la gestione dei dati alfa-numerici: Excel come strumento per elaborare e visualizzare efficacemente le informazioni”, November 24, December 1 and 7 2010. Support educational activity and teaching • two hours of class teaching of Pharmacology Oncology of the degree course in “Biotecnologie Mediche”, University of Trieste, January 15, 2009: “Gli inibitori della farnesiltransferasi” e “Il proteasoma: ubiquitina e Bortezomib” 51 Dottorandi del 26 ciclo: DAMIANO CASSESE Title of the thesis:Design and realization of nanoelectromechanical and plasmonic devices for Raman spectro-microscopy Supervisor: Marco Lazzarino Tutors (if any): Research Activity During the first year, the following research activities were carried: • Design: FEM simulation were performed with COMSOL software to study the development of a cantilever chip capable of high temperature heating (>400oC) in a small area (<2 micrometers), to localize the nanowires growth. Following the result obtained, an optical mask for the chip fabrication was designed with Ledit software. • Fabrication: the chip fabrication was begun, even though further analysis of structure compensation in wet etching is needed. Nanowires growth has been achieved on silicon oxide in PECVD; some tests of growth with MBE are underway. • Raman spectroscopy: the Raman spectroscopy setup was optimized and the optical components aligned. Some spectra of various samples of interest (graphene, AlGaAS nanowires, carbon nanotubes) were taken along with Raman maps aat the micro-scale using an Andor Technologies spectrograph coupled with JPK AFM movement stage and a ZEISS inverted microscope. Objectives for the following year (if applicable) In the following year we aim to produce the chips with the cantilevers integrated; following the optimization of the nanowires growth process, the complete devices will be produced. The chips will be tested, to confirm their TERS potentiality and their behaviour as AFM cantilevers. We will also focus on raman spectroscopy and maps of samples, both using micro-Raman and TERS, Educational Activity Classes followed (date, course, professor, type of course) z Intense course on “Molecular self-assembling and nanostructures”, held by A. Morgante, L. Casalis, L. Pasquato, 21/06/2011 – 18/07/2011 z Winter collage in Optics: advances in nano-optics and plasmonics (and preparatory school) at ICTP, to be held from 30th of January till 17th of February Conferences, seminars, advanced courses and other didactic activities • Massimiliano Di Ventra (Department of Physics University of California, San Diego), “Fast DNA sequencing: a physicist’s perspective”, seminar at SISSA – Condensed Matter department • Workshop on "Circulating Tumor Cells", 7th November 2011, Udine 52 • • • • Conference Monalisa’s Quidproquo “Nanotechnology Meets Clinical Medicine", October 6-8, 2011, Aviano/Udine Summer school of Nanotechnology, Trieste, September 20-23 Konrad Misiura, ‘New Approches in Cancer Therapy’, Trieste János Kristóf and Erzsébet Horváth, “Synthesis and structure elucidation of kaolinite organo-complexes”, May 12 2011 53 STEFANIA CORVAGLIA Titolo della tesi: Modellare substrati su scala nanometrica per la caratterizzazione di singole cellule Supervisore: dr. Loredana Casalis, dr. Denis Scaini Tutori (eventuali): Attività di ricerca La ricerca in ambito biomedico dei meccanismi molecolari di patologie come il cancro ha rivelato come i tessuti malati provenienti da biopsie presentino una distribuzione spaziale molto eterogenea di popolazioni di cellule tumorali all’interno dello stesso campione che lasciano supporre differenze sostanziali anche tra singole cellule. Le tecniche attuali riescono al meglio ad estrapolare dati mediando su campioni di qualche centinaio di cellule e sono perciò insensibili alle variazioni a livello di singola cellula. Per questo, abbiamo come obiettivo lo sviluppo di una nuovo metodologia che ci permetta di isolare e caratterizzare decine di singole cellule dal punto di vista del contenuto proteico (secretoma/proteoma) e di farne un’analisi statistica. Abbiamo sviluppato un array di micropozzetti delle dimensioni di una singola cellula, con lo scopo di immobilizzare le cellule in un volume piccolo che aumenti la concentrazione di proteine rare. Per la detection della proteine stiamo lavorando allo sviluppo di un nano/microarray di anticorpi specifici, prodotto utilizzando una litografia AFM-mediata (Nanografting), a chiusura del pozzetto per l’analisi di specifiche proteine, biomarkers significativi dello stato della cellula. In questo primo anno di dottorato ho lavorato alla realizzazione degli array di micropozzetti, con particolare attenzione alla scelta del materiale più adatto alla crescita di cellule, allo studio dell’influenza delle proprietà meccaniche del materiale sull’adesione e la crescita, all’intrappolamento all’interno del pozzetto di singole/poche cellule e alla chiusura del pozzetto per l’analisi. Sto testando il sistema utilizzando un modello cellulare semplice e facilmente reperibile (linea tumorale HeLa) che faciliti l’applicazione futura a sistemi d’interesse medico. Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) - SIBBM Frontiers in molecular Biology, Trieste, Italy- poster abstract_26-28 maggio 2011; - EBSA 8th European Biophysics congress, Budapest, Ungheria- poster abstract, 23-27 agosto 2011; - CFN Summer School on Nano-Biology, Karlsruhe, Germany- poster abstract, 7-10 settembre 2011; - Summer school of Nanotechnology, Trieste, Italy- poster abstract, 20-23 settembre 2011; - ICTP Conference on Nanotechnology for Biological and Biomedical Applications (Nano-Bio-Med), Trieste, Italy- poster abstract, 10-14 ottobre 2011 54 Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) - 21 giugno 2011- 15 luglio 2011, corso "Molecular self-assembling and nanostructures" Lucia Pasquato, Alberto Morgante and Loredana Casalis Congressi, seminari, corsi avanzati e altre attività didattiche passive -17-19 gennaio 2011, congressino nanotecnologie, Scuola di dottorato in Nanotecnolgie, università di Trieste, Trieste, Italy ; -2 febbraio 2011 workshop biomol @ ELETTRA Seminari: -10 febbraio Zehra Sayers, “Structural and functional studies on plant metallothioneins and heteromeric G-proteins”; -1 aprile Filippo Lutisani, “Single molecule fluorescence microscopy: new insights”; -7 aprile Ario de Marco “Application opportunities for single domain antibodies”; - 3 maggio -11 maggio Alessandro Laio “Colloquium on condensed matter physics: Exploring the universe of protein structures beyond the protein data bank”. -12 maggio Konrad Misiura, “New approaches in cancer therapy” -13 maggio Giacinto Scoles, “The importance of numbers (with units) and common sense: the inevitability of solar energy for the resolution of energy need”. -21 giugno Massimiliano di Ventra, “Fast DNA sequencing: a physicist’s perspective”; -1 luglio Hlcham Hmamoudi “Self assembled on gold the challenge” -6 luglio Flavio Maran “Superefficient electron transfer trought 310 –helical peptides” 55 VALENTINA DAL COL Titolo della tesi: In silico prediction of drug resistance: from cancer targeted therapy to cancer targeted prevention Supervisore: Prof.ssa Sabrina Pricl Tutori (eventuali): Prof. Maurizio Fermeglia Attività di ricerca Le recenti scoperte sulla natura dei processi genetici, implicati nelle trasformazioni neoplastiche, hanno permesso di identificare le lesioni cellulari che promuovono il cancro, individuando target selettivi per la progettazione di nuovi agenti terapeutici efficaci. Durante questo primo anno il mio studio si è focalizzato su due diversi sistemi recettoriali: il recettore tirosin chinasico c-Kit e il recettore σ1. Per il primo sistema si è andati a studiare, attraverso tecniche di simulazione molecolare, i cambiamenti strutturali che coinvolgono il dominio JXM (juxtamembrane) del c-Kit in seguito a due differenti mutazioni geniche: Δ559-560 e V560G. Queste modificazioni portano ad una diversa interazione tra il farmaco d’elezione (Imatinib) e la tasca di binding recettoriale. Si è visto che la mutazione di delezione (Δ559560) conduce ad uno shifting dell’equilibrio verso la forma attiva della chinasi mentre la missense (V560G), andando ad alterare la conformazione del dominio JXM, permette una migliore interazione dell’Imatinib con il recettore nella sua conformazione chiusa. Si è inoltre sviluppato un modello predittivo 3D, per omologia, del recettore σ1, per il quale è mancante una struttura cristallizzata. E’ stata utilizzata una procedura multistep: sviluppo e ottimizzazione della struttura 3D, identificazione del possibile sito di binding, docking di una serie di ligandi, conseguente calcolo dell’energia libera di binding così da confrontare i risultati con i valori sperimentali e, alla fine, verifica della capacità predittiva utilizzandolo per il design di una nuova classe di composti. L’obiettivo finale è renderlo, dopo ulteriori validazioni, uno strumento per il design di ligandi altamente selettivi e per comprendere meglio le interazioni che il recettore instaura con altri sistemi biologici. Pubblicazioni su riviste scientifiche (pubblicate oppure in stampa), •“2-Difluoromethylene-4-methylenepentanoic acid, a paradoxical probe able to mimic the signaling role of 2-oxoglutaric acid in Cyanobacteria” Liu X, Laurini E, Dal Col V, Posocco P, Ziarelli F, Fermeglia M, Zhang CC, Pricl S, Peng L Organic Letters, Jun 3; 13(11):2924-7 •“Homology model and docking-based virtual screening for ligands of the σ1 receptor” Laurini E, Dal Col V, Mamolo MG, Zampieri D, Posocco P, Fermeglia M, Vio L, Pricl S ACS Med Chem Lett 2011, 2: 834-839 •“Activate and respond. A molecular rationale for c-kit activation and drug response by juxtamembrane mutations in GISTs” Dal Col V et al. Mol Cancer Ther 2011 submitted 56 •“Activity vs. toxicity of acridine compounds as anti-BVDV agents: a molecular modeling study” Dal Col V et al. Antiviral Res 2011 submitted Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) •Comunicazione a VNPCF Trieste 2011 28-30 marzo “The long and winding road of the c-Kit JXM domain” Dal Col V et al. •Comunicazione a VNPCF Trieste 2011 28-30 marzo “Overview on σ1 receptors: a 3D homology model to solve a part of the enigma” Dal Col V et al. •Comunicazione a CDDD L’Aquila 2011 21-23 novembre “Nanozapped! DNA, siRNA, and their dendritic nanovectors: a combined in silico/in vivo/in vitro approach” Dal Col V et al. •Comunicazione a CDDD L’Aquila 2011 23-25 novembre “The Sigma-Enigma. A multistep homology modeling of σ1 receptors” Dal Col V et al. Comunicazione a Nanotechitaly 23-25 novembre 2011 “Trekking across GISTs: the clinical journey of KIT, PDGFRA, and the in silico prediction of drug resistance in cancer targeted therapy” Dal Col V et al. Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) 60 ore laboratorio MOSE Scuole AMBER school 3-6 maggio 2011 Barcellona Summer school on Nanotechnology 20-23 settembre Trieste COST Training school 2011 (Dendrimers as composites of advanced drug delivery nano systems) Atene 3-7 ottobre 2011 Congressi, seminari, corsi avanzati e altre attività didattiche passive Congressi VNPCF (Vcongresso nuove prospettive in chimica farmaceutica) Trieste 28-30 marzo 2011 CDDD (Computationally driven drug discovery) L’Aquila 21-23 novembre 2011 Seminari “Brached Peptides as Therapeutics” Prof. Bracci 21 marzo 2011 “Challenging the mistery of marine toxins” Prof. Yasumoto 15 aprile 2011 “New approaches in cancer therapy” Prof. Misiura 12 maggio 2011 “Nanosistemi per il drug e il gene delivery a base di derivati dell’acido aspartico” Prof. Cavallaro 1 giugno 2011 “Self assembled monolayers the Challenge” Dr. Hicham Hamoudi 1 luglio 2011 “The effect of confinement on enzyme diffusion and reaction inside DNA nanostructures” Dr. Castronovo 29 luglio 2011 57 Corsi “Molecular self- assembling and nanostructures”, Prof. Morgante, Casalis, Pasquato Periodo 21/06-29/07/2011 Altre attività didattiche passive Congresso dottorandi Scuola di Nanotecnologie 17-19 gennaio 2011 Presentazione delle attività scientifiche dei gruppi di ricerca del dipartimento DI3 25 febbraio 2011 58 ANDREA FRASSETTO Title of the thesis: Nanostructural analysis of the adhesive interface in dentistry Supervisor: Prof. Milena Cadenaro Tutor: Prof. Lorenzo Breschi Research Activity The first part of the program was focused on the literature review of the adhesive layer degradation and nanoleakage development and on laboratory training, including an accurate analysis at SEM of the interaction of different adhesive systems with the dentin substrate, by the application of adhesive agents on human dentin surfaces, then stored in appropriate in vitro conditions to simulate the oral environment for different time intervals in order to assess nanoleakage expression. Despite acceptable immediate bonding effectiveness of dental adhesives, the durability of resin bonded interface on dentin created by several bonding systems remains questionable. All the commercial adhesives tested presented nanoleakage phenomena after 6 months of aging in artificial saliva. Thus the intrinsic degradation mechanisms originated from beneath dentine hybrid layer by the slow action of matrix metalloproteinases (MMPs) was investigated. The release and activation of these endogenous enzymes during bonding to dentin are thought to be responsible for the in vitro and in vivo manifestation of thinning and disappearance of collagen fibrils from incompletely infiltrated hybrid layers in aged, bonded dentine. Collagen degradation generates several collagen fragments; one of them (ICTP) was quantified by means of commercialized immunoassays. Moreover the loss of mechanical properties of dentinal collagen was correlated, in particular the biaxial flexural modulus of elasticity (EBF). Evaluation of both collagen denaturation and E-modulus could lead to a more clear understanding of the durability of adhesive systems and nanoleakage development. Objectives for the following year (if applicable) • Analysis of new inhibitors of the enzymatic activity of dentin endogenous matrix metalloproteinases (MMPs) • Influence of collagen cross-linkers in the inhibition of MMPs’ activity and subsequent increase of mechanical properties of the adhesive layer Publications on scientific journals (printed or in press) • Frassetto A, Navarra CO, Marchesi G, Turco G, Di Lenarda R, Breschi L, Ferracane JL, Cadenaro M. Contraction stress and degree of conversion of selfadhesive resin cements. Dental Materials, submitted. Publications/abstracts in conferences/congresses (national or international) •Stress of polymerization of a new self-adhesive vs a conventional dual-cured cement. XVII National Meeting of the College of Dentistry Teachers, Siena. 59 • Stress of polymerization and degree of conversion of two self-adhesive vs a conventional dual-cured cement. 21st European Dental Materials Conference; Turku (FI). • Microtensile bond strength test of four self-etch commercial adhesives. 21st European Dental Materials Conference; Turku (FI). • Influence of chewing simulation on bond strength of cemented composite-disks. Dent Mater 2011; 27s: e8. • Effects of 6-month water storage on micro-tensile bond strength of self-etch adhesives. Dent Mater 2011; 27s: e10. • Influence of chewing simulation on bond strength of cemented ceramicdisks. Dent Mater 2011; 27s: e24. Participation to conferences (as speaker) • Firenze-Siena 14-16 April 2011; XVII National Meeting of the College of Dentistry Teachers. Poster Presentation, Stress of polymerization of a new selfadhesive vs a conventional dual-cured cement. Educational Activity Periods abroad (date and place) • San Diego (USA) 16-19 March 2011 • Augusta (USA) 20-22 March 2011 • Seili-Turku (FI) 22-26 August 2011 • Salvador (BR) 13-15 October 2011 Classes followed (date, course, professor, type of course) • Course of Material Sciences, CLSOPD II Semester, Prof. L. Breschi • Course of Adhesive Dentistry, CLSOPD II Semester, Prof. L. Breschi Conferences, seminars, advanced courses and other didactic activities • Trieste 17-20 January 2011; Annual Meeting of the PhD School in Nanotechnology • San Diego (USA) 16-19 March 2011; Annual Meeting of the International Association of Dental Research • Augusta (USA) 21-22 March 2011; Research Stage at Medical College of Georgia (Prof. D. Pashley) • Trieste 8 April 2011; PhD Final Dissertations of School in Nanotechnology 60 • Firenze-Siena 14-16 April 2011; XVII National Meeting of the College of Dentistry Teachers • Trieste 12 May 2011; Seminar of Prof. K. Misiura: New Approaches in Cancer Therapy • Trieste 1 July 2011; Seminar of Dr. H. Hamoudi: Self assembled monolayers on gold the challenge • Trieste 4-8 July 2011; FVG Summer School/Workshop on Structural Bioinformatics • Trieste 12 July 2011; Seminar of Prof. S.-W. Hla: Nanoscience at Work: Imaging and Manipulation at Atomic and Molecular Scale • Seili (FI) 22-24 August 2011; Dental Materials Summer School • Turku (FI) 24-26 August 2011; European Dental Materials Conference • Trieste 15 September 2011; Seminar of Dr. G. Forte: Adult Stem Cell and Thermo-responsive Polymers for Cardiac Muscle Tissue Engineering • Trieste 20-23 September 2011; Summer School of the PhD School in Nanotechnology • Salvador (BR) 13-15 October 2011; Annual Meeting of Academy of Dental Materials • Bologna 18-19 November 2011; Annual Meeting of Italian Academy of Prosthetic Dentistry • Milano 25-26 November 2011; Annual Meeting Expo Dental 61 ELISA MINIUSSI Titolo della tesi: Interaction of metal nanoclusters with graphene and low dimensional systems Supervisore: Dr. Alessandro Baraldi Tutori (eventuali): Attività di ricerca Il mio progetto di Dottorato verte sulla produzione e caratterizzazione di nanocluster metallici depositati su opportune superfici solide, in modo particolare sul grafene cresciuto epitassialmente su diversi substrati. La mia attività si articola dunque essenzialmente su due versanti: la crescita epitassiale del grafene e lo sviluppo di una macchina per la produzione e deposizione di nanocluster selezionati in massa. Sul primo fronte, un risultato di rilievo è stato recentemente ottenuto con la pubblicazione su Physical Review Letters di uno studio, iniziato durante la mia tesi specialistica, sul grafene cresciuto epitassialmente su un nuovo substrato, un cristallo singolo di Re(0001). È noto che la forza di interazione tra il grafene e il substrato determina la corrugazione del layer di carbonio, che a sua volta è responsabile delle proprietà di trasporto sia elettronico che termico di quest’ultimo. Le nostre ricerche hanno evidenziato una diretta correlazione tra la forte corrugazione del grafene su questo substrato e la sua instabilità ad alte temperature. È stato inoltre intrapreso lo studio di un nuovo sistema, il grafene cresciuto epitassialmente su una lega di superficie PtRu, finalizzato a comprendere come variando la concentrazione di Pt nel primo layer sia possibile modificare selettivamente l’accoppiamento grafene-substrato, e di riflesso le proprietà morfologiche ed elettroniche del sistema. In parallelo, sono iniziati i lavori di assemblaggio della sorgente di nanocluster presso il laboratorio di Fisica delle Superfici (Dipartimento di Fisica dell’Università di Trieste e Laboratorio TASC (IOM-CNR)). Nell’ambito di questo progetto ho trascorso quattro mesi con una borsa Erasmus Placement presso il Dipartimento di Chimica Fisica della Technische Universität di Monaco di Baviera (TUM), dove questa tecnologia è stata sviluppata allo stato dell’arte nel corso degli ultimi anni. In questo modo ho potuto apprendere i principi di funzionamento e le modalità operative delle sorgenti e della strumentazione scientifica utilizzata in combinazione con esse. Ho successivamente sfruttato le conoscenze così acquisite per portare a termine la fase preliminare di assemblaggio della macchina. Pubblicazioni su riviste scientifiche (pubblicate oppure in stampa) E. Miniussi, M. Pozzo, A. Baraldi, E. Vesselli, R. R. Zhan, G. Comelli, T. O. Menteş¸ M. A. Niño, A. Locatelli, S. Lizzit, and D. Alfè, “Thermal Stability of Corrugated Epitaxial Graphene Grown on Re(0001)”, Phys. Rev. Lett. 106, 216101 (2011). Altre pubblicazioni 62 E. Miniussi, M. Pozzo, A. Baraldi, E. Vesselli, R. R. Zhan, G. Comelli, T. O. Menteş¸ M. A. Niño, A. Locatelli, S. Lizzit, and D. Alfè, “A link between corrugation and thermal stability of epitaxial graphene”, Elettra Highlights 2010-2011, pagg. 66-67. Partecipazione a congressi (come relatore) Presentazione orale del seminario intitolato: “A link between corrugation and thermal stability of epitaxial graphene”, in occasione dell’assegnazione del premio Fonda-Fasella 2011 conferitomi durante il workshop “Nanoenergetics: theoretical and experimental approaches” (Trieste, 15-16 Novembre 2011). Attività formativa Periodi di permanenza all’estero (data e Sede) Borsista Erasmus Placement dal 1 aprile 2011 al 31 luglio 2011 presso il Dipartimento di Chimica Fisica della Technische Universität di Monaco di Baviera (TUM) (tutori presso l’istituzione ospitante: Prof. U. Heiz e Dr. F. Esch). Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) “Physikalische Chemie von Nanoteilchen und Oberflächen” (Chimica Fisica delle Nanoparticelle e Superfici) http://www.pc.ch.tum.de/index.php?id=193 - Docenti: Dr. F.Esch, Prof. U. Heiz - Numero di ore: 40 Contenuti: Introduzione alla Chimica Fisica dei cluster: transizione dagli oggetti di dimensioni atomiche ai solidi di bulk; fabbricazione dei cluster, loro proprietà fondamentali e caratterizzazione sperimentale (diffrazione, spettroscopia, microscopia); cluster elementari ed eterogenei, cluster supportati e loro proprietà catalitiche. Congressi, seminari, corsi avanzati e altre attività didattiche passive Seminar at Elettra: Optical and Dynamical Properties of Hydrogen Bonded Systems Nadja Doslic, Department of Physical Chemistry, University of Zagreb 10 Febbraio 2011, Seminar Room (Elettra) Seminar at Elettra: X-Ray absorption spectroscopy and science at extreme conditions: previous results and new opportunities for the XAFS beamline at Elettra Giuliana Aquilanti, Sincrotrone Trieste 14 Marzo 2011, Seminar Room (Elettra) Seminar at Elettra: Images of excited states Giovanni Piani, Laboratoire Francis Perrin, CEA Saclay, France. 14 Marzo 2011, Seminar Room (Elettra) Seminar at Elettra: Electronic Properties of Functionalized Quasi-Free-Standing Graphene and Monolayer Boron Nitride Danny Haberer, IFW Dresden, Dresden, Germany 21 Marzo 2011, Seminar Room (Elettra) 63 Joint Workshop on Energy and Sustainability: Materials and Processes Chemistry Department, Northwestern University, and Catalysis Research Center, Technische Universität München Institute for Advanced Study (IAS) Technische Universität München, Lichtenbergstr. 2a, 85748 Garching, Germany 13-14 Maggio 2011 4. Joint Nanoworkshop of TU/e, DTU and TUM TUM Institute for Advanced Study (IAS) TUM Campus Garching 1 Giugno 2011 DFH/UFA Photokat Workshop 2011: Photokatalytische Eigenschaften von Nanostrukturen / Propriétés photocatalytiques des structures nanométriques IAS Building, TUM Campus 14-15 Luglio 2011 XI School on Synchrotron Radiation: Fundamentals, Methods and Applications Duino Castle, Trieste, Italy 5-16 Settembre 2011 First Joint Summer School on Nanotechnology Università di Trieste, Campus di Piazzale Europa 20-23 Settembre 2011 Seminar at Elettra: Adventures in Catalytic Nanospace: resolving catalytic phenomena at the atomic scale Michael Bowker, Wolfson Nanoscience Laboratory and Cardiff Catalysis Institute, School of Chemistry, Cardiff University, Wales, UK. 2 Novembre 2011, Seminar Room (Elettra) Workshop on Nanoenergetics: theoretical and experimental approaches ICTP, Adriatico Guesthouse, Trieste, Italy 15-16 Novembre 2011 Seminar at Elettra: Probing ultrafast symmetry changes with light Simon Wall, Department of Physical Chemistry, FHI (Berlin) 25 Novembre 2011, Seminar Room (Elettra) Seminar at Elettra: XAFS at Elettra: recent achievements and future projects Giuliana Aquilanti, Sincrotrone Trieste 1 Dicembre 2011, Seminar Room (Elettra) Attività didattica di supporto e attività didattica attiva Lettura di articoli e review su argomenti attinenti alla mia attività di ricerca, in particolare: studio sperimentale e teorico delle proprietà del grafene (in generale), crescita del grafene su 64 diversi substrati solidi e sua caratterizzazione, nano cluster metallici e investigazione della loro morfologia, proprietà elettroniche e reattività. 65 ELISA MITRI Titolo della tesi: Fabbricazione di dispositivi microfluidici per lo studio della risposta biologica di cellule vive sottoposte a stimoli chimico-fisici mediante tecniche di microspettroscopie vibrazionali Supervisore: Massimo Tormen Tutori: Gianluca Grenci, Lisa Vaccari Attività di ricerca La microspettroscopia infrarossa (MIRS) è considerata tra i più promettenti metodi per lo screening medico e diagnostico, grazie alle informazioni strutturali e conformazionali, contenute in uno spettro infrarosso. Lo studio di cellule vive tramite MIRS richiede l'utilizzo di un set-up microfluidico trasparente all'IR, capace di mantenere le condizioni necessarie alla vita delle cellule. Negli anni scorsi presso il mio gruppo è stata messa a punto una piattaforma microfluidica su finestre di CaF2 (materiale trasparente all'IR). Il dispositivo è stato testato con successo presso la beamline SISSI (Elettra, Trieste). Nel mio primo anno di dottorato ho lavorato all'ottimizzazione del set-up con l'intento di risolvere i problemi emersi nei precedenti esperimenti, tra cui: • Scarsa aderenza del resist durante il processo fabbricativo dovuto alla bassa energia superficiale del CaF2 (30-50 mJ/m2). • Effetti sconosciuti del CaF2 sulle linee cellulari (es neuroni) • Protocollo di chiusura del dispositivo In riferimento ai punti 1 e 2, abbiamo modificato le proprietà superficiali del CaF2 tramite sputtering di un sottile strato di Silicio. Questo approccio porta i seguenti vantaggi: • Possibilità si operare il processo litografico su un substrato Si-like Assenza di contatto tra cellule e CaF2 • Per migliorare il protocollo di incollaggio si propone un nuovo metodo che sfrutta la quantità di solvente residuo nel resist per promuovere l'adesione e la protezione dell'ambiente in cui si confineranno le cellule. Per dimostrare la validità del nostro approccio abbiamo condotto una serie di studi, monitorando diverse linee cellulari (MCF-7, HCT116) all'interno del dispositivo per intervalli di tempo fino a 48 ore. Pubblicazioni/abstracts in conferenze/congressi “Optimization of Microfluidic Systems for IRMS real Time Monitoring of Living Cells” Gianluca Grenci1, Giovanni Birarda1, Elisa Mitri1, Luca Businaro2, Sabrina Pacor3, Lisa Vaccari4, Massimo Tormen1 1CNR-IOM, Laboratorio TASC – Lilit beam line, Basovizza/Italy, 2 CNR ISTITUTO DI FOTONICA E, ROMA/Italy, 3 Life Science Dept., Trieste University, Trieste/Italy, 4 Elettra Synchrotron Light Laboratory, SISSI beam line, Basovizza/Italy “Microfluidic devices for real-time infrared imaging of living cells” G. Birarda1, G. Grenci2, L. Businaro3, E. Mitri2, M. Tormen2, S. Pacor4 and L. Vaccari1 66 1 Elettra Synchrotron Light Laboratory, ITALY, 2 IOM - CNR, ITALY, 3 Istituto di Fotonica e Nanotecnologie, ITALY, and 4 Trieste University, ITALY Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite “Nanotecnologie e nanomicroscopie” (60 h 7,5 CFU laurea specialistica in biotecnologie mediche) Carlo Dri - Gianluca Grenci “Biologia Cellulare Animale” (48 h, 5 CFU laurea magistrale in chimica e tecnologie farmaceutiche) Sabrina Pacor Congressi, seminari, corsi avanzati e altre attività didattiche passive Seminari "Synthesis and structure evaluation on kaolinite Organo-Complexes" Prof. Janos Kristof – Dr. Elisabeth Horvath 03/05/11 “Self assembled monolayers on gold the challenge” Dr. Hicham Hamoudi “” Dr. Matteo Castronovo Congressi Congresso annuale della scuola 17-19 gennaio 2011, Trieste Conferenze Wirms 2011 - 6th International Workshop on Infrared Spectroscopy and Microscopy with Accelerator-Based Sources – 4-9 settembre 2011, Trieste MNE 2011- 37th International Conference on Micro and Nano Engineerin – 19-23 Settembre 2011 Berlino 67 GIUSEPPINA PALMA Titolo della tesi: Celle solari dye-sensitized nanostrutturate Supervisore: Alessandro Fraleoni Morgera Tutori (eventuali): Attività di ricerca Le attività di ricerca del primo anno di dottorato possono essere riassunte in tre punti fondamentali: 1) Comprensione generale dello stato dell’arte relativo alla fabbricazione ed ottimizzazione di celle solari a colorante organico; 2) Messa a punto del set up di caratterizzazione che consiste in un sistema di misura di curve I/V e uno di efficienza quantica; 3) fabbricazione di dispositivi come da letteratura e studio preliminare di metodi per lo sviluppo di uno strato semiconduttore altamente poroso da impiegare nelle celle suddette per aumentarne l’efficienza. Il punto 1) è stato perseguito mediante uno screening approfondito della letteratura del settore e la frequenza di una scuola internazionale dedicata al settore fotovoltaico. Il punto 2) è stato sviluppato dapprima attraverso la frequenza di un corso base di programmazione in Labview, strumento utilizzato per realizzare i software di guida di un set up di caratterizzazione I/V, costituito da un simulatore solare accoppiato ad un multimetro, e di un sistema di determinazione di efficienza quantica. Il punto 3) è stato perseguito cercando di riprodurre le prestazioni delle DSSC riportate in letteratura, che raggiungono l’11% di efficienza. Attualmente la realizzazione di dispositivi altrettanto validi non è stata ancora raggiunta, dato che il lavoro effettivo sui dispositivi è iniziato a partire da Settembre 2011. In particolare, ad oggi i parametri di fill factor e Voc delle celle realizzate sono in linea con i valori dei dispositivi stato dell’arte, mentre la corrente estraibile dal circuito è ancora scarsa. Questo problema verrà affrontato introducendo uno strato compatto di TiO2 tra l’anodo e lo strato semiconduttore mesoporoso, così da reprimere il forte processo di ricombinazione locale; inoltre verrà caricata una maggiore quantità di colorante sullo strato mesoporoso attraverso un processo di multidipping. Inoltre ottimizzazioni dello spessore dello strato nano cristallino e della struttura generale dei dispositivi (contro-elettrodo, elettrolita, isolamento dall’ambiente esterno, ecc) dovrebbero portare ad aumentare l’efficienza globale dei dispositivi, attualmente ferma allo 0.7%. Studi preliminari sull’utilizzo della metodologia ASB-SANS (Auxiliary Solvent-Based Sublimation-Aided NanoStructuring) per incrementare l’efficienza delle celle, attraverso l’aumento di porosità dello strato nanocristallino di TiO2, sono in corso. Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) • 19-23 Settembre 2011: Nanotech Summer School; Trieste, poster session • 17-21 Ottobre, 2011: Workshop on New Materials for Renewable Energies, ICTP, Trieste, poster session 68 Attività formativa Periodi di permanenza all’estero (data e Sede) • 11-18 Settebre 2011: Quantsol Summer School; Hirschegg (Austria) Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) • 7 Aprile- 5 Maggio 2011: Corso base di Labview, G. Cautero, corso di formazione presso Elettra (16h) • 21 Giugno- 15 Luglio 2011: Summer course on Molecular self-assembling and nanostructures (docenti: L. Casalis (8h), A. Morgante (6h), L. Pasquato (6h)) Congressi, seminari, corsi avanzati e altre attività didattiche passive • 17-19 Gennaio 2011: Workshop sulle nanotecnologie (Università di Trieste) • 03 Maggio 2011 ore 10: Seminario Nanotech: Synthesis and structure elucidation of kaolinite organo-complexes (János Kristóf and Erzsébet Horváth, University of Pannonia, Institute of Environmental Engineering, Hungary) • 03 Maggio 2011 ore 14: Seminario Elettra: The unusual physics of Dirac fermions in graphene (Alessandra Lanzara, University California, Berkeley) • 13 Maggio 2011 ore 15: Seminario Elettra: The importance of numbers (with units) and common sense: the inevitability of solar energy for the resolution of energy needs (Giacinto Scoles, University of Udine, Faculty of Medicine, Department of Medical and Biological Sciences, Ospedale di S. Maria della Misericordia in Udine, Italy. • 27 Maggio 2011: Celle solari polimeriche e dye-sensitized (Alessandro Fraleoni Morgera, Sincrotrone Trieste) • 29 Luglio 2011: ‘The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA Nanostructures’ (Matteo Castronovo) • 1 Luglio 2011 ‘Self assembled monolayers on gold the challenge’ Dr. HIcham Hmamoudi (Université-Paris Sud) • 19-23 Settembre 2011: Nanotech Summer School; Trieste (Italia) • 17-21 Ottobre 2011: Workshop on New Materials for Renewable Energies, ICTP, Trieste, Italy 69 ANDREA RADIVO Titolo della tesi: Studio sperimentale della fisica di dispositivi fotovoltaici organici nano strutturati. Supervisore: Massimo Tormen Tutori : Simone Dal Zilio, Enrico Sovernigo Attività di ricerca In questo primo anno ho concentrato la prima parte del mio lavoro sull’acquisizione delle conoscenze necessarie al progetto e sulla messa a punto di procedure di preparazione e caratterizzazione di celle fotovoltaiche organiche. A tal fine, ho quindi prodotto e caratterizzato celle fotovoltaiche aventi un'interfaccia planare tra strati donore ed accettore, utilizzando diverse combinazioni di materiali. In una seconda parte del mio lavoro, ho elaborato un processo per produrre celle fotovoltaiche organiche aventi un'interfaccia nano strutturata con una struttura interdigitata di materiali donore ed accettore, conformazione che viene considerata in letteratura come ottimale al fine di incrementarne il rendimento. Ho scelto, come materiali attivi diverse coppie di piccole molecole organiche e fullereni ampiamente trattate in letteratura, e come tecnica di nano strutturazione a costo contenuto, il nanoimprinting. La categoria di materiali in esame offre un’ampia gamma di possibili coppie di materiali dalle diverse proprietà optoelettroniche, tuttavia pochi di questi sono risultati adatti al nanoimprinting diretto. Ho quindi scelto un approccio indiretto: nanoimprinting del substrato PEDOTT-PPS, utilizzato come conduttore/collettore di lacune e facilmente stampabile, ottenendo una struttura a righe con diversi periodi e larghezze; deposizione di uno strato conformale di materiale donore per evaporazione; riempimento delle strutture rimanenti mediate deposizione da soluzione o evaporazione del materiale accettore; evaporazione del contatto in alluminio per terminare la cella. Ho applicato questa procedura a diversi materiali, ed i migliori risultati sono stati ottenuti con la coppia Pentacene-PCBM. E’ stato infatti possibile depositare il pentacene in modo quasi conformale sul substrato nanostrutturato in PEDOT:PPS e riempire in modo apparentemente completo e con poche porosità le strutture, con PCBM depositato da soluzione, ottenendo così una struttura interdigitata dei due materiali. Obbiettivi da raggiungere per l’anno successivo: Gli obbiettivi per il prossimo anno di lavoro si possono articolare in: • Affinare i processi di produzione per avvicinarsi allo stato dell’arte nella qualità e rendimento delle celle planari; • Proseguire con lo sviluppo delle celle nano strutturate in pentacene PCBM e trovare altri materiali per cui il medesimo approccio sia possibile; • Sviluppare nuovi sistemi di nano strutturazione delle celle fotovoltaiche organiche; 70 • Caratterizzare approfonditamente le celle prodotte per determinare l’effetto della variazione di processi, strutture e materiali, sul rendimento e le proprietà optoelettroniche della cella; Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) •Poster alla Summer school di nanotecnologie. Titolo del poster: Experimental Study of the physics of nanostructured organic photovoltaic devices. Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite: Formazione in laboratorio all’utilizzo di strumenti di caratterizzazione e fabbricazione celle fotovoltaiche presso laboratorio TASC e Elettra. In particolare: •Caratterizzazione: formazione per l’utilizzo autonomo di AFM, SEM, Simulatore solare, diffrattometria RX profilometria e fotoluminescenza. •Fabbricazione: formazione su macchinari e nozioni necessarie a deposizione film per spin coating, evaporazione termica a vuoto, sputtering, deposizione elettrochimica; formazione utilizzo pressa per il nanoimpriting, tecniche per il patterning di substrati e celle (attacco chimico e fotolitografia). • Trattamenti substrati e celle: formazione per l’utilizzo di forno ossidativo, RIEE, tecniche di pulizia e funzionalizzazione substrati. Congressi, seminari, corsi avanzati e altre attività didattiche passive Attività organizzate dalla scuola di dottorato: •Summer school of nanotechnology dal 20 al 23 settembre. •Seminario: Matteo Castronovo. The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA Nanostructures. July 18 2011 •Seminario: János Kristóf and Erzsébet Horváth; synthesis and STRUCTURE elucidation of kaolinite organo-complexes •Seminar: Dr. Hicham Hmamoudi ‘Self assembled monolayers on gold the challenge’ July 1, 2011 Attività al di fuori della scuola di dottorato: •Workshop on New Materials for Renewable Energy 17 - 21 ottobre 2011 (ICTP, Miramare, Trieste, Italy). (36h di seminari, poster session, con certificato di partecipazione). •Presentazione: Michael Felsmann, da Gatan, presentazione sulle tecniche EELS, TEM e SAM ed I recenti avanzamenti in queste tecnologie. (1h) •Seminario: Serdar Sariciftci on organic photovoltaic at ICTP 13 Aprile (1h) Attività didattica di supporto e attività didattica attiva 71 Studio di articoli scientifici e rewiews riguardanti le celle fotovoltaiche organiche o l’elettronica organica in generale. 72 MICHELE ROMEO Titolo della tesi: “Sviluppo e applicazione di metodologie DFT e TDDFT per la descrizione di osservabili spettroscopici in sistemi condensati” Supervisore: Prof. GIOVANNA FRONZONI (DSCF) Tutori (eventuali): Attività di ricerca L'adsorbimento di molecole organiche su superfici semiconduttrici ha attratto un'attenzione crescente per la sua importanza nelle tecnologie emergenti. La spettroscopia NEXAFS viene largamente utilizzata per caratterizzare strutture adsorbite su superfici dal momento che permette di investigare i vari modi di adsorbimento così come l'estensione dell'interazione adsorbato-substrato. Computazioni quantistico-chimiche sono importanti per acquisire la maggior parte di informazione dagli esperimenti che sono spesso di difficile interpretazione e razionalizzazione. L'obiettivo principale del progetto è lo sviluppo di uno schema computazionale utile per la simulazione di spettri NEXAFS di molecole adsorbite su superfici nel contesto del design di modelli molecola/superficie ed in quello del calcolo ed interpretazione dei risultati spettroscopici. Durante il primo anno di dottorato è stata condotta una simulazione di spettri NEXAFS di etilene adsorbita su una superficie regolare di Silicio, nella fattispecie Si(100), considerando diverse geometrie di adsorbimento. Un primo step ha riguardato l'implementazione di un codice di interfaccia con ADF (Amsterdam Density Functional code) per il calcolo si spettri NEXAFS risolti angolarmente per date direzioni di polarizzazione della luce incidente secondo l'espressione canonica di calcolo. In un secondo step sono stati ottimizzati modelli di superfici adsorbenti con e senza le molecole di etilene per mezzo di computazioni DFT periodiche su opportuni geometrizzazioni di slab. Sono state considerate entrambe le geometrie di adsorbimento ontop e bridge. Dalle strutture risultanti dal calcolo periodico sono stati estratti razionalmente cluster finiti utili alla successiva computazione degli spettri NEXAFS dell'etilene a livello C1s. Il confronto fra gli spettri risolti angolarmente calcolati e quelli sperimentali è risultato soddisfacente e mette in luce l'evidente potenziale della tecnica computazionale nello studio delle configurazioni di adsorbimento di molecole su superfici. Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) “C K-edge NEXAFS Spectra of Model Systems for C2H4 on Si(100): a DFT Simulation”, contenuti riportati negli “Atti del XXIV Congresso Nazionale della Società Chimica Italiana” per la Divisione Computazionale Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) z Marzo - Giugno 2011, Chimica Quantistica, Prof. Mauro Stener, corso specialistico 73 Marzo - Giugno, 2011, Applicazioni Chimiche della Simmetria Molecolare, Prof. Piero Decleva, corso specialistico Congressi, seminari, corsi avanzati e altre attività didattiche passive • Serie di seminari su Molecular Self-assembling and Nanostructures, 21 Giugno – 15 Luglio, 2011, Trieste • Scuola Estiva del FVG su Bioinformatica Strutturale, 4-6 Luglio 2011, SISSA, Trieste • Scuola Estiva su Tecniche di Simulazione Atomistiche, 11- 29 Luglio 2011, SISSA, Trieste, (affiliazione CECAM-SISSA) • Scuola Estiva di Nanotecnologia 2011, 20-23 Settembre 2011, Scuola di Dottorato in Nanotecnologie, Trieste • Workshop su Nanoenergetica, 15-16 Novembre, 2011, ICTP, Trieste Attività didattica di supporto e attività didattica attiva • Analisi Matematica, Fisica ed attività di esercitazione per studenti del 1o anno dei corsi fondamentali di Fisica • Attività di esercitazione intensiva per studenti del 1o anno dei corsi di STAN e z Scienze Geologiche 74 SAJID HUSSAIN Title of the thesis: Synthesis of Ordered Semiconductor Nanostructures by Directed SelfAssembly for Photonic Applications Supervisor: GIORGIO BIASIOL Research Activity Silicon mold with 45 - 50nm diameter pillars, with a height of 90nm & period of 300nm have been fabricated using nanoimprint lithography. These molds are used in a second nanoimprint lithography step to pattern the GaAs substrates used for QDs growth. Different nanoimprint & optical resist have been tried, but good surface quality (i.e. RMS surface roughness ≥ 0.2nm) of GaAs substrate after the removal of the resist have been achieved using mr-I 7010E. After hot plate pressing of the mold and resist coated GaAs wafer, there is a very thin residual layer of resist inside the holes underneath of the pillars. This residual layer is etched using oxygen plasma in Inductively Coupled Plasma (ICP) system. These GaAs patterned substrates are chemically etched to get 50-60nm dia holes with a 5 – 10nm depth. Different solutions (i.e. HCl:H2O2:H2O & NH4OH:H2O2:H2O) with different dilution have been tried to fabricate these nanopores. Best results have been achieved with HCl:H2O2:H2O solution with a ratio of 1:1:9. Substrate is cleaned using wet chemistry & oxygen plasma in Reactive Ion Etching (RIE) system. Then oxide layer from the patterned GaAs substrate is thinned chemically before its introduction into the Molecular Beam Epitaxy (MBE) System. Silicon molds and patterned GaAs substrates have been analysed using Scanning Electron Microscopy & Atomic Force Microscopy at different stages of the process. Then patterned GaAs substrate is loaded in MBE system for QDs growth. Since thermal removal of the oxide before growth would lead to a disappearance of the holes and to a roughening of the surface. We are testing a method to desorb chemically the oxide through exposure to atomic Ga beams, followed by annealing in As4 and deposition of a thin (<10nm) GaAs buffer before deposition of InAs QDs. Understanding & optimization of the growth kinetics and parameters of QDs growth using MBE System is in process. Objectives for the following year (if applicable) Kinetics and parameters of QDs growth using Molecular Beam Epitaxy System will be studied. All parameters of QDs growth (i.e. Oxide layer removal using Ga flux, annealing, buffer layer thickness, InAs QDs growth) will be optimized using Molecular Beam Epitaxy System. Currently, nanopores on GaAs substrate are being fabricated using wet etching. As an alternative to reduce hole size, dry etching will be used to fabricate these nanopores using RIE/ICP system. Optical characterization of the QDs samples will be done using photoluminescence & microphotoluminescence spectroscopy. 75 Educational Activity Conferences, seminars, advanced courses and other didactic activities Seminar of Dr. HIcham Hmamoudi from Université-Paris Sud on ‘Self assembled monolayers on gold the challenge’ at University of Trieste on July 1, 2011. Seminar of Matteo Castronovo on ‘The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA on July 18 2011. The regional Summer school on Nanotechnology 2011 at University of Trieste on 20 -23 September 2011 Support educational activity and teaching Literature study/survey for material selection for QDs fabrication. Research papers/thesis/articles have been studied to carry out the research work. 76 FRANCESCA SANTESE Titolo della tesi: Modellistica molecolare per materiali e rivestimenti multifunzionali nanostrutturati Supervisore: Prof. Maurizio Fermeglia Tutori (eventuali): Prof.ssa Sabrina Pricl Attività di ricerca Durante il mio primo anno di dottorato ho concentrato la mia attività di ricerca su due progetti principali. Il primo è un progetto europeo, Multhybrids, il cui obiettivo primario era lo sviluppo di una tecnologia innovativa per la preparazione di componenti con nanomateriali multifunzionali; il secondo è un progetto nazionale, Nanostrata, che ha come scopo lo sviluppo di nuovi rivestimenti nanostruttuati per diverse applicazioni industriali. In Multhybrids abbiamo caratterizzato 13 sistemi con nanofillers di diversa natura e forma, puri o modificati con diversi compatibilizzanti, in diverse matrici polimeriche, utilizzando una procedura di modellistica molecolare multiscala sviluppata dal nostro gruppo di ricerca. I risultati ottenuti sono incoraggianti vista l’ottima concordanza dei valori delle proprietà termofisiche calcolate con i corrispetivi dati sperimentali. Inoltre, si è visto che nei sistemi esfoliati le caratteristiche chimico/fisiche dei modificatori non influiscono sulle proprietà macroscopiche, mentre le dimensioni e la forma dei nanofillers hanno un grande impatto sulle proprietà del materiale finale. In Nanostrata abbiamo svolto uno studio sulla bagnabilità di superfici polimeriche con liquidi di diversa natura (acqua, olio, miscela di acqua e sapone) per sviluppare una metodologia che consenta di predire alcune importanti proprietà dell’interfaccia, quali l’angolo di contatto, la tensione superficiale e il lavoro di adesione. La concordanza dei risultati ottenuti con i valori sperimentali disponibili in letteratura ha permesso di convalidare la procedura sviluppata. Si potrà quindi procedere con la progettazione di nuovi rivestimenti andando a modificare le matrici polimeriche con l’aggiunta di nanoparticelle di diversa natura. Pubblicazioni su riviste scientifiche (pubblicate oppure in stampa), “Size and shape matter! A multiscale molecular simulation approach to polymer nanocomposites” R. Toth, F. Santese, S. P. Pereira, D. R. Nieto, S. Pricl, M. Fermeglia and P. Posocco, Journal of Material Chemistry, 2011 sottomesso “Contact angles of water and oil on polymer surfaces by MD simulations” F. Santese, D. R. Nieto, P. Posocco, R. Toth, S. Pricl, M. Fermeglia, Chemical Communications, 2011, sottomesso “Water, oil, and surfactant solution on polymer surfaces: converging simulation methods for contact angle determination” F. Santese, D. R. Nieto, P. Posocco, R. Toth, S. Pricl, M. Fermeglia, Journal of Physical Chemistry C, 2011 sottomesso 77 Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) AIChE Annual Meeting 2011, comunicazione: “The Factory of the Future: Integrating Multiscale Modeling and Experiments to Produce New, Better Nanocomposite Materials” M. Fermeglia, P. Posocco, R. Toth, D. R. Nieto, F. Santese and S. Pricl, 24 ottobre 2011 Minneapolis Eurofillers 2011 comunicazione: “Chemistry and shape effects in polymer based nanocomposites: a multiscale modeling study.” M.Fermeglia, P. Posocco, R. Toth, D. Romero, F. Santese, S. Pricl 21-22 agosto 2011 Dresden, Germany NanotechItaly, comunicazione: “Nanoparticles at large. A multiscale molecular modeling protocol to predict/explain structure-property relationships in nanocomposite systems” P. Posocco, F. Santese, D. R. Nieto, E. Laurini, M. Fermeglia, J. W. Handgraaf, H. G.E.M. Fraaije, M. Lisal, S. Pricl, 23-25 novembre 2011, Venezia NanotechItaly 2011, comunicazione: “Interfacial wettability of polymeric surfaces by oil, water and surfactant/water nanodroplets. A molecular dynamic study” F. Santese, D. R. Nieto P. Posocco, R. Toth, M. Fermeglia, S. Pricl, 23-25 novembre 2011, Venezia Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) 60 ore laboratorio MOSE Scuole AMBER school 3-6 maggio 2011, Barcellona Summer school on Nanotechnology 20-23 settembre, Trieste Congressi, seminari, corsi avanzati e altre attività didattiche passive Congressi VNPCF (V congresso nazionale di chimica farmaceutica) Poster: “The long and winding road of the c-Kit juxtamembrane domain”, 28-30 marzo 2011, Trieste Seminari “Brached Peptides as Therapeutics” Prof. Bracci 21 marzo 2011 “Seminario GPU@UniTS - Processori Grafici & Calcolo Intensivo” 18 febbraio 2011 “New approaches in cancer therapy” Prof. Misiura 12 maggio 2011 “Nanosistemi per il drug e il gene delivery a base di derivati dell’acido aspartico” Prof. Cavallaro 1 giugno 2011 “Self assembled monolayers the challenge” Dr. Hicham Hamoudi 1 luglio 2011 “The effect of confinement on enzyme diffusion and reaction inside DNA nanostructures” Dr. Castronovo 29 luglio 2011 78 Corsi “Molecular self- assembling and nanostructures”, Prof. Morgante, Casalis, Pasquato Periodo 21 giugno-29 luglio 2011 Altre attività didattiche passive Congresso dottorandi Scuola di Nanotecnologie 17-19 gennaio 2011 Presentazione delle attività scientifiche dei gruppi di ricerca del dipartimento DI3, 25 febbraio 2011 79 LETIZIA TAVAGNACCO Titolo della tesi: Ruolo dell'acqua nel riconoscimento molecolare di bionanostrutture in sistemi alimentari. Supervisore: Prof. Attilio Cesàro Tutori (eventuali): Prof. John W. Brady Attività di ricerca Il tema di questo progetto di dottorato è rivolto alla identificazione di possibili parametri molecolari che controllano la sicurezza e la qualità degli alimenti. Particolare attenzione è rivolta verso l'acqua negli alimenti ed il suo ruolo fondamentale all'interfaccia di superfici biomolecolari. L'obbiettivo generale è ottenere informazioni sulla strutturazione dell'acqua in alimenti tradizionali attraverso l'utilizzo di una varietà di tecniche sperimentali a diversa risoluzione. In questo primo anno di dottorato, si è considerato il sistema caffè, e in particolare la caffeina è stata identificata come molecola modello di studio in quanto costituita da una superficie idrofobica ma solubile in acqua grazie alla presenza di gruppi funzionali capaci di formare legami a idrogeno. Attraverso simulazioni di dinamica molecolare è stato possibile caratterizzare il dettaglio molecolare della strutturazione dell’acqua attorno alla caffeina e l’associazione del soluto in soluzione. In particolare la caffeina si è rivelata un buon sistema perché ha reso possibile il confronto tra risultati computazionali e misure sperimentali e recenti teorie sull’idratazione di soluti idrofobici. Sono inoltre stati condotti esperimenti SAXS su soluzioni acquose di caffeina e preliminari misure AFM. Attraverso simulazioni di dinamica molecolare è stata inoltre valutata l’associazione di biomolecole in soluzione acquosa e in particolare l’interazione della caffeina con zuccheri quali glucosio e saccarosio. Obbiettivi da raggiungere per l’anno successivo (se applicabile) I principali obbiettivi per il seguente anno di dottorato riguardano innanzitutto il completamento degli esperimenti di SAXS e AFM. Successivamente un sistema modello di estesa superficie idrofobica sarà caratterizzato attraverso l’uso di diverse tecniche sperimentali e computazionali. Pubblicazioni su riviste scientifiche (pubblicate oppure in stampa), L. Tavagnacco, P. E. Mason, U. Schnupf, F. Pitici, L. Zhong, M. E. Himmel, M. Crowley, A. Cesàro, J. W. Brady, “Sugar-binding sites on the surface of the carbohydrate-binding module of CBH I from Trichoderma reesei” Carbohydr. Res., 2011, 345(6), 839-846. L. Tavagnacco, U. Schnupf, P. E. Mason, M-L. Saboungi, A. Cesàro, J. W. Brady, “Molecular dynamics simulation studies of caffeine aggregation in aqueous solution”, J. Phys. Chem. B, 2011, 115(37), 10957-10966. 80 J. W. Brady, L. Tavagnacco, L. Ehrlich, M. Chen, U. Schnupf, M. E. Himmel, M-L. Saboungi, A. Ceasàro, “Weakly-hydrated surfaces and the binding interactions of small biological solutes” Eur. BioPhys. J. DOI 10.1007/s00249-011-0776-2 (in stampa). Pubblicazioni/abstracts in conferenze/congressi (nazionali o internazionali) L. Tavagnacco, A. Cesàro, J. W. Brady, “Thermodynamics of aqueous caffeine selfassociation: a revisitation”, “10th Mediterranean Conference on Calorimetry and Thermal Analysis - MEDICTA 2011”, 24 - 27 Luglio 2011, Porto, Portogallo. Partecipazione a congressi (come relatore) L. Tavagnacco, A. Cesàro, U. Schnupf, P. E. Mason, J. W. Brady, “Hydration and association of biomolecules in aqueous solution”, Studium Conference “Cosmetics and Pharmaceutics: New Trends in Biophysical Approaches”, 14-15 Febbraio 2011, CNRSOrleans, Francia (presentazione orale). L. Tavagnacco, A. Cesàro, J. W. Brady, “Thermodynamics of aqueous caffeine selfassociation: a revisitation”, “10th Mediterranean Conference on Calorimetry and Thermal Analysis MEDICTA 2011”, 24 - 27 Luglio 2011, Porto, Portogallo (presentazione orale). L. Tavagnacco, M. Borgogna, J. W. Brady. A. Cesàro, “ How do water molecules probe and control bionanostructures and food functionalities”, Nanotechnology Summer School 2011, 20 – 23 settembre 2011, Trieste (presentazione poster). L. Tavagnacco, M. Borgogna, J. W. Brady. A. Cesàro, “ How do water molecules probe and control bionanostructures: caffeine and sugars”, Studium Conference “Water in biological systems”, 5 – 6 Dicembre 2011, CNRS-Orleans, Francia (presentazione poster). Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea) - “Meccanica Statistica”, Prof. C. Micheletti, 8 novembre 2011 – 28 febbraio 2012, Phd course, Sissa, Trieste. - Laboratorio SAXS, Dr. H. Amenitsch, Elettra, Trieste, marzo – giugno 2011. - Laboratorio AFM, Dr. D. Scaini, Nanolab, Elettra, Trieste, settembre – novembre 2011. Congressi, seminari, corsi avanzati e altre attività didattiche passive Nanotechnology School Congress, 17-19 gennaio 2011, Trieste. Seminario "Synthesis and structure elucidation of kaolinite organo-complexes”, János Kristóf e Erzsébet Horváth, Trieste. Seminario “The Effect of Confinement on Enzymes Diffusion and Reactions Inside DNA Nanostructures”, Matteo Castronovo, Trieste. 81 Corso intensivo "Molecular self-assembling and nanostructures", organizzato dalla Scuola di Nanotecnologie, Trieste. Giornate didattiche 2011 SISN, “Introduzione alle tecniche neutroniche per lo studio microscopico della materia, con applicazioni alla Fisica, Chimica, Biologia e Geologia”, 25 giugno – 5 luglio 2011, Valle Aurina (Bz) – Grenoble (Francia). XI Scuola di Radiazione di sincrotrone , “Radiazione di Sincrotrone: fondamenti, metodi e applicazioni”, 5 – 16 settembre 2011, Castello di Duino, Trieste. Nanotechnology Summer School 2011, 20 – 23 settembre 2011, Trieste. Attività didattica di supporto e attività didattica attiva Laboratorio di Chimica delle Macromolecole II, corso di laurea magistrale in Chimica, Prof. A. Cesàro (attività didattica di supporto). 82 SHITAL VAIDYA Title of the thesis: Study of magnetic properties in low dimentionality systems using synchrotron radiation Supervisor: Dr. Roberto Gotter Tutors (if any): Research Activity Measurement of magnetic properties of NiO/Ag antiferomagnetic films by means of x-ray magnetic linear dichroism (XMLD) at the ALOISA beam line of ELETTRA. For the estimation of the dichroism, an accurate set of parameters have been chosen for fitting the Ni L2 edge and then calculating areas under the peaks corresponding to Ni L2 edge. Neel (TN) transition temperature has identified by fitting the dichroism as a function of the temperature by means of power law exponent function for two dimensional systems. Angle resolved Auger photoelectron coincidence spectroscopy (AR-APECS), which is able to disentangle high spin and low spin contribution to the Auger intensity, has been performed below and above TN in order to deepen the sensitivity of the techniques to the local magnetic order. The data analysis for data as acquired by the new experimental set up is under development. In the mean time a subsequent experiment on a prototypical ferromagnetic system, Ni/Cu(001), is going to be prepared with preliminary characterizations for in-situ sample synthesis. Theoretical study has been done by collaborating groups. On one side AR-APECS for ferromagnetic systems has been explained by convoluting DFT ab-initio calculated DOS of majority and minority sub-bands and on another side AR-APECS has been explained by means of atomic-like high-spin and low-spin multiplet terms, for antiferromagnetic systems. On progress experiments aim to join the two findings in a single modelisation, by exploiting the Cini-Sawatzky theory, describing the trend of the Auger spectra from band-like to atomiclike behaviors depending upon the degree of electron correlation of the system (material, dimensionality, size) and to understand why dichroism in AR-APECS, which is related to local electronic structure, disappears above the magnetic transition temperature (indeed it is believed that only long range magnetic order disappear above them). Educational Activity Classes followed (date, course, professor, type of course) Date Course Professor 24/06/2011 Molecular self-assembling Loredana and nanostructures Casalis Corso per dottorato 27/06/2011 Molecular self- assembling Alberto and nanostructures Morgante Corso per dottorato 83 Type of course 28/06/2011 Molecular self-assembling Alberto and nanostructures Morgante Corso per dottorato 5/07/2011 Molecular self-assembling Loredana and nanostructures Casalis Corso per dottorato 7/07/2011 Molecular self-assembling Loredana and nanostructures Casalis Corso per dottorato 11/07/2011 Molecular self-assembling Lucia and nanostructures Pasquato Corso per dottorato Molecular self-assembling Lucia and nanostructures Pasquato Corso per dottorato 13/07/2011 Conferences, seminars, advanced courses and other didactic activities 1) XI School on synchrotron radiation: Fundamentals, methods and applications. 5-16 September 2011. 2) Summer school of nanotechnology. 20-23 September 2011. 84 VIRGILIO FRANCESCA Titolo della tesi: “Sviluppo di sensori elettrochimici mediante processi nanotecnologici per impieghi diagnostici biologici e medici” Supervisore: Massimo Tormena, Paolo Ugob Tutori (eventuali): Mauro Prasciolua a b CNR-IOM, laboratorio TASC, Basovizza SS14 km 163.5, 34149 Trieste; Dipartimento di Scienze Molecolari e Nanosistemi, Unversità Ca’ Foscari di Venezia, Santa Marta 2137, 30123 Venezia. Attività di ricerca La fabbricazione degli array di nanoelettrodi è stata eseguita attraverso la deposizione di un film sottile di polimero (strato isolante) su uno strato di materiale conduttore. Il film polimerico è stato successivamente “patternato”, attraverso litografia elettronica, in modo tale da esporre delle aree, di forma e geometria definita, dello strato conduttore sottostante. Nella prima parte dell’attività di ricerca sono stati quindi valutati i materiali da utilizzare per questo processo di fabbricazione ed è stato svolto il training per l’utilizzo dell’electron beam litography (EBL), presso il laboratorio di microfabbricazione del TASC1. Quindi sono stati ottimizzati i parametri litografici per i materiali selezionati e sono stati ottenuti i primi array di nanoelettrodi. Nell’ultima parte dell’anno gli array ottenuti sono stati caratterizzati elettrochimicamente presso il Laboratorio di sensori per elettroanalisi (LSE)2 attraverso misure di voltammetria ciclica e testati con il label luminoforo Ru(bpy)32+ per valutare l’applicabilità di una strategia di rivelabilità di tipo elettrochemiluminescente. Gli studi preliminari hanno dimostrato che l’ampia finestra di potenziale di questi sistemi può consentire di utilizzare il Ru(bpy)32+ come strategia di rilevamento. La bassa corrente di fondo del BDD (Boron Doped Diamond, materiale conduttore selezionato per la fabbricazione) aggiunto alle proprietà dei NEA e l’elettrocatalisi del sistema Ru(bpy)32+/ammina indicano che questo sistema può essere applicato per lo sviluppo di sensori ad alta sensibilità. Nella fase successiva si prevede di funzionalizzare opportunamente la superficie del polimero/resist (policarbonato) con molecole biologiche per verificare l’applicabilità nel campo di riconoscimento molecolare. Altre pubblicazioni • Presentazione Poster durante la Summer School on Nanotechnology 1 Laboratorio Nazionale CNR-IOM, S.S. 14 Km 163.5 Basovizza - 34012 Trieste. 2 Dipartimento di Scienze Molecolari e Nanosistemi, Unversità Ca’ Foscari di Venezia, Santa Marta 2137, 30123 Venezia. 85 Attività formativa Esami sostenuti, ore di lezione e di laboratorio seguite (data, corso, docente, tipo di corso di laurea). Lezioni: 20h Processi elettrodici, primo semestre 05/05/2011–25/05/2011, Prof. C. Tavagnacco, Corso di Laurea Specialistica in Chimica. Trainings: ¾ Scanning Electron Microscopy, dott. Regina Ciancio, Researcher CNR-IOM, TASC Laboratory; ¾ Electron Beam Lithography, dott. Mauro Prasciolu, Researcher CNR-IOM, TASC Laboratory. Libri: • Yamazaki K. “Electron Beam Direct writing” Nanofabrication Fundamentals and applications Ed. Ampere A. Tseng, Ch.10, 341376. • Moretto L.M. et al. “Templated Ensembles of Nanoelectrodes” Handbook of Electrochemical Nanotechnology vol.1, Ed. Yuehe Lin and Hari Singh Nalwa, Ch.4, 87-105. Reviews: o Chen Y., Pepìn A. “Nanofabrication: Conventional and nonconventional methods” Electrophoresis 22, 2001, 187-207; o Arrigan D.W.M. “Nanoelectrodes, nanoelectrode arrays and their applications” Analyst 129, 2004, 1157-1165; o Richter M.M. “Electrochemiluminescence (ECL)” Chem. Rev. 104, 2004, 3003-3036. Congressi, seminari, corsi avanzati e altre attività didattiche passive • “Syntesis and structure elucidation of kaolinite organo-complexes” J. Kistof and E. Horvath; “Virtual private network” M. Fermeglia; 03.05.2001 • “Novel Studies in Photoelectrochemistry” H.B. Yildiz, 24.05.2011 • “Self assembled Monolayer the challenge” H. Hamoudi, 01.07.2011 • FVG Summer School on structural bioinformatics 04-06.07.2011 • “The effect of confinement on enzyme diffusion and reaction inside DNA nanostructures” M. Castronovo, 29.07.2011 • XI School on Synchrotron Radiation: Fundamentals, Methods and Applications. 05-16.09.2011 • Summer School on Nanotechnology. 20-23.09.2011 86 Dottorandi del 27 ciclo ABDOLLAHZADEH Iman, ANGELONI Valeria, BORIN Daniele, CAPOLLA Sara, CECCHINI Paolo, COCEANO Giovanna, DIOLOSA‘ Marina, ELISEI Elena, FORNASARO Stefano, GANBOLD Tamiraa, IONESCU Andrei Cristian, LOVAT Giacomo, MARSON Domenico, NKOUA Ngavouka Maryse Dadina, OTTAVIANI Giulia, PANIGHEL Mirco, PIANTANIDA Luca, PITTIA Paola, SALGADO Bernardes Pereira Simâo Pedro, SCOTTI Nicola, STOKELJ Tina, STOPAR Alex, TARUSHA Lorena, VEGA Marienette, VENTURELLI Leonardo, WANG Lianqui, ZANNIER Valentina. 87 Progetti Dottorandi del 28 ciclo: Sono inclusi in questa parte del documento i progetti scientifici dei seguenti dottorandi del 28 cilco: AMNA ABDALLA MOHAMMED KHALID Email: [email protected] Title of the thesis: Atomic force microscopi investigation of the structural properties of DNA replication origins in tumor cells Laboratory: NanoInnovation Laboratory- Sincrotrone Trieste Supervisor: Dr. Loredana Casalis & Dr. Silvia Onesti Tutors (if any): Research Activity foreseen State of the art and motivation Basic cellular processes as DNA replication are crucial to cell life. Understanding at the molecular level the mechanisms that govern DNA replication in proliferating cells is fundamental to understand disease connected to genomic instabilities, as genetic disease and cancer. The process of replication, in human cells begins specific sites on the gnome called “replication origins”, whose activity is finely rregulated during the cellular cycle, and involves several proteins which recognize the origins and recuit other protein or protein complexes responsible for DNA unwinding and replication. From preliminary studies, it seems evident that DNA topology plays a fundamental role in the replication process, and that protein factors should be responsible for the correct assembling of replication complexes. Our idea is to use Atomic Force Microscopy (AFM) to study topology features on genomic DNA associable to replication origins, in the presence different protein factors. Also, we plan to highlight the unwinding mechanism of MCM (mini-chromosome maintenance) helicase complex. AFM can be used to detect the morphology, the stiffness and the frictional forces of any kind of material, in almost any kind of environment. 88 During my ICTP Diploma thesis project, I started working with AFM to studythe interaction of DNA with MCM protein complexes, which are supposed to form a ring around one strand and unzip the DNA by moving along, using energy from ATP hydrolysis. Objectives for the three years The main goal of the project is to identify topological properties of DNA replication origins, to understand the mechanism of DNA replication with hope to learn how to control the replication process in tumor cells. Moreover, since MCM is expressed only in proliferating cells it could be considered as a good candidate for novel cancer biomarkers, and could be tested in my lab (NanoInnovation lab) using the nanoarry and the microfluidic immunosensor technologies developed there. Objectives for the first year ¾To learn different biochemical and single molecule techniques to be used during the research project. ¾To concentrate our work on the optimization of the mica surface properties in order to bind DNA molecules as well the DNA-protein complexes, which is a necessary step for AFM imaging, without disturbing DNA free conformation, to study DNA topology. ¾Final step for the first year, will be to perform AFM images in air and liquid with high resolution. Research project The structural properties of the DNA origin can be understood through the topographic imaging of the sample with nanometer resolution via AFM (Atomic Force Microscopy) where the topography maps depend on the tip-sample interaction. In order to achieve this goal first we need to optimize the surface to obtain clear AFM images at high resolution. Then we will make different experiments in air and liquid to study the interaction of DNA with protein complexes, including MCM complex. Next we plan to perform AFM measurements at different temperature, to confirm the presence of an origin: origins in fact share some 89 common characteristic for example A-T richness that causes a structural instability of the DNA by increasing the temperature. The A-T bonds will in fact break earlier than G-C (two hydrogen bonds instead of three). We also expect conformational changes that can be determined by structural studies using AFM. After getting interesting results for DNA-protein complex interaction we will try to study more precisely cancer cells and understand more about the replication process in these cells. Educational Activity foreseen ¾Molecular self-assembling and nanostructures, given by Lucia Pasquato, Alberto Morgante and Loredana Casalis. ¾Other seminars and courses at UniTs, SISSA and ICTP. 90 ALESSIA AMODIO Email: [email protected] Title of the thesis: Quantitative Analysis of Tumor Suppressor and Oncogene Proteins in Tumor Micro-Samples Laboratory: Laboratorio di Nanomedicina, S.O.C. di Farmacologia Sperimentale e Clinica, Centro di Riferimento Oncologico (CRO), Aviano; Laboratorio di Chimica Analitica Università Tor Vergata di Roma Supervisor: Dr. Giuseppe Toffoli Tutors: Dr. Matteo Castronovo, Dr. Francesco Ricci Research Activity foreseen State of the art and motivation To develop novel, effective treatments for cancer patients, the experimental clinical research is certainly bound to the ability to detect, characterize and understand the molecular basis of cancer development and progression. The cellular heterogeneity in tumour samples, patients’ diversity and their different response to therapies are among the several factors that unpredictably bias experimental results found in different laboratories. For instance, laser micro-dissection (LCM) seems to properly address the issue of tissue heterogeneity and represents the state-of-the-art in reducing biological noise that bias biomarkers identification [Cadron I. et al., Gynec. Onc., 2009]. High-throughput evaluation of biomarkers in tumour micro-samples, however, is particularly hampered by the lack of sensitive analytical tools [Nan Y. et al., Med. Oncol., 2009]. For instance, currently available methods to analyze protein-nucleic acid interactions within biological samples mostly rely on one or more purification/separation steps that require >0.1mL sample amounts, and, in addition do not allow detection of biomolecular complexes under equilibrium conditions (as they might form in the cell). These critical aspects reduce our capability to quantify protein-nucleic interactions in biological micro-samples (i.e. in µL amounts) such as those that can be obtained from early tumours or LCM samples. Basic research has identified a number tumour suppressor or oncogene proteins among transcription factors [Darnell J.E. Jr, Nat Rev Cancer, 2002] that are sequence-specific, DNA-binding proteins that regulate gene expression [Latchman D.S., Int. J. Bio. Chem. Cell. Bio., 1997]. Nanotechnology overcomes the aforementioned analytical limitations with the possibility of measuring protein amounts down to a hundred molecules and sub-nanomolar concentrations, and in nanoliter to picoliter volumes [Chiu D.T. et al., Acc. Chem. Res., 2009], that are compatible with the aforementioned tumour micro-samples. Furthermore, electrochemical analysis is one of the most sensitive methods for detecting biologic substances [Li J. et al., 91 Electroanalysis, 2012] and can be used to detect cancer biomarker [Wang J., Biosens. Bioelectron, 2006; Chikkaaveeraiah B.V., ACS Nano, 2012]. Recent years have seen the development of a broad class of electrochemical biosensors that employ a redox-tagged DNA probe that is covalently attached to an interrogative electrode (hereinafter E-DNA). The detection signal is produced by a binding-induced change of the efficiency by which an attached redox tag approaches the electrode surface. Such sensors perform well in complex media, as e.g. crude cellular extracts and undiluted blood serum, because the inherent binding-induced changes are generally not mimicked by the nonspecific adsorption of interferants to the electrode surface, and also electroactive contaminants are rare in biological samples. For these reasons this kind of biosensor has the potential to provide fast, highly sensitive and economic detection, to be used in medical diagnostics. Objectives for the three years The objective of this project is to develop and apply an easy-to-use, portable sensor for the functional analysis and detection of tumour suppressor and oncogene proteins in tumour micro-samples with label-free, electrochemistry-based devices. Also, in this project I plan to develop specific protocols for analyzing biological samples with increasingly reduced volume with the proposed approach. Objectives for the first year The aim of the first year is the development of useful “signal-off”3 and “signal-on”4 probes. To test the feasibility of the sensing systems, control experiments will be performed under different conditions (e.g., pH, ionic strength, frequency), these experiments will also allow to optimize the experimental parameters in order to achieve the best sensing performance. The aim will be reached through these steps: •targets identification and selection; 3 “Signal-off” E-DNA. In the absence of a target protein, the probe-attached, redox tag is free to collide with the electrode surface and, in turn, a large faradaic current is produced at the redox potential corresponding to the redox tag. In the presence of a target protein, the faradic current is suppressed upon recognition between target and probe. The latter leads to a “signaloff” behaviour, which allows target detection [Ricci F. et al., Anal. Chem., 2009]. 4 “Signal-on” E-DNA. The inherent, novel sensor relies on a probe structure-switching mechanism. Specifically, the probe is an electrode-bound, redox-tagged DNA forming two, stable, and rapidly interconverting conformations (nanoswitch) [Bonham A. et al., J. Am. Chem. Soc., 2012]. In one state, a redox-active reporter is located adjacent to the electrode, thereby leading to an efficient electron transfer. In the other state (the nonbonding state), the redox label is located far away from the electrode, thereby reducing the electron transfer efficiency. In absence of the target, the nonsignalling, nonbinding state is thermodynamically favoured. On the contrarily, in the presence of the target, the conformational equilibrium is shifted, thereby favouring its target binding-competent state. The inherent, structural remodelling of the E-DNA probe corresponds to a large increase of faradaic current through the electrode, which allows the “signal-on”-based, target detection. 92 •probes design; •electrochemical analysis with different experimental conditions; •electrochemical analysis with different nanoswitches; •Atomic Force Microscopy experiments with experimental conditions; Research project To achieve the objective of my PhD project both “signal-off” and “signal-on” E-DNA probes will be implemented. In order to develop E-DNA, targets will be selected and probes will be designed (a nucleic acid folding and hybridization prediction program, such as Mfold, will be used in order to construct sequences and to have information about several features of the probes such as free energy estimation of specific conformations of the probes). In order to demonstrate the sensing principles, I will first use conventional macro-electrodes. To select the best experimental parameters and evaluate the analytical performance of the molecular switches, I will perform a series of electrochemical analysis (using an Autolab) of purified solutions modifying the experimental parameters, using different nanoswitches, redox labels and novel nanoelctrode materials. For each trial probe, calculated and experimentally derived values of Ks will be systematically compared. To determine the switching equilibrium constant of each variant, I will use urea denaturation. AFM will be used to investigate the mechanochemical properties of the surface-bound biomolecules, and their influence on the behaviour of the electrochemical sensors and to monitor the formation of probe-target molecular complexes in a label-free manner, and directly on the surface of the electrode (without requiring its operation) as a function of the aforementioned surface properties. The E-DNA sensors thus developed and optimized will be adapted to a multi-array platform. We will couple these arrays with portable instrumentation (such as PalmSens) and low-cost gold screen-printed electrodes. Results obtained with electrochemical DNA-based sensors will be calibrated by means of currently available technologies (e.g. ELISA, Western-blot experiments). This calibration step will be also undertaken to demonstrate the advantages and the limitations of our approach. A tentative project Gantt diagram is shown below. 93 Activity Task 1 1. Development of “signal-on” and “signal-off” probes 2 3 4 5 First Year Second Year Month Month 6 1.1 targets selection 1.2 probes design 2. Best experimental parameters selection and analytical performance of the molecular switches or Sensing systems testing, evaluation and improvement 2.1 electrochemical analysis of purified solutions with different experimental parameters 2.2 electrochemical analysis of purified solutions with different nanoswitches 2.3 electrochemical analysis of purified solutions with different redox labels 2.4 electrochemical measurements with novel nanoelectrode materials 3. Dissociation constants (Ks) determination 3.1 Binding curves 4. Switching equilibrium constants determination 4.1 Urea denaturation experiments 5. Effect of surface confinement 5.1 AFM experiments 6. Analysis of complex biological samples 6.1 Procedures development 6.2 Electrochemical measurements 7. Electrochemical analysis of complex biological microsamples 7.1 Screen-printed electrodes fabrication 7.2 E-DNA sensors adaptation to to a multi-array platform 7.3 Microsamples preparation 7.4 Electrochemical measurements 8. Calibration of the obtained results by means of currently available technologies 8.4 ELISA experiments 8.5 Western-blot experiments Figure 1 – Gantt diagram 94 7 8 9 10 11 12 13 14 15 14 17 18 19 20 21 22 23 24 25 Third Year Month 26 27 28 29 30 31 32 33 34 35 36 Educational Activity foreseen I will improve my knowledge in the field of E-DNA by studying literature about their development, application and characterization and by taking part to meetings, seminars and courses. At the moment I plan to participate to: -Interdisciplinary spring school (7-8 March 2013, Udine) -Summer school on nanotechnology (usually first week of July, Trieste) Until now I participated to the Annual Meeting of PhD School in Nanotechnology (9-11 January 2013) and I’m attending an English course at UPTER- Rome. 95 FRANCESCA CAMMISULI Email: [email protected] Title of the thesis: Effects of nanomaterials on biological barriers fetal and post-natal and toxicity evaluation epigenetic. Laboratory: Laboratorio integrato di immunopatologia - I.R.C.C.S. Materno-infantile «Burlo Garofolo» di Trieste Supervisor: Pascolo Lorella Research Activity foreseen State of the art and motivation Nanoscience is a result of scientific progress in the twenty-first century. The diffusion of the studies on nanomaterials and nanotechnology appears to be growing. Nanotechnology, in fact, represents a great opportunity for development. Nanomaterials represent a significant opportunity for innovation that is covering across many areas ranging from medicine, electronics, energy production. To date, this science has provided remarkable results. The utility of nanostructures and nanomaterials is linked to their particular flexibility. Beyond the merits and the substantial opportunities offered by nanotechnology research, however, it is important to focus on another aspect of the research: that is the potentially associated risk for health. There is a great need of studies aimed at understanding the possible harmful effects of nanomaterials. People are exposed to nanomaterials from many sources from final products at manufacturing processes. In some working environments, certain nanoparticles can be inhaled by workers and there is a risk that they can act such as asbestos. Many scientists argue that nanomaterials could put the health of people at risk, causing inflammation and possibly cancer. From the actual definition, nanoparticles (NPs) are structures of various shapes and different composition with the size ranging 1 and 100 nm. They are divided in NPs of natural origin (produced by combustion as in volcanoes), NPs of anthropogenic origin (produced by diesel engines or industrial incinerators) and artificial NPs (obtained through nanotechnology). These structures possess unique physical and chemical properties, which depend on their nanoscale dimensions and especially on the high ratio surface area/volume, that give to the NPs peculiar chemical reactivity, optical, magnetic, catalytic and electrochemical properties. 96 In the last decades, these characteristics have made the new NPs of considerable interest in technological development and are widely used in medicine and diagnostics, in biotechnology and in cosmetics, food and materials. However, the increasing exposure to nanoscale particles requires studies in order to characterize the properties and potential toxic effects. Although they are applied in a vast number of fields that seem to be destined to increase, the effect of exposure in humans remains undetermined. From the first studies, it seems that some NPs may lead to in vitro alteration of gene expression and cell death and that they are able to induce DNA damage both directly and indirectly, causing oxidative stress and inflammatory responses. Although many suppositions have been made about the possible harmful effects of nanoparticles on the body, it is not clear yet what is the exact mechanism by which these nanostructures interact with cells and subcellular structures. My Ph.D. work is part of the project that aims to unravel the possible effects and the toxicity induced by nanomaterials. In particular my project will deal with the effects of exposure during fetal and post natal life. The work will concentrate on the ability of the placenta and other biological barriers to prevent nanoparticle diffusion into the body. At the same time both short term effects (at barrier level) and long term effects (DNA damage) will be investigated. Appropriate cell models will allow to investigate the relationship between physico-chemical properties and toxicity. I’ll particularly concentrate on the possibility to use unconventional approaches to reveal unknown features of effects of nanomaterials in biological systems. Objectives for the three years 1.Evaluation of the toxicity at tissue level in human placental and other physiological barriers (lung, brain): Collection and classification of human tissues (human at term placentas from donors, other tissues from archives and biobanks) of patients exposed to nanoparticles. Investigation for the possible presence, histological localization and chemical characterization of nanomaterials on biological barriers (mainly placenta and lung) trough conventional and innovative microscopic techniques based on the synchrotron radiation. 97 Correlation of multiple approaches and techniques (conventional and advanced techniques, molecular and physico-chemical analyses) to evaluate the toxicity of nanomaterials on biological barriers. Use of molecular techniques to evaluate the toxicity due to epigenetic effects of nanomaterials at the DNA. 2.Evaluation of the toxicity in models of biological barriers (placenta/lung/brain) by in vitro studies with cell lines of human chorion carcinoma (BeWo,Jar,JEg-3) and others. Identification of cellular targets, and sub-cellular and molecular mechanisms of toxicity of nanomaterials using conventional and innovative microscopic techniques. Investigate if the chemical-physical characteristics of nanomaterials and their reactivity are translated into special effects and biological mechanisms. 3.Search of epigenetic effects due to the toxicity of nanomaterials: Assessment of molecular and innovative microscopy to evaluate the toxicity due to epigenetic effects of nanomaterials on the DNA. 4.Potential validation of new protocols for the study of toxicity of nanomaterials. Assessment of epigenetic toxicity evaluating modifications connected to the microenvironment that alter the degree of activity of genes without modifying the gene sequence. One of the epigenetic mechanisms from exposure to environmental agents is DNA methylation. Assessment of microscopic techniques of vibrational (IR-FTIR/ IR-RAMAN) to detect macromolecular changes in biological systems. Set up of molecular techniques to detect the methylation at the DNA by bisulphate sequencing. Assessment of molecular techniques to evaluate the alteration of gene expression by DNA microarrays technology. 5. Integration of different data and risk assessment of the exposure to nanomaterials (mainly ambiental) during pregnancy and in post-natal life. Objectives for the first year Collection and classification of human tissues (human at term placentas from donors, other tissues from archives and biobanks) of patients exposed to nanoparticles. 98 Evaluation of the toxicity in models of biological barriers (placenta/lung/brain) by in vitro studies with cell lines of human chorion carcinoma (BeWo,Jar,JEg-3), identifying the cytotoxic and genotoxic effects. Development of multiple approaches and techniques (conventional and advanced techniques, molecular and physico-chemical analyses) for the accurate evaluation of the characteristics of toxicity nanomaterials on biological barriers fetal and post-natal. Utilization of microscopic innovative techniques based on the synchrotron radiation (XRM-XRF-XRD) to assess the presence and morphology of nanomaterials in biological systems model. Development of protocols with microscopic techniques of vibrational (IR-FTIR) to detect changes in biological systems at the macromolecular model. Development of protocols with molecular techniques to evaluate the toxicity due to epigenetic effects of nanomaterials at the DNA (ie. methylation) Development of protocols with microscopic techniques of vibrational (IR-Raman) to analyze macromolecular changes at the DNA (ie. methylation). Validation of these new techniques for the study of toxicity. Research project The project implies the following activities: 1.Sample selection and identification. Collection of tissue samples (biological barriers fetal and post-natal) from persons exposed in areas of interest and classification according to the hazard of exposure. Extraction of DNA from tissues and classification according to the hazard of exposure of the subject to nanoparticulates. Identification and selection of control samples: DNA control / control tissues (other biological barriers, for example the lungs or the blood-brain). 2.Sample preparation: cellular models. Models of toxicity (placenta/ lung / brain), with particular reference to the chorion carcinoma cell lines of human (BeWo, JAr and JEg-3). 99 Study of the cellular localization of nanomaterials and on effects of exposure to various concentrations of nanomaterials model by conventional and innovative microscopy. −Conventional microscopy: optical microscopy based on color "vital" and "non-vital" to reveal morphological details otherwise not visible or indicate the metabolic state of the cell, thus determining cell vitality. −Fluorescence microscopy: for evaluation of whether the nanoparticles induce cell death by apoptosis; the cell lines will be analyzed by fluorescence microscopy after fixation with the nuclear dye DAPI to highlight the nuclear morphology and the presence of apoptotic bodies. −Innovative microscopy: xX-ray microscopy to study the morphology of the sample. xX-ray fluorescence to identify and quantify the chemical elements present in the sample. xX-ray diffraction for determining concentration profiles, film thicknesses, the atomic arrangement in amorphous materials and multilayer. 3.Microscopic analysis of tissue. Conventional microscopy: histochemical stains to localize the presence of transition metals (i.e Fe) and discriminate the oxidation state in regions of tissue that incorporated nanoparticles. − Hematoxylin and eosin staining to analyze the morphology of the tissue and the presence of any nanoparticles. − Perls/ Lillie/ Schmorl staining to discriminate the different oxidation states of iron ion. 4.Analysis of histological samples processed by optical microscopy. Innovative microscopy analysis exploiting the synchrotron radiation: XRM-XRF analysis of histological samples to study with better resolution the morphology of the tissue sample, and simultaneously to identify and quantify the chemical elements present in the sample; the data will be analyzed by appropriate software (ie. PyMCA). 100 5.Analysis of epigenetic changes. Microscopic techniques of vibrational (IR-FTIR) to detect changes in biological systems at the macromolecular model. Microscopic techniques of vibrational (IR-Raman) to analyze macromolecular changes at the DNA (ie. methylation or phosphorylation). Molecular techniques to evaluate the toxicity due to epigenetic effects of nanomaterials at the DNA (ie. methylation). −With the technology of DNA microarrays it is possible to measure the level of expression of thousands of genes simultaneously, using the basic principles of hybridization of nucleic acids: microarray experiments will allow to understand which genes are modulated by methylation as the effect of nanomaterial presence. −Analysis of DNA methylation using bisulphite sequencing: The method is based on the deamination of cytosine residues to uracils in the presence of NaOH and sodium bisulfite. Since methylcytosine is not converted under these conditions, the original methylation state of the DNA can be analyzed by sequencing of the converted DNA. After the conversion reaction, the DNA sequence under investigation is amplified by polymerase chain reaction (PCR) with primers specific for one strand of the bisulfite-converted DNA. The PCR product is cloned and individual clones are sequenced. 6.Integration of data obtained with different microscopy and molecular techniques . 101 Tasks 1. Sample selection and identification 2. Sample preparation: cellular models 3. Microscopy analysis of tissue 4. Analysis of epigenetic changes 5. Integration of the data obtained Start month Duration (months) End month mar-13 12 mar-14 apr-13 giu-13 mag-13 dic-15 21 32 38 10 gen-15 mag-16 lug-16 set-16 Educational Activity foreseen For the first year I plan to follow one or two courses at University: xOptical spectroscopies applied and analysis of images xIntroduction to organic spectroscopy. 102 CANDIDATE PIETRO CAPALDO Email: [email protected] Title of the thesis: “Capacitance Immunosensors for the early detection of circulating cancer biomarkers” Laboratory: NanoInnovation Laboratory at Elettra-Sincrotrone Trieste Supervisor: Dot.ssa Loredana Casalis Research Activity foreseen State of the art and motivation Medical diagnosis requires point-of-care biosensor arrays at the patient's bed. This requirement is due to new emerging demands for personalized therapies because therapeutic agents amount in tissue and blood serum is different on a patient-by-patient basis. Therefore, the development of low-cost, point-of-care technologies for array biochips is a necessary step to introduce personalized therapies in clinical practice and the miniaturization, developed in recent years, of biosensors and their integration in microarrays and functional biochips will enable massive parallel detection of analytes, diseases and disease susceptibilities, as well as identification of personalized drug response profiles. The concept of a “Micro Total Analysis System” (mTAS), where attempts are made to completely integrate (bio)chemical systems on silicon or glass substrates, has been envisioned as a new concept for analytical devices, because it is expected that miniaturization will improve the speed and reliability of the measurements and will dramatically reduce the sample volume and the system costs. The gold standard for single protein measurements is immunoassay, which exploits the specificity and sensitivity of antibody-antigen recognition, like in the Enzyme-Linked Immuno-Sorbent Assay (ELISA), which has a well-established specification for measurement of single proteins in a solution, with a lower limit of reliable quantitation of ~1 pg/ml and dynamic range of 3 logs. Such devices can assay up to 16 different sample in some commercial platform, like Pierce Biotechnology, in few hours [S. Kingsmore, Nat. Rev. Drug Disc., 5, 310 (2006)]. Also, protein array technology has evolved and found its way into quantitative proteomics through the construction of what is called a “protein microarray”.[K.D. Kumble, Anal. Bioanal. Chem., 377, 812 (2003)] based on optical detection, such as fluorescence [B.B. Haab et al., Genome Biol., 2, RESEARCH0004 (2001); H. Zhu et al., Science, 293, 2101 (2001)], or SPR (Surface Plasmon resonance) [C.T. Campbell and G. Kim, Biomaterials, 28, 2380 (2007); J.M. McDonnell, Curr. In such optical sensors the target molecules can be labeled with fluorescent tags such as dyes and the fluorescence is detected in presence of the targeted molecule. This allows for extremely sensitive detection down to a single molecule. However, the process is laborious and may also affect the function of the biomolecules. In label-free techniques, proposed as alternative to fluorescence and chemi-luminescence, the targeted molecules are detected in their natural form. These molecules are attached to the optical sensor surface using probe molecules and the attachment is detected by measuring the change in optical properties for the sensor. In particular, sensors based on silicon-on-insulator (SOI) photonic wire waveguides are important because of their compatibility with CMOS fabrication and possibility of integrating detection and decision on the same chip leading to “laboratories on a chip”. Further, guided-wave sensors allow for integration of multiple sensors on a single chip. But, the considered micro-array technology based on optical 103 detection and molecular labeling is costly and time consuming. Thus, it is not adapted for applications to personalized therapy in hospital or at home. The aim of the present research project is to develop a successful design for a point-of-care immuno-sensor, optimized in terms of simplicity, reproducibility, sensitivity, and cost. Our idea is to perform electrochemical impedance measurements in microfluidic channels, where the electrodes are properly functionalized with biomarker-specific capture proteins to allow for a label-free detection of fM concentration of biomarkers in small biosample volumes Objectives for the three years The final goal of my PhD is to create a microfluidic immunosensor based on the electrical detection on array of a series of parallel microfluidic channels (four or five), in other words a multiplexing system, where each channel is characterized by a series of bio-functionalized microelectrodes, thus providing the possibility to recognize 4 or 5 biomarkers simultaneously. Objectives for the first year ¾The first year will be, almost entirely, spent in learning different techniques of microfabrication and (bio)functionalization of the electrodes so constructed. In particular, talking of micro-fabrication, I should learn to use the basic equipment for the manufacture of electrodes. Below is a list instruments that should be used and its function: Spin coater: It is used to cover a sample with a uniform thin film. An excess amount of resist is placed on the slide which is then rotated at high speed in order to spread the fluid by centrifugal force. Mask Aligner: It uses light to transfer a geometric pattern from a photo-mask to a light-sensitive chemical photoresist, or simply "resist," on the substrate. Electron Beam Evaporator: is a form of physical vapor evaporation in which a target (in our case Ti and Au) anode is bombarded with an electron beam produced from a hot tungsten-filament under high vacuum. The electron beam causes atoms from the target to transform into the gaseous phase. These atoms then precipitate into solid form, coating our samples in the chamber with a thin layer of the anode material. Atomic Force Microscopy (AFM) to check and optimize the biofunctionalization protocols. Set-up of the read-out system, based on a HEKA Potentiostat/ Galvanostat PG 340 usb, for the detection of 1 reference biomarker. Calibration of the capacitance read-out of 1 single channel device, compared to standard ELISA and nano-arrays (developed in our laboratory) outputs. Research project We plan to develop a new class of immune-sensors where antigen-antibody interactions are detected via impedimetric detection as for Electrochemical Impedance Spectroscopy (EIS). In other words, the signal in this type of sensors depends on the impedance change produced by 104 the measured quantity in the geometry of an electrical equivalent circuits (EECs) [Figure 1] related to electrochemical cell constant, and thus the change can be used for the sensing mechanism of biological species. To better understand the application of a EIS microfluidic chip, try to define its structure. In particular, we discuss the alternating current (AC) frequency characteristics of these sensors as parameters for sensor design, such as interelectrode spacing and electrode area. Consider a glass device [Figure 2 (c)], which consisted of a capillary channel and coplanar impedance sensors. This latter feature is important because coplanar electrodes can be easily patterned at very small dimensions which allows to build miniaturized and low cost devices. Design parameters are as shown in Figure 2 (d). In this context, Rsol represents the properties of the electrolyte solution and the diffusion of the redox probe. If two electrodes of equal area S [m2] are placed in parallel at a perpendicular distance D [m] from each other, the solution resistance Rsol [W m], measured by driving the electrodes with an AC voltage v [V] and by measuring the resulting current [A], is related to the solution resistivity rsol [W m]. A parasitic resistance, RPara, is present in series with the sensor and it resulted from the resistance in the connecting cables and mainly Au (or Pt) thin film electrodes. Direct capacitive coupling between electrodes is represented by the cell capacitance, CCell, whose value is determined by the dielectric constant of the electrolyte and the geometry of the electrodes. The coplanar electrodes are usually embedded in dielectric substrates (glass) and the only small area of electrodes contacts with biomolecule solutions for sensing and so, the parasitic capacitance due to dielectric substrates cannot be ignored. Thus, the parasitic capacitance must be reduced to enhance the sensitivity. Additionally, a metal electrode in contact with an electrolyte possesses a natural charge density due to an excess or a deficiency of electrons at electrode-electrolyte interface, in order to maintain electrical neutrality. This accumulation of ions forms an electrical double layer that consists of an adsorbed fixed layer, which is independent of electrolytic (ionic)concentration, and a diffusive mobile layer, which is a function of the ionic concentration. This electrostatic phenomenon is electrically represented by a double-layer capacitance, CDL . The interfacial capacitance (of the level nF to mF) can be used as a sensing mechanism combined with specific surface reactions. When antibodies bind to antigens, the change in the electric properties results in a change of impedance, enabling the measurement of direct electrical signal, such as magnitude and phase angle and the surface modification may be accompanied to improve the sensitivity and selectivity. 105 Fig.1. (a) An electrified interface in which the electrode is negatively charged. (b): An idealized electrical equivalent circuit for the interface. Abbreviations: IHP inner Helmholtz plane; OHP outer Helmholtz plane. Fig.2. Schematic diagram of a glass-based micro-channel chip with coplanar impedance sensors: (c) layout of a glass device and (d) rectangular planar electrodes. (e) Schematic diagram of total Impedance frequency plots divided into dominant components. An EIS microfluidic chip so constructed and with a particular detection technique allows the identification of various biomarkers of interest within a fluid/serum such as may be human blood. So, the next step, in the chip development, will be characterize the electrode of the chip, i.e. design and develop innovative biosensors for the routine detection of extremely small amounts of genetic material. In this context, a novel approach for the functionalization of the electrode of the EEC, which takes advantage of AFM-based nanografting, is the SelfAssembled Monolayers (SAMs) of organic molecules. And, it is thanks to this nanografting technique that I can characterize the electrode in my EEC and therefore can make measurements of electrochemical impedances very sensitive to certain biomarkers. 106 Educational Activity foreseen •Molecular selfassembling and nanostructures, given by Lucia Pasquato, Alberto Morgante and Loredana Casalis. •A course focused on learning of system design platform LabView, given by Dr. Cautero at Elettra-Sincrotrone. •Other seminars-conferences held in Trieste, such as the training course, given by the Prof. Scoles, on intermolecular forces. 107 LUCIA CORAL Email: [email protected] Title of the thesis: Detection of tumor cell surface biomarkers in microsamples Laboratory: Centro di Riferimento Oncologico di Aviano Supervisor: Giuseppe Toffoli Tutors (if any): Matteo Castronovo, Giacinto Scoles Research Activity foreseen State of the art and motivation Cancer research requires a truly accurate evaluation of biomarkers that yet have not been met due to several factors that unpredictably bias experimental results found in different laboratories such as the different developmental stages of tumor and the cellular heterogeneity in tumor samples beside patients’ diversity and their different response to therapies. Nanotechnology-based approaches to protein detection can be more sensitive than ELISA (see for instance Nanosphere – Gold Nanoparticle technology). Several ELISA variant have been developed and 0.01 pg/mL sensitivity have been demonstrated (see High Sensitivity ELISA Kits commercialized by eBioscience). ELISA, however, is based on enzymatic reactions that have a limited application to the analysis of solid samples, and in vivo. For instance, fluorescence activated cell sorting (FACS) analysis of cells marked with fluorescently labeled antibodies is one of the most commonly used methods for analyzing cell surface protein biomarkers. However, this technique can be used only for studying highly and moderately expressed biomarkers (102-104 proteins per cell are required) (Joensson H.N. et al. Angewandte Chemie Int. Ed. 2009). Chemiluminescence is the detection methods of choice for Western-blot analysis. This approach however provides semi-quantitative results and is based on enzymatic reactions. Furthermore, in general, quantitative gel analysis is performed by using the less safe immuno-radioactive labeling approach. In the last five years, DNA self-assembly has been used to generate molecular nanodevices where biomolecules are confined with controlled molecular packing, composition and chemical functions, and allowed the implementation of unprecedented detection approaches for analyzing biomolecules in small sample-volumes (potentially down to single cell amounts). Water-soluble, dense, DNA nanostructures (also called ‘DNA-origami’) were introduced by P.Rothemund in 2006, who provided a software tool to design planar shapes that form via Watson-Crick hybridization of several, short single strand DNA (ssDNA) sequences (the staples) with a long circular ssDNA molecule (the scaffold) (Rothemund P. Nature 2006). Since then, several papers demonstrated the functionalization of DNA-origami with different probes among which antibodies for immuno-detection (Douglas S.M. et al., Science 2012). DNA self-assembly allows precise spatial positioning of attached probes: 108 P.Tinnefeld and co-workers demonstrated that the precise localization of fluorophores on a two-dimensional DNA-origami breadboard allows for alternative energy-transfer pathways dependent on the incorporation of a “jumper” dye at specific positions (Stein I.H. et al., JACS, 2011). S.Lindsay and co-workers demonstrated that DNA-origami display enhanced resistance to enzymatic digestion in complex biological mixtures such as cell lysate at different incubation times, temperature and concentrations, with respect to unfolded scaffolds (Mei Q. et al., Nano Letters 2011). A major limit to the widespread application of DNA-origami in biomedical research is provided by their relatively high cost. M-13 ssDNA-based DNA-origami can be conveniently amplified by e.g. phage display, and also other scaffolds can be used (Castro C.E. et al., Nature Methods 2011; Högberg B. et al., JACS Communications 2009). In addition, ssDNA engineered staples could be amplified after being incorporated in DNA vectors, and extracted from these latter via restriction enzymes processing. Objectives for the three years The major objective of this short-range project is to develop low-cost, programmable probes for the highly sensitive immunodetection of cell surface, tumour biomarkers in microsamples, based on fluorescence optical imaging. The goal is also to limit sample preparation as to reduce sample degradation. In the long range, this approach will allow quantify amounts of candidate, innovative biomarkers in heterogeneous tumour samples, where they are scarcely expressed. My work will comprise: -development of low-cost, water-soluble DNA nanostructures, functionalized with 10-100 copies of a fluorescent molecules for signal amplification; -linkage of these nanostructures to probes (e.g. DNA aptamer, or monoclonal antibody) that are specific to the pre-selected, cell surface biomarkers; -calibrating this novel quantitative approach with simplified samples such as decreasing volumes of standard solutions containing the target protein or cultured tumour cell lysates, for comparison with ELISA assay, Western Blot assay and FACS; -quantification of amounts of cells-surface biomarkers by means of fluorescence optical imaging within different type of samples. These include, in particular, ex-vivo, unprocessed, solid tumour tissues with sizes ranging from a few cm (corresponding to volumes of a few mL) down to a few hundred μm (corresponding to volumes of a few μL); -developing some simple protocols for reducing the cost of synthesis of these DNA nanoassemblies and enabling high throughput applications. Objectives for the first year For the first year I plan: -to synthesize and purify already known DNA nanostructure; 109 -to label DNA nanostructure starting from published shapes with several copies of a fluorescent dye (to obtain so called ‘OriFluo’ complexes); -to label OriFluo with antibodies directed against a tumour cell surface biomarker (to obtain so called ‘Ab-OriFluo’ complexes); -to perform exploratory test of Ab-OriFluo in calibration samples; -to amplify M-13 ssDNA scaffold by cultured cells transfection. Research project Synthesis of Fluorescently labelled DNA-origami linked to an antibody (Ab-OriFluo). DNA-origami will be designed by using the online-available software called CadNano 2. Folding of DNA-origami will be obtained by hybridizing the scaffold (e.g. M-13 ssDNA, 130 nM) and ss-oligonucleotide staples in a 5x excess during a thermal ramp (typically: T=95°C for 15min, followed by cooling at -1°/min, up until T=20 °C is reached). Different buffers will be used. Typically M-13 based DNA-origami properly folds in 10mM Tris, 12.5 mM MgCl2, pH 8.0. Agarose gel electrophoresis analysis will be used to monitor the weight of the obtained DNA-origami as to select best synthesis conditions. DNA-Ab likage. Solulink provides a kit to directly link an antibody to an oligonucleotide through two organic linkers (sulfo-S-4FB e S-HyNic) without needing HPLC purification. The extraction of the complex is made by conjugate adsorption on magnetic affinity beads. DNA-fluorophore linkage. Staples modified with organic fluorophore can be purchased from almost any manufacturer (e.g. Integrated DNA Technologies – IDT). Otherwise, (thiol / amine) modified fluorophores can be linked to (amine / thiol) modified staples via sulfoSMCC etherobifunctional crosslinker (Pierce). In general each copy of a DNA-origami based on the M-13 ssDNA scaffold contains about 200 staples. Therefore, compared to commercially available, fluorescently labelled antibodies, I expect Ab-OriFluo to provide fluorescence intensities two order of magnitude higher. Analysis of Ab-OriFluo. I plan to use AFM to analyse the structure of obtained DNA nanoassemblies adsorbed on a mica surface (Rothemund P. Nature 2006). Also, side-by-side, AFM topographic images will be used to detect antibodies linked to the DNA structure as their presence produces a significant height increase. Fluorescence, optical imaging of the obtained DNA-origami adsorbed on a fused-silica support will be carried out to determine the functionality of the DNA-attached fluorophores. A transmission electron microscopy-based analysis will be needed to provide structural characterization of the DNA-origami. Dr. Castronovo and I are working to develop specific collaborations with researches in EU or USA for this. 110 Purification of Ab-OriFluo. Samples need to be purified as to remove the unbound fluorescently labelled staples. Different technique will be tested in order to obtain high recovery yield and low degradation of the structures. Development of low-cost amplification method of ssDNA scaffold for Ab-OriFluo synthesis. In contrast to most other bacteriophages, which assemble inside the cytoplasm, and are released by cell lysis, the morphogenesis of filamentous bacteriophage (M-13) is simultaneous to virus extrusion, without inducing cell lysis. Infected cells continue their growth and divide while extruding progeny phage particles into the medium. In turn, I plan to produce high amounts of M-13 in cell cultures by standard precipitation by adding PEG to culture medium. Development of low-cost amplification method of ssDNA staples for Ab-OriFluo synthesis. I plan to engineer a phage vector that contains several staples, which are connected by spacers, each one containing a restriction site. 111 GANTT DIAGRAM Year 1 I trim. II trim. III trim. IV trim. Year 2 I trim. II trim. III trim. IV trim. Year 3 I trim. II trim. III trim. IV trim. Synthesis of Fluorescently labelled DNA‐origami linked to an antibody (Ab‐OriFluo) Developing a method for the synthesis and purification of DNA‐origami with known or novel structures Labelling of the DNA‐origami with antibodies directed against a cell surface tumour biomarker and caractherization of the obtained structure (Ab‐Ori) Linkage of several copies of a fluorescent dye to the DNA‐origami and characterization of the obtained structure (OriFluo) Labelling of the OriFluo with antibodies directed against a cell surface tumour biomarker and caractherization of the obtained structure (Ab‐OriFluo) Exploratory test of Ab‐OriFluo in calibration samples Calibrating Ab‐OriFluo with standard solutions containing the target protein and sensitivity comparison with ELISA and Western Blot assays Calibrating Ab‐OriFluo with lysates of tumor cell cultures of decreasing volumes and sensitivity comparison with ELISA and Western Blot assays Application of Ab‐OriFluo in ex‐vivo samples Application of Ab‐OriFluo in cultured tumour cells and target tumour marker quantification Application of Ab‐OriFluo in solid tumour tissues and target tumour marker quantification Development of low‐cost Ab‐OriFluo Amplification of M‐13 ssDNA scaffold by cultured cells transfection Development of staples amplification methods Analysis of Ab‐OriFluo performances Structural characterization, for enabling data analysis Application of Ab‐OriFluo to micro‐samples of solid tumours 112 Educational Activity foreseen I will improve my knowledge in the field of DNA nanostructures by studying literature about their synthesis and biomedical application and by taking part to meetings, seminars and courses. At the moment I plan to participate to: -Interdisciplinary spring school (7-8 March 2013, Udine) -Summer school on nanotechnology (usually first week of July, Trieste) -One of the following International conferences: o“Self-Assembly & Supramolecular Chemistry” (Gordon Research Conferences), May 5-10 2013, Les Diablerets-Switzerland; o“BioPhotonics & Imaging Conference BioPIC 2013” (The National Biophotonics and Imaging Platform, Ireland), March 25-27 2013, Dublin-Ireland; o“Nanomedicine 2013 (Select Bioscience), April 11-12 2013, Barcellona-Spain; o“NanoBioeurope 2013 Conference” (NanoBioeurope), June 10-12 2013, ToulouseFrance. So far I participated to the Annual Meeting of PhD School in Nanotechnology (9-11 January 2013) and I’m taking an English course provided from CRO – Aviano. CANDIDATE ILENIA D’AGOSTINO Email: ILENIA.D’[email protected] Title of the thesis: “Biopolymer based matrices for encapsulation and delivery of nutrients typical of the mediterranean diet.” Laboratory: 244 Supervisor: Dott.ssa A. Gamini Tutors (if any): Research Activity foreseen State of the art and motivation An increasingly important determinant in food choice is the growing consumer concern about nutrition and health. This focusing on consumer interest on the food supply, and also extensive research and technological developments in food science will provide further opportunities for new products developments. The Food-based Dietary Guidelines of the World Health Organisation and European Union legislation on health claims play an important role in regulating information about a wholesome diet [1]. In food field there is an increasing attention towards use of specific biopolymers to optimize the release of special nutritions. Food grate biopolymer such as protein and polysaccharides can be used to create a diverse range of delivery systems suitable for encapsulating, protecting, and delivering lipophilic functional components such as omega-3 rich oils, conjugated linoleic acid (CLA), oil soluble vitamins, flavors, colors, and nutraceuticals. There are many different approaches that can be used to create structured delivery systems based on biopolymers including molecular complexation, coacervation, thermodynamic incompatibility, moulding and extrusion method [2]. The research project is aimed to the preparation and the study of supramolecular systems made by polymers, polymer particles or vesicles able to release proteins or other nutrients typical of the Mediterranean diet. The apparent ability of the Mediterranean diet to reduce the risk of development of cardiovascular disease, cancer and degenerative disease has been attributed in part to the content of nutrients as α-tocopherol, ascorbic acid, retinol, β-carotene. The constant presence of fruits and vegetables, virgin oil, red wine, aromatic herbs and garlic, onion and chilli, ensures the intake of phenols, polyphenols, flavonoids, isoflavonoids, phytosterols, terpenes, monounsaturated and polyunsaturated fatty acid. But there are any conditions in which there is a difficult to provide an adequate nutrition as in case of intolerance or allergy towards a compound, in other situation of stress or in particular case as in oldness in which there is a natural vitamins deficiency and a high proteins-calories supply is necessary, or in specific disease in childhood. Particular attention will be given to the use of biopolymer as matrices suitable for encapsulation of nutrients to improve their absorption, bio-availability and environmental stability. The first steps of the project will be addressed to the characterization of several types of biopolymers like alginate, scleroglucan, chitosan or starch able to exhibit properties suitable for nutrients loading and release. We will study the biopolymer-biopolymer interaction to check Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 114 thermodynamic compatibility since low mixing entropy of large size molecules is responsible for their incompatibility in common solvents. The general condition for compatibility is an exotermic mixing process i.e. the formation of soluble biopolymer-biopolymer complex [3]. There are many numbers of factors that must be considered when selecting a suitable polysaccharide or a combination of polysaccharides to fabricate a biopolymer-based delivery system. It is important to establish the environmental and medium conditions favoring supramolecular structures formation. This usually requires knowledge of physicochemical properties of the polysaccharides involved, such as helix coil transition temperatures, electrolyte properties, sensitivity to specific monovalent or multivalent ions or susceptibility to enzyme or chemical reactions [4]. In some cases is possible that a mixture of polymers causes a change on the behavior of the components. This modification can active a process of sequestering essential components from the solution in which polymers are immersed as we have observed in a mixture of chitosan and alginate immersed in milk. In fact an important aspect is the study of the specific interaction between polymers and active molecules (nutrients) as proteins, peptides, vitamins and so on leading to stable polymer-nutrient complex. Biopolymers in biological environment have to satisfy important requirements such as biocompatibility and biodegradability as well as to be neither toxic nor immunogenic. Bioactive compounds have different characteristics in terms of molecular structure, molecular weight and polarity, ranging from polar to amphiphilic to non polar species. Therefore the delivery system has a vital role in preventing and/or increasing the bioavailability of an added bioactive compound. A delivery system must than protect the functional ingredient from biological or chemical degradation that may occur during processing, storage, and consumption (oxidation, hydrolysis); must as well control the release of the nutrient at the target site of the body (pH, ionic strength, temperature) and be compatibility with the bioactive compound. References: 1) Nehir El S. and Simsek S. Food Technological Applications for optimal nutrition:an overview of opportunities for the food industry, Comprehensive Reviews in Food Science and Food Safety, Vol. 11, 2012 2) Matalanis A, Griffith Jones O. and McClements D. J. Structured biopolymer-based delivery systems for encapsulation, protection, and release of lipophilic compounds, Food Hydrocolloids 25 (2011) 1865e1880 3) Tolstoguzov V. Why were polysaccharides necessary Nestlè research center 4) BeMiller, J. N., & Whistler, R. L. (1996). Carbohydrates. In O. Fennema (Ed.), Food chemistry. New York, NY: Marcel Dekker, Inc. Objectives for the three years The project is aiming to the development of suitable biopolymers based matrices for the up-take and the delivery of specific nutraceuticals. • Test and optimize the procedures to develop nano-gels, emulsions, polymer particles and solid matrices exploiting polymer-polymer and polymer-nutraceutical interactions. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 115 • Characterize the systems in terms of size, structural inhomogeneities and physicochemical properties. • Study of the stability and the delivery properties of the developed systems as a function of environmental conditions like temperature, pH or enzymes. Objectives for the first year The first year is dedicated to a theoretical approach to the nanosystem and their application in food field and a practical approach to the learning of the principal procedures and techniques for the preparation and the characterization of the systems. The main objective is to select the biopolymerbioactive compound systems that show the most promising features in terms of stability, compatibility and releasing ability. Research project The Project is based on the study of biopolymers behavior and their capacity to release nutrients. The programme can be summarized in: I.Characterization of the biopolymers and of their functionalized derivatives (DSC, viscometry, spectroscopic techniques) II.Study of the polymer-polymer and polymer-bioactive compound interactions. Study the thermal behavior of polymers and their compatibility with nutrients (DSC, Surface Plasmon Resonance, spectroscopic techniques, SAXS, NMR). III.Development of biopolymer based nano- and micro-systems. IV.Study of the physicochemical properties of the biopolymer-based matrices as their morphology, physical properties, size and charge (as a function of pH, ionic strength, temperature) because these factors will determine how the particles may impact stability and functional characteristics (SEM, TEM, IR, NanoTracking). V.Rheological characterization to study of the viscoelastic properties of the components. VI.Study of the nutrient diffusion in the polymer network (spectroscopic techniques, NMR). VII.Test of the different structures of the final products to select those that show good performances in terms of environmental stability. The possible structures include polymer films (also multilayer), scaffolds, polymeric particles (self assembled) and vesicles (or liposomes). VIII. The study of the terms and conditions for the release of bioactive compounds (spectroscopic techniques, HPLC, capillary electrophoresis. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 116 Years1 Activities 3 6 Years2 Years3 9 12 15 18 21 24 27 30 33 36 LITERATURE RESEARCH EDUCATIONAL ACTIVITY CHARACTERIZATION OF BIOPOLYMERS AND NUTRIENTS PREPARATION OF BIOPOLYMER MATRICES RHEOLOGICAL CHARACTERIZATION OF BIOPOLYMER MATRICES FUNCTIONALISATION OF BIOPOLYMER MATRICES STUDY OF BIOPOLYMER-NUTRIENTS INTERACTION INSTRUMENTAL CHARACTERIZATION WITH DSC, DLS, SAXS,SURFACE PLASMON RESONANCE, NMR, RHEOLGY, NANOTRACKING, IR, HPLC, UV-vis, CD STUDY OF THE RELEASE OF BIOACTIVE COMPOUNDS PAPER WRITING Educational Activity foreseen Courses : •Chimica delle sostanze organiche naturali (Forzato) •Biopolimeri (Rizzo) Schools : •Interdisciplinary Phd Spring School (7-8 March 2013) •X Scuola di Reologia (8-12 September 2013) Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 117 CANDIDATE: MATTEO DE BIASI Email: [email protected] Title of the thesis: Study of nanostructured dental materials and nanometric relationship between dental materials and dental tissues. Laboratory: Research Laboratory of the Dental Clinic, Dental Clinic, University Department of Medical, Surgical and Health Sciences, Piazza Ospedale 1 Supervisor: Prof. Daniele Angerame Research Activity foreseen State of the art and motivation Nanotechnology is one of the most recent and innovative field of study in dental research (1). In particular, the development of nanostructured dental materials and the study of the nanostructure of already available dental materials have started promising lines of investigation. In dentistry, composite resins constituted by inorganic fillers (e.g. glass, quartz or ceramic particles) embedded in an organic resin matrix consisting of a mixture of dimethacrylates, are used for tooth restoration. Composite resins were introduced in dentistry during the Nineteen Sixties and underwent a substantive evolution during the following decades. One of their major changes concerns the reduction of the filler particle size, so that nanofilled composites, with a filler size ranging from 5 to 100 nm, have been nowadays developed and introduced in the dental practice (2,3). Some authors advocate their use because of improved aesthetical and mechanical properties compared to conventional packable composites (2,4,5). The nanofilled composites category is heterogeneous and filler particle size is not the only significant factor in determining the material’s mechanical performance (2). The resistance to surface wear and degradation plays a key role in the success of restorative dentistry, which aims to avoid recurrent caries and other complications. For these reasons, the identification of the best materials among those available on the market has relevant clinical implications. In implant dentistry the modification of the implant surface to promote the osseointegration represents a remarkable matter of study and debate. There is general agreement that micro-rough implants are more effective than smooth ones in terms of bone-to-implant contact rate and retention into the bone (6); clinical data confirm this trend (7). Surface topography modifications at a nanoscale level constitute a recent frontier and the information about their possible benefits and limitations appears to be still insufficient. Consequently, this issue needs further laboratory and clinical investigations. A very recent article about the physicochemical properties of nanomodified mineral trioxide aggregate reports reduced setting time and increased microhardness even at lower pH values after hydration (8), thus opening new research possibilities also in endodontics. 1.Ozak ST, Ozkan P. Nanotechnology and dentistry. Eur J Dent 2013; 7: 145-51. 2.Papadogiannis DY, Lakes RS, Papadogiannis Y, et al. The effect of temperature on the viscoelastic properties of nano-hybrid composites. Dent Mater 2008; 24: 257-66. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 118 3.Moszner N, Klapdohr S. Nanotechnology for dental composites. Int J Nanotechnol 2004; 1: 13056. 4.Mitra SB, Wu D, Holmes BN. An application of nanotechnology in advanced dental materials. J Am Dent Assoc 2003; 134: 1382-90. 5.Beun S, Glorieux T, Devaux J, et al. Characterization of nanofilled compared to universal and microfilled composites. Dent Mater 2007; 23: 51-9. 6.Shalabi MM, Gortemaker A, Van't Hof MA, et al. Implant surface roughness and bone healing: a systematic review. J Dent Res 2006; 85: 496-500. 7.Balshe AA, Assad DA, Eckert SE, et al. A retrospective study of the survival of smooth- and rough-surface dental implants. Int J Oral Maxillofac Implants 2009; 24: 1113-8. 8.Saghiri MA, Asgar K, Lotfi M, Garcia-Godoy F. Nanomodification of mineral trioxide aggregate for enhanced physiochemical properties. Int Endod J 2012; 45: 979-88. Objectives for the three years The research activity will be focused on the characterization of nanostructured dental materials by direct laboratory and/or clinical research: (i) to study the surface characteristics and degradation of dental restorative materials, such as nanofilled and/or nanohybrid composite resins and ceramics; (ii) to define the clinical implications of the use of dental implants with nanostructured surface topography. A further objective might be the nanometric analysis of dental materials, e.g. mineral trioxide aggregate or its nanomodified counterpart, under particular experimental condition, such as in case of pH variations. Objectives for the first year The first year will be mainly devoted to deepen the knowledge in nanostructured dental materials and surfaces, with particular attention to restorative, prosthetic and implant dentistry. Ongoing in vitro and in vivo experimentations about the surface degradation of a nanohybrid flowable composite resin will be monitored and preliminary data will be gathered. The possibility to apply systematic reviews and meta-analyses to the field of dental nanotechnology will also be taken into account. Research project The surface deterioration of composite resins will be evaluated by profilometric analysis and scanning electron microscope observation of positive resin replicas of specimens either aged in vitro or under clinical conditions (i.e. after being applied to the tooth surfaces of volunteer subjects). The use of other instruments (transmission electron microscope, small-angle X-ray scattering, and atomic force microscope) to evaluate further characteristics of nanostructured dental materials or conventional materials at a nano-scale level will be discussed with the Supervisor and, if needed, included in the research project. The Gantt chart is given as attachment. Educational Activity foreseen During the first year I am going to perform extensive study of the literature concerning nanostructured dental materials in the fields of restorative, prosthetic, implant dentistry and endodontology. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 119 Furthermore, I have been to/I plan to attend the following national and international meetings/courses on dental materials and related topics: 1.Metodologia della ricerca e preparazione di un lavoro scientifico in ortodonzia: corso intensivo teorico-pratico, Florence, 28th and 29th January 2.17° Congresso Nazionale della Società Italiana di Odontoiatria Conservatrice, Rome, 15th17th February 3.Corso di alta formazione – La letteratura in ambito di ricerca scientifica: come leggerla, interpretarla, selezionarla e proporla, Due Carrare (PD), 2nd March 4.20° Congresso Nazionale dei Docenti di Odontoiatria, Rome, 18th-20th April 5.46th Meeting of the Continental European Division of the International Association for Dental Research with the Scandinavian Division, Florence, 4th-7th September 6.16th European Society of Endodontology Biennial Congress, Lisbon, 12th-14th September 7.32° Congresso Nazionale della Società Italiana di Endodonzia, Bologna, 8th-10th November Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 120 FABIO DEL BEN Email: [email protected] Title of the thesis: A bridge between the electrical and mechanical signature of cancer. Laboratory: Nanomedicine - Udine Supervisor: Giacinto Scoles (Uniud) Tutors (if any): Scaini Denis (Units) Research Activity foreseen State of the art and motivation The field of bioelectrical signaling is focused on the link between cell biology and electrical events. One of the main values of bioelectrical signals the electrical potential difference across plasma membranes (Vmem)1. Vmem is the result of the complex activity of a lot of different trans-membrane ion channels (Na+, K+, Cl-) and its values change from cell to cell, maintaining a general pattern of high values in non-proliferating cells (e.g.: muscle and neurons) and low values in highproliferating, stem cells and cancer cells; it also displays fluctuations through the cell cycle. There is evidence that changes in Vmem value can affect cell proliferation and differentiation1,2. It’s worth noting that the biological effect is not linked to the particular ion channel affected, but to the final change in Vmem value1. Nowadays methods applied to change Vmem are modulation of ion channels through different approaches (pharmacological, knockout genes, siRNA) and patch-clamp. Since there are a lot of feedback loops between ion channels and cell functions, we don’t know precisely the Vmem value obtained by inhibiting a channel; furthermore, we don’t know if the channel is part of a signaling cascade: we could disrupt important pathways knocking it out. Besides this, ion channel expression and Vmem are not necessarily linked: there can be the same Vmem value in different patterns of ion channels, and there are different Vmem with the same expression of channels. Patch-clamp approach is a single-cell technique, challenging and most likely leaving the cell damaged and dying in few hours. For these reasons we think that the best way for our purposes is to modify directly Vmem in a cell population, without modifying ion channel expression, keeping the cells viable long-term: a recent solution is using micro-electrode arrays (MEAs) coupled to nanostructures allowing for direct intracellular electrical stimulation. Nanostructured that gave the best results are gold mushroomshaped microelectrodes (gMµEs) or vertical nanowire electrode arrays (VNEA). In particular, gMµEs functionalized with RGD-based peptide provide multisite, simultaneous, intracellular recording and stimulation for periods of (at least) days without damaging the cells3. We know that cancer cells are softer than normal cells4, and our aim is to assess whether the electrical and mechanical properties of cell membranes are linked, using atomic-force microscope (AFM) to monitor the stiffness while we keep Vmem value close to the healthy one. If the membrane stiffness can be reverted to normal values, we want to evaluate if other malignant features can be reverted as well with this technique (E.g.: morphology, proliferation, gene expression). Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 121 1. 2. 3. 4. Levin, M. & Stevenson, C.G. Regulation of cell behavior and tissue patterning by bioelectrical signals: challenges and opportunities for biomedical engineering. Annual review of biomedical engineering 14, 295-323 (2012). Blackiston, D.J., McLaughlin, K.A. & Levin, M. Bioelectric controls of cell proliferation: ion channels, membrane voltage and the cell cycle. Cell cycle 8, 3519-3528 (2009). Spira, M.E. & Hai, A. Multi-electrode array technologies for neuroscience and cardiology. Nature nanotechnology 8, 83-94 (2013). Cross, S.E., Jin, Y.S., Rao, J. & Gimzewski, J.K. Nanomechanical analysis of cells from cancer patients. Nature nanotechnology 2, 780-783 (2007). Objectives for the three years -To establish a robust technique able to detect and control Vmem, using nanostructures and MEAs. -To define precise stimulation patterns able to: oChange stiffness of cells oArrest cancer cells at different cell cycle checkpoints -Additional tasks (regenerative medicine) oIncrease cell proliferation, especially of cells not normally cycling (neurons, cardiomyocytes) oA guide to stem cell differentiation. Objectives for the first year -To establish the best method to stimulate the cells. -To learn to use AFM -To learn to use MEAs and stimulation/recording techniques Research project Activities: -Isolation of cells from tumoral tissues and cell culture -Electrophysiology -AFM microscopy -Optical/fluorescence microscopy -Cell cycle labeling methods (e.g.: FUCCI method) -Gene expression (RT-PCR, immunostainings) -Single cell analytical techniques Tasks: -To culture cells on MEAs with nanostructures -To monitor and modulate Vmem -To track cell stiffness in response to Vmem changes. -To track cell cycle/proliferation in response to Vmem changes. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 122 Educational Activity foreseen Linz, 15-18 Feb 2013 – XV Annual Winter Workshop, Advances in Single-Molecule Research for Biology and Nanoscience (12-14 Feb 2013 – Hands on Winter school) Cycle of lectures on intermolecular forces held by prof. Giacinto Scoles. Experiences in other labs. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 123 ISMAEL ROMERO OCAÑA Email: [email protected] Title of the thesis: “Nanomaterials for Solar Fuels” Laboratory: “Department of Chemical and Pharmaceutical Sciences” Supervisor: Prof. Paolo Fornasiero Tutors (if any): Dr. T.Montini , Dr. J.J. Delgado Research Activity foreseen State of the art and motivation It is unquestionable that one of the most important challenges of our society is the development of new energy strategies to tackle global warming and the exhaustion of fossil fuels. Therefore, the design of innovative low-cost and environmentally friendly energy storage and conversion systems is crucial for stable economic growth in a world whose energy needs are continuously increasing. In this context, catalysis has been proven as a critical enabling science for developing the use of alternative feedstocks, such as biomass or hydrogen, and increasing energy production efficiency. Sunlight is one of the most abundant renewable and clean energy sources in the world. For this reason, the research community has intensely studied how to use it for developing sustainable energy production technologies. Unfortunately, conventional photovoltaic cells have the inconvenience of their high production costs and daylight-dependency. In this context, Photocatalytic fuel production has recently emerged as a promising approach to face the sustainable energy production and more importantly its storage. Since the discovery of photocatalytic splitting of water to produce hydrogen by Fujishima and Honda in 1972, [1] the approach have been extended to the bio-alcohols photo-reforming and carbon dioxide reduction to carbon fuels. The last option, so called synthetic photosynthesis, has the advantage of CO2 carbon capture and sequestration. In addition to the production of carbon-neutral fuels, they can be directly used in actual energy production systems in the residential, industrial and transportation sectors. It should be pointed out that although the efficiency of water splitting and CO2 photoreduction using solar radiation is poor, it is one of the most challenging tasks of environmental catalysis and the US Department of Energy (DOE) has identified it as one of their priority research directions. The DOE have suggested that efficiency higher than 10% should be reach to guarantee the successful implementation of photocatalysis devices. At the present time, the most active photocatalyst show a very poor efficiency of 1-5%. In this sense, traditional photocatlysts, such as TiO2, commonly requires Ultraviolet light, so using only around 4% of the sunlight. Therefore, it is desirable to develop active catalysts that harvest a wide spectrum of the solar light irradiation, improving the catalyst efficiency. The main aim of this project is to design new plasmonic TiO2-based photocatalysts for harvesting visible light, which covers 43% of the sunlight. In this sense, it is well-known that noble metal nanoparticles (Au, Ag, Pt, etc) can strongly absorb visible light [2] due to their unique Surface Plasmon Resonance (SPR) properties. These noble-metal nanoparticles are able to transfer Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 124 photogenerated electrons to a metal-semiconductor and promote the generation rate of e-/h+ pairs in the semicoductor. This configuration is obviously a promising photocatalyst that can efficiently operate under visible light. The optical properties of some metal nanoparticles, such as Au and Ag, (AuNPs) are dominated by Surface Plasmon Resonance (SPR) effects, which can be defined as the collective oscillation of the conduction electrons induced by light irradiation [3,4]. The synergy effect of the metal NP-semiconductor is illustrated in figure 1 for the Ag/AgBr photo-catalyst. Figure 1. The synergy effect of metal NP-semiconductors [adapted from 8] Objectives for the three years The main objective of this project is the evaluation of the effect of different Au and Ag nanoparticle architectures on the absorption properties of a number of TiO2 semiconductors with different morphology (core-shells, cubes, rods, pyramids, etc.) and sizes. In the case of the TiO2 semiconductors I would pay especial attention to bi-dimensional nanoparticles to decrease the e-/h+ recombination rate. Another of the central goals of this project is the development of supra-structured systems where the most active metal-semiconductor configurations will be immobilized. This step is crucial before real application. The work will be focused on the use of carbonaceous materials due to their unique and controllable morphology and structural-electrical properties [9] Objectives for the first year First year 9Synthesis of morphologically controlled TiO2 nanoparticles, paying special attention to one and two dimensional nanoparticles with high crystallinity degree to reduce e-/h+ recombination. I will take advance of my knowledge in the synthesis of nanostructured catalysts by solvothermal methods to successfully achieve this task. 9Synthesis of morphologically controlled Ag, Au and Ag-Au nanoparticles with enhanced SPR. I will pay special attention to those system previously reported in the literature such as metal-dielectric-metal (MDM) structures and double concentric nanoshells (DCNs). 9Sub-nanometric characterization of nanoparticles by mean of Advanced Electron Microscopy Techniques, such as SEM, HRTEM, HAADF-STEM using associated XEDS and EELS detector for chemical analysis. Research project. The methodology proposed for achieving the previously describe reach objective are based on the following four pillars: Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 125 1) Synthesis of novel nanomaterials, including the preparation of morphologically controlled nanoparticles and hierarchically ordered nanomaterials taking advanced of the SPR properties of noble metal nanoparticles. 2) Catalytic evaluation of water splitting and CO2 reduction under realistic conditions to evaluate the deactivation process and the effect of the reaction parameter in both activity and selectivity. 3) Advanced characterization of the catalysts, preferentially, under operation conditions using TEM, IR and light absorption techniques. Structural, morphological and compositional study of the newly developed materials at subnanometric scale will be studied by both High Resolution Transmission (HRTEM) and Scanning Transmission (STEM) Electron Microscopy. A number of analytical techniques, such as XEDS and EELS, will be used to provide information about the composition and electronic structure of the samples, including the plasmon properties of the metal nanoparticles. Importantly, these techniques will allow us to determine the interactions between all the elements of the complex multicomponent photo-catalysts. In addition, a model of the nanoparticles will be obtained by combining experimental STEM-HAADF and HRTEM images with nano-structural modeling and images simulation techniques. This model will be useful for theoretical calculations. 4) Use of advanced theoretical and computational methods to fully understand the catalytic behavior and propose new formulations. This will be carried out in collaboration with other international lab. In particular, the intensified electric field at the interface between the metal particles and the subdomain on TiO2 would be studied by Finite Element Method (FEM) electromagnetic simulation. My research plan has the aim of solving real problem existing in the implementation of Photocatalysis for sustainable energy production. For this reason, patenting results will be a priority. Therefore, research results will only be published after an initial review of their potential for patenting and commercial exploitation by the inventors, the local patent and technology units and eventual industrial partners. In order to reinforce this objective, I will be trained in knowledge transfer skills, which would facilitate the identification of patentable results. Presentation of oral and poster communications in conferences, and publication of scientific papers in high impact journals will also be one of my priorities Educational Activity foreseen Sub-nanometric characterization of nanoparticles by mean of Advanced Electron Microscopy Techniques, such as SEM, HRTEM, HAADF-STEM using associated XEDS and EELS detector for chemical analysis will carry out at the University of Cadiz (Spain) sunder the supervision of Dr. J.J. Delgado at the “Structure and Chemistry of Nanomaterials” group. Plasmon characterization of metal NPs will be carried out by EELS technique. Activities of the PhD School. Conferences. Clasification Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 126 1.- B1; B3; B4; F1; F3; F4; F15; F16; F17 2.- F (Energy& Environment) References 1. A. Fujishima and K. Honda, Nature, 1972, 238, 37-38. 2. Peng Wang, Baibiao Huang, Ying Dai and Myung-Hwan Whangbo, Phys. Chem. Chem. Phys., 2012, 14, 9813-9825. 3. A. Merlen, V. Gadenne, J. Romann, V. Chevallier, L. Patrone and J. C. Valmalette, Nanotechnology, 2009, 20, 1-7. 4. D. J. Wu, X. D. Xu, X. Liu, J. Solid State Commun. 148, 163-167, 2008. 5. P. Wang, B. B. Huang, X. Y. Qin, X. Y. Zhang, Y. Dai, J. Y. Wei and M.-H. Whangbo, Angew. Chem. Int. Ed., 2008, 47, 7931–7933. 6. H. Zhang, X. F. Fan, X. Quan, S. Chen and H. T. Yu, Environ. Sci. Technol., 2011, 45, 5731–5736. 7. W. Liu, W. B. Hou, P. Pavaskar, M. Aykol and S. B. Cronin, Nano Lett., 2011, 11, 1111–1116. 8. Jing Jiang, H. Li and L. Zhang, Chemistry A European Journal, 2012, 18(20), 6360–6369. 9. R. Leary and A. Westwood, Carbon, 2011, 49, 741-772. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 127 Graduate student LUCA OMICIUOLO Email: [email protected] Title of the thesis: Study of the growth processes and of the physical and chemical properties of graphene-based low dimensional systems Laboratory: Surface Science Laboratory (Physics Department – University of Trieste, Elettra Sincrotrone Trieste) and SuperESCA beamline at Elettra. Supervisor: Prof. Alessandro Baraldi Co-supervisor: Dr. Silvano Lizzit • Research Activity foreseen State of the art and motivation Since its first isolation in 2004 [K.S. Novoselov et al., Science 306, 666 (2004)] graphene, a single layer of carbon atoms arranged in a honeycomb lattice, has been the subject of a number of scientific publications. This staggering interest is motivated by the outstanding properties of this material. In particular, the valence and conduction bands of graphene show a unique conical shape at the high-symmetry points of the first Brillouin zone, leading to a linear E(k) energy dispersion for electrons near the Fermi energy [K.S. Novoselov et al., Nature 438, 197 (2005)]. This linear dispersion is qualitatively identical to that of ideal massless fermions and is responsible for a series of unusual electronic transport properties, making graphene extremely interesting for application in nano-electronic devices [A.K. Geim et al., Nature Materials 6, 183 (2007)]. This is why reliable methods for large-scale, high-quality graphene synthesis are needed. A promising way for mass production of high quality carbon layers is the epitaxial growth of graphene on transition metal surfaces [X. Li et al., Science 324, 1312 (2009)]. The problem, in this case, is that graphene grown on metal surfaces generally interacts strongly with the substrate, so that most of its peculiar properties are lost [A.B. Preobrajenski et al., Phys. Rev. B 78, 073401 (2008)]. One way to overcome this drawback is to remove the substrate by chemical etching, once the layer is formed, but this method poses a series of difficulties, and leads to low quality graphene layers due to the high concentration of point and extended defects, such as vacancies, grain boundaries and multiple domains. Figure 1: Synthesis of SiO2 under epitaxial graphene on Ru(0001). Each process step is schematically illustrated. [S. Lizzit et al., Nano Lett. 12, 9 (2012)] A valid alternative to this procedure consists in the epitaxial growth of graphene on metal surfaces, and subsequent oxidation of the substrate below the carbon layer. As a matter of fact, a number of studies have shown the possibility to intercalate various atomic species underneath graphene layers. In the recent years, our research group has developed a new method to synthesize Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 128 graphene on SiO2 [S. Lizzit et al., Nano Lett. 12, 9 (2012), see also the comments on Research Highlights, Nature Nanotech 7, 613 (2012)]. After intercalation of Si atoms under a well-ordered graphene layer grown on ruthenium substrate, the Silica layer below graphene was obtained by direct oxidation of the Si interface. The development of new efficient procedures to grow high quality, large-scale, graphene layers directly on dielectric material with tunable interaction, would be extremely useful for fundamental studies on quasi free-standing graphene, and it would a primary requirement for fabrication of graphene based nano-electronic devices. Objectives for the three years The main objectives of my PhD research program are the comprehension of the physical and chemical properties of epitaxial graphene grown on different monometallic and bimetallic surfaces, and the development of techniques to decouple it from the substrate, by means of atomic intercalation and/or subsequent selective oxidation. Beside that I will also be involved in the other research activities carried out in our laboratory, with the goal to obtain graphene functionalization by means of metal nanoclusters deposition, using a mass-selected nanoclusters source which is currently under commissioning. Here is a list of the main issues I'm going to deal with: . structural and electronic characterization of epitaxially grown graphene on transition metals and bi-metallic surface alloys; . carbon layers decoupling from metal substrates by intercalation of various atomic species, or by direct substrate oxidation; . graphene functionalization by means of mass-selected nanoclusters ; . investigation of the structural, electronic and chemical properties of nanoclusters supported on epitaxial graphene. Objectives for the first year During the first year of my PhD I'm going perform a part of the activities listed above, in particular: . characterization of epitaxial graphene growth on the Ni3Al(111) bi-metallic alloy surface and selective Al oxidation by intercalation of oxygen. The GR/Al2O3/Ni3Al properties will be investigated by means of diffraction techniques (LEED), photoelectron spectroscopy (XPS) and angle-resolved photoelectron spectroscopy (ARPES). . oxidation of transition and noble metal clusters supported on epitaxial graphene. Research project Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 129 As already anticipated in the previous paragraphs, my work will be aimed to two main issues: epitaxial growth of graphene on transition metal and bi-metallic alloy surfaces, and selective oxidation of the substrate below the carbon layer. More precisely, due to their heavy use in electronics, Fe, Si, Al, Zr and Ti oxides are very interesting substrates, and it would be extremely useful to produce high quality graphene layers grown on these oxides. Unfortunately it is not possible to grow graphene directly on oxide surfaces by using chemical vapour deposition. One way to overcome this obstacle is to use, as a substrate, transition metal surface alloys containing the mentioned atomic species, such as, for example, NiAl and FeAl surface alloys. As a matter of fact, transition metal surfaces are known for their catalytic properties for hydrocarbons dissociation, which can be exploited to grow extended high quality carbon layers. Therefore, our goal will be to characterize graphene grown on such bi-metallic surface alloys and then to selectively oxidize the atomic species at issue by means of oxygen intercalation under the carbon layer. Another strategy that will be followed to obtain graphene supported on oxide thin layers, consists in intercalation of various atomic species underneath the carbon layer followed by selective oxidation of these species. Moreover I will join my laboratory group in the setup of a mass-selected nanoclusters source which, once completed, will be a unique experimental apparatus in the national research landscape. This machine will allow us to study physical and chemical properties of transition and noble metals nanoclusters as a function of their dimensions. Finally I will spend few months with the research group headed by Prof. Ph. Hofmann at the Aarhus University in Denmark. This laboratory is somehow complementary to ours, being specialized in valence band photoelectron spectroscopy, while both the Surface Science Laboratory and the SuperESCA beamline are focused in core level photoelectron spectroscopy and photoelectron diffraction. To deeply investigate all these system I will rely on state-of-the-art experimental techniques, in particular: X-ray Photoelectron Spectroscopy (XPS) and X-ray Photoelectron Diffraction (XPD), both from conventional sources and from synchrotron radiation, Low Energy Electron Diffraction (LEED) and Angle Resolved Photoelectron Spectroscopy (ARPES). Beside that, our research group has a productive collaboration partnership with the group of Prof. Dario Alfè at the University College of London, who will provide Density Functional Theory (DFT) calculation to support our experimental work. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 130 1st year SCHEDULED ACTIVITIES 2nd year 3rd year 1st term 2nd term 1st term 2nd term 1st term 2nd term Growth and properties of epitaxial graphene Graphene on NiAl alloys Graphene on Ti-based alloys Graphene on FeAl alloys Graphene supported nanoclusters Chemical reactivity of transition metal nanoclusters supported on epitaxial graphene Chemical reactivity of noble metal nanoclusters supported on graphene • Educational Activity foreseen During the first year I will attend schools, seminars and courses focused on increasing my knowledge, both at the theoretical and experimental level, on topics related to my research activities. Both ELETTRA and the IOM-CNR TASC Laboratory regularly hold seminars on this topic, moreover several theoretical seminars on graphene and low-dimensional systems periodically take place also at the ICTP and at SISSA and I'm going to attend them. Lecture activities will be complemented by the reading of subject-specific papers and reviews, to keep myself up to date in the fields related to my research project. Moreover I'm going to attend several courses on data acquisition and analysis software, such as LabView, Igor Pro and Cad, held at the Elettra synchrotron radiation laboratory. Finally, during the period at the Aarhus University, I expect to attend some subject-specific lectures on electronic structure in condensed matter. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 131 LAERTE LUIGI PATERA Email: [email protected] Title of the thesis: “An in-situ and in-operando study of graphene growth and properties on metal surfaces” Laboratory: IOM-CNR, TASC Laboratory Supervisor: Dr. Cristina Africh Research Activity foreseen State of the art and motivation Write a description of the state of the art and the motivations for the research project, justifying particularly all aspects related to nanotechnology. Please keep the description in one page maximum, including graphs, literature and tables. Please do note modify characters and paragraphs settings of the present document. Graphene1, a single layer of graphite, has recently focalized the attention of physicists, chemists and engineers for its electronic and structural properties2,3. Electrons in graphene obey a linear dispersion relation and behave like Dirac massless relativistic particles, leading to peculiar electronic properties such as the quantum Hall effect, ambipolar electric field effect, good optical transparency. Due to its huge carrier mobilities (200.000 cm2/Vs), high thermal and electrical conductivity, graphene based devices can potentially change semiconductor electronics for nanoelectronics applications4 and in the gas sensors field5. One of the most promising techniques for producing high-quality single layers of graphene is Chemical Vapour Deposition (CVD), using hydrocarbons as C feedstock and the surfaces of transition metals as catalyst for its decomposition, like Cu(111), Ru(0001), Ir(111), Ni(111), Pt(111), Co(0001) and Rh(111)6. At the moment, the state of art to fabricate low cost / mass production suitable graphene is reached with catalytic copper surfaces, because of the low C solubility and the small mismatch between graphene and Cu(111) lattices (≈4%), that lead to large areas of high quality monolayer graphene7. However, the high temperatures needed to dissociate hydrocarbons (≈1000°C), close to the melting point of copper, cause a sublimation of the substrate and a surface faceting. For these reasons, other substrates such as bimetallic alloys8 and nickel surfaces9 are been attracting attention because of the possibility to grow graphene at lower temperature (400-600°C). Despite this, graphene uniformity and layer control over large areas remain very difficult to achieve on this kind of substrates and a clear comprehension of the growth mechanisms and of the influence of parameters as temperature, hydrocarbon pressure and C concentration into the sample is missing at the moment. So, further efforts to shed light on how to control graphene quality through the CVD parameters are needed. In addition, the possibility to grow graphene with tunable chemical activity, through defects engineering, is very promising for the heterogeneous catalysis field, but, a deeper understanding of the correlation at the atomic scale between defects and chemical properties is still needed. (1) Geim, A.; Novoselov, K. Nature materials 2007, 183–191. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 132 (2) Chen, Z.; Lin, Y.; Rooks, M.; Avouris, P. Physica E: Low-dimensional … 2007, 40, 228–232. (3) Schedin, F.; Geim, A. K.; Morozov, S. V; Hill, E. W.; Blake, P.; Katsnelson, M. I.; Novoselov, K. S. Nature materials 2007, 6, 652–5. (4) Schwierz, F. Nature nanotechnology 2010, 5, 487–496. (5) Hill, E. W.; Vijayaragahvan, A.; Novoselov, K.; Exfoliation, A. M. 2011, 11, 3161–3170. (6) Batzill, M. Surface Science Reports 2012, 67, 83–115. (7) Li, X.; Cai, W.; An, J.; Kim, S.; Nah, J.; Yang, D. Science 2009, 324, 1312–1314. (8) Weatherup, R.; Bayer, B.; Blume, R. Nano Letters 2011, 11, 4154–4160. (9) Kim, K.; Zhao, Y.; Jang, H.; Lee, S.; Kim, J. Nature 2009, 1–5. Objectives for the three years Write a description of the objectives to be reached in three years. Few lines and a bulleted list is sufficient. I am going to study graphene growth and properties on metal surfaces. Starting from model systems (single-crystal substrates, UHV), I intend to achieve a comprehension also in conditions typical of the industrial reactors for graphene and carbon nanotube CVD (poly-crystalline catalysts, higher hydrocarbons pressure), aiming to bridge both material and pressure gaps. In addition I will characterize different kinds of graphene grown on metal substrates, particularly focusing on electronic properties and chemical activity. The main steps are: •First year: study of graphene growth dynamics on single crystal surfaces by CVD, during exposure at low pressures of hydrocarbons (10-7 mbar range) and characterization of the graphene properties, like electronic structure and chemical properties. •Second year: extension of the understanding reached with model system to “real” conditions: graphene growth on poly-crystal surfaces. •Third year: investigation of graphene growth at higher hydrocarbon pressure (10-5-10-3 mbar range). Objectives for the first year Write a description of the objectives to be reached in the first year. Few lines and a bulleted list is sufficient. During this first year I will focus on the study of graphene growth on Ni substrates, starting from a model system such as a Ni(111) single crystal surface, trying to reach a control on graphene structural quality, through different growth mechanisms and CVD parameters. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 133 •Study of the correlation between growth parameters (temperature, hydrocarbon pressure, level of C contamination into the sample), growth mechanisms and graphene quality (defect density and structure, domain size). •Identification of reproducible recipes to obtain different kinds of graphene on Ni(111), by changing the CVD parameters, and characterization of the electronic and structural properties of the grown surfaces. •Investigation of the chemical properties of CVD graphene via controlled formation of defects and surface morphologies. Research project Write a description of the research program divided into activities and tasks, describing also the tools to be used. Include also a project Gantt diagram During my PhD, I aim at investigating graphene on metallic substrates in different CVD conditions, focusing on growth dynamics and electronic structure, and characterizing the physical/chemical properties induced by defects in the honeycomb lattice. The main steps are: 1.to follow the graphene growth by CVD under in-situ and in-operando conditions on metal surfaces, both for model systems (well oriented single crystals) and more “realistic” substrates (thin poly-crystalline films). 2.to study of the correlation between growth parameters, growth mechanisms and graphene quality. 3.to achieve recipes to obtain different kinds of graphene, changing the CVD parameters. 4.to understand how to control particular defect structures formation and to exploit their chemical properties, with particular attention to possible applications in heterogeneous catalysis. 5.to extend the expertise reached for low pressure CVD (10-7 mbar range) to higher pressure conditions (10-5-10-3 mbar range) trying to bridge the so-called “pressure gap”. In order to reach these goals, I will use some of the standard surface science techniques to investigate under in-situ and in-operando conditions the graphene formation, structures and properties. The main instrument that I will use during the PhD is a Variable Temperature Scanning Tunneling Microscope (VT-STM), which allows us to follow surface dynamics at high temperature and during gas exposure with atomic resolution. In addition, also electronic spectroscopies will be used, allowing for complementary information, especially X-ray Photoelectron Spectroscopy (XPS), Ultraviolet Photoelectron Spectroscopy (UPS) and Angle Resolved Photo-Electron Spectroscopy (ARPES). The activities that will be performed are the following: Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 134 1.Real time in-situ and in-operando measurements of graphene formation on Ni substrates during hydrocarbon exposure with both STM and XPS. 2.Characterization of the as-grown graphene morphology at the sub-nanometer scale with STM. 3.Photoelectron spectroscopy measurements to investigate the electronic band structures of the graphene layers grown by CVD. 4.High pressure CVD growth studies with in-situ and in-operando XPS measurements (available at “Bessy” synchrotron) and post-growth STM data. 5.STM characterization of the different defects morphologies on CVD-graphene. 6.STM and XPS investigations of the interactions between these defective structures and different adsorbates (e.g. CO, CO2, O2, water, etc…). 7.Creation of recipes to obtain graphene layers with a specific chemical activity. Educational Activity foreseen Write a proposal of the educational activity to be carried out during the first year. During the first year I will attend a LabView course. The motivation is that this software integrates a lot of tools that engineers and scientists need to build a wide range of applications like data acquisition and instrument control. I will also take part to several seminars, e.g. the ones organized at Elettra, at TASC laboratory and at the University , concerning topics useful to my project. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 135 ELENA PELLIZZONI Email: [email protected] Title of the thesis: Interatomics in tumor cells studied with a nanotechnology approach Laboratory: 330-333, dept. of chemical and pharmaceutical science Supervisor: Giuseppe Toffoli Tutors (if any): Federico Berti, Flavio Rizzolio Research Activity foreseen State of the art and motivation The aim of this project is the identification, preparation and characterization of artificial or biological binder molecules to be used as sensing elements for the development of innovative nanobiosensors to apply in cancer therapies. The target are three anticancer drugs: paclitaxel 1a, irinotecan 2a and sunitinib 3a. 3b: R = CH2CH 2CH 2CH2NEt2 , R' = N N N 4 3c: R' = H, R = -(CH2 )5NH 2 O Scheme 1 The narrow therapeutic indices and the inter-individual pharmacokinetic variability of anticancer drugs, cause many sides effects leading poor patient compliance and decreasing the efficiency of the therapy. In this frame, Therapeutic Drug Monitoring (TDM) may represent a valuable tool for the clinician to quantify drug level in biological fluids during the therapy and verify the drug effectiveness and the tolerability of the therapy. Therefore TDM is useful to establish an individual dosing regimen of drug [Alnaim,2007]. High-performance liquid chromatography or gaschromatography are the analytical methods usually implemented for determining drug plasma Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 136 concentrations [Schoemaker, 2003], however these methods are laborious and not always practical for routine implementation [De Jonge, 2005]. So the ultimate goal of this project is the development of biosensors for irinotecan, paclitaxel and sunitinib that will be used for the design of new point of care devices or test kits useful for clinicians or patients to quantify blood drug levels. Artificial receptors /binders with high specificity for the target molecules are useful to this purpose. Such binders interact with the target through the molecular recognition mechanisms that play a key role in biology, where enzymes, antibodies and drug receptors catalyze biochemical reactions, neutralize exogenous antigens and bind agonists and antagonists. The high specificity and catalytic activity of these macromolecules are due to binding sites in which multiple interactions can be established with the target molecule [Pavan, 2011]. Binder elements from biological sources (such as antibodies), or developed by artificial, bio-inspired design (such as designed peptides [Hong, 2012] and imprinted polymeric materials), are widely used in drug delivery, drug targeting, sensing and diagnostic field. For example, antibody-based immunoassays have been developed for the detection of paclitaxel in Taxus tissues and in human serum during clinical trials [Grothaus, 1995; Svojanovsky, 1999]. Anti-irinotecan and anti-SN-38 antibodies have been exploited in the development of ELISA assays [Saita, 2000]. Molecularly imprinted polymers, instead, are micro- and nano-structured materials with three dimensional cavities that complements the shape, structure and functional groups of the target molecule. Molecularly imprinted polymers are characterized by long-term stability and by the ability to perform well under harsh conditions, such as high temperature, extreme pH values and organic solvents. Therefore MIPs have found much interest in the production of sensing elements, of stationary phases for chromatographic separations and affinity solid-phase extraction, of polymeric nanoparticles for drug delivery, and of catalysts by enzyme mimicking approaches [Flavin, 2008]. Finally, electrochemical sensors with MIP are very useful for the production of point of care devices [Sharma, 2012]. References Alnaim L.(2007) Therapeutic drug monitoring of cancer chemotherapy. J Oncol Pharm Practice 13: 207-221 Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 137 De Jonge M.E., Huitema A.D.R., Schellens J.H.M., Rodenhuis S., Beijnen J.H.(2005)Individualized cancer chemotherapy. Strategies and performance of prospective studies on therapeutic drug monitoring with dose adapttion. Clin.Pharmacokinet. 44(2):147-173 Flavin K., Resmini M.(2009) Imprinted nanomaterials: a new class of synthetic receptors. Anal Bioanal Chem 393: 437-444 Grothaus P.G., Bignami G.S., O’Malley S., Harada K.E., Byrnes J.B., Waller D.F., Raybould T.J.G.(1995) Taxane-specific monoclonal antibodies: measurement of taxol, baccatin III, and”total toxanes” in taxus brevifolia extracts by enzyme immunoassay. Journal of natural products. 58(7): 1003-1014 Hong Enriquez R., Pavan S., Benedetti F., Tossi A., Savoini A., Berti F., Laio A.(2012) Designing short peptides with high affinity for organic molecules: a combined docking, molecular dynamics and Monte Carlo approach. J. Chem. Theory Comput. DOI: 10.1021/ct200873y Pavan S., Berti F.(2011) Short peptides as biosensor transducers. Anal Bioanal Chem 402(10): 3055-70 Saita T., FujitoH.,Mori M.(2000) Development of ELISAs for irinotecan and its active metabolite SN-38. Biol.Pharm.Bull. 23(8): 911-916 Schoemaker N., Rosing H., Jansen S., Schellens J., Beijnen J.H. (2003) High-Performance Liquid Chromatographic analysis of the anticancer drug irinotecan (CPT-11) and its active metabolite SN-38 in human plasma. Therapeutic drug monitoring. 25:120-124 Sharma P.S., D’Souza F., Kutner W.(2012) Molecular imprinting for selective chemical sensing of hazardous compounds and drugs of abuse. Trends of Anal Chem 34: 59-77 Svojanovsky S.R., Egodage K.L., Wu J., Slavik M., Wilson G.S. (1999) High sensitivity ELISA determination of taxol in various human biological fluids. J. Pharm. Biomed. Anal. 20: 549-555 Objectives for the three years •Chemical modification of target molecules for either immobilization on gold or polymeric surfaces, bioconjugates synthesis, and reference compounds labeling, in order to develop both MIPs and antibody based technologies. •Synthesis of molecularly imprinted polymers with irinotecan, paclitaxel and sunitinib as template and study of MIPs binding capacity. •Immunogenic bioconjugates will be also prepared with the modified drugs, for the production of antibodies and the preparation of drugs labelled with enzymes (HRP), for the development of enzymatic assays. •Setup and development of ELISA with the best antibodies. •Development of nanosensors based on the artificial receptors. Objectives for the first year •Irinotecan, paclitaxel and sunitinib will be chemically modified with linkers for immobilization over solid surfaces for the screening of receptors libraries and for the measure of binding affinity on standard biosensors like surface plasmon resonance (SPR). •Different functional monomers will be chosen and synthetized or modified, for the synthesis of molecularly imprinted polymers. Research project Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 138 1) Paclitaxel, irinotecan and sunitinib chemistry Paclitaxel will be acylated with succinic anidride to obtain the hemisuccinyl-derived 1b, however, the carbonyl group at position 9 can also be modified to obtain the carboxymethyl oxime 1c (scheme1). Irinotecan will be modified on aromatic ring by diazotization to obtain the maleimide derivate 2b, while lactone ring opening leads a free carboxylic group that can be conjugated or modified in the same way of paclitaxel. Finally the only one hydroxyl group of the drug will be also considered in order to obtain the hemisuccinate 2c. Diazotization of the indole ring may be possible also on sunitinib to obtain the maleimide derivate 3b. Moreover, the diethylaminoethyl chain can be replaced with a chain containing a primary amine group, like in 3c, to allow direct conjugation with biotin and proteins. 2) Synthesis of molecularly imprinted polymers In this project MIPs with specific binding sites for irinotecan, sunitinib and paclitaxel will be synthesized. Small peptides or single amino-acids as functional monomers will be chosen. Short peptides will be designed by computational studies with the collaboration of prof. Laio (SISSA) and will be produced by automated solid phase peptide synthesis. The N-terminus of peptides or amino-acids will be acryloylated with acryloyl chloride to allow the monomer incorporation into the polymeric matrix of MIP. Functional monomers will be characterized by nuclear magnetic resonance (NMR) spectroscopy and electrospray ionization (ESI)-mass spectrometry, while the conformation of peptides in solution will be investigated with circular dichroism. Binding affinity of peptides for the target molecule will be studied by fluorescence spectroscopy and isothermal calorimetry. The size of MIP nanoparticles will be characterized by dynamic laser light scattering. Rebinding tests will be performed to assess the MIP capability to capture target molecules. 3) Development of antibodies Modified drugs will be conjugated with cationized bovine serum albumin or keyhole limpet hemocyanin to obtain immunogens for the immunization of rabbits or mice, to raise polyclonal antisera or monoclonal full chain antibodies. Phage libraries of single chain Fv antibodies will be also screened for anti-target globulins. The antibodies will be purified by affinity chromatography, and their binding capability will be characterized by immunoassays and surface plasmon resonance analyses. Horseradish peroxidase conjugates will act as enzyme-labelled references for the developing of Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 139 competitive ELISA assays, which will be validated on spiked and real samples in both serum and plasma, by statistical comparison with standard liquid chromatography-mass spectrometry (LC-MS) titrations. 4) Development of nano-sensors Atomic force microscopy (AFM) will be employed to develop a novel approach to detect drugs and metabolites able to quantify drug levels in a very small volume of plasma, blood or tissue. This device will be based on a competitive assay between the drug linked on a gold surface and the free drug in the sample for the binding to the antibody. AFM technique will be also employed to test molecularly imprinted polymers because they acts as receptors for a specific drug. Finally the new developed sensors and ELISA assays will be tested to optimize the working conditions, and define the selectivity and sensitivity limits. Also matrix effects and the sensors applicability of plasma samples will be evaluated. Activity month Î 1 Irinotecan modifications 1 Sunitinib modifications 1 Paclitaxel modfications 2 Synthesis of monomers 2 Synthesis of MIPs 2 Characterization of MIPs 3 Immunization 3 Antibody selection 3 ELISAs setup 4 5 6 3 6 9 12 15 18 21 24 27 30 33 36 Nanosensors setup for TDM TDM in purified solutions and cultured cells TDM in complex samples (serum-plasma-blood) Educational Activity foreseen Courses: •“Hybrid organic-inorganic nanoparticles” (Prof. Lucia Pasquato) •“Experimental design and optimization” (Prof. Cynthia Ebert) Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 140 •“Introduzione alla sintesi organica” (Prof. Federico Berti) Schools: •Interdisciplinary Phd Spring School (7-8 March 2013) Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 141 DAVIDE PORRELLI Email: [email protected] Title of the thesis: “Nanocomposites biomaterials based on polysaccharides and carbon nanostructures for biomedical applications” Laboratory: Department of Life Science, building Q, lab. 113 Supervisor: Prof. Sergio PAOLETTI Tutors: Massimiliano BORGOGNA, Ivan DONATI Research Activity foreseen State of the art and motivation This project is aimed at designing innovative biomaterials composed by natural biopolymers (alginate, hyaluronic acid, chitosan) and Carbon Nanostructures (CNSs) for biomedical applications; in particular, these materials will be developed for the treatment of Spinal Cord Injury (SCI) and for bone tissue regeneration. Carbon Nanostructures (CNSs) have been receiving increasing attention during the last years for their unique physical and chemical characteristics that made these structures good candidate for their use for neurological and tissue engineering applications[Nano Lett. 2010, 10, 3223-30]. Although the current scientific data have shown conflicting results about potential nano-toxicity of CNSs, many studies are pointing out the biocompatibility of several forms of CNSs (especially in functionalized form) and their ability to support growth and proliferation of cells like neurons and osteoblasts [J. Tiss. Eng. 2012, 2, 1, 674287; Chem. Neurosci. 2012, 3, 611-8]. The use of CNSs in combination with bioactive biopolymers aims at the development of novel biocompatible nanocomposites in which biopolymers are implemented by physical and biological properties of CNSs [Life Sciences 2010, 87, 215-22]. The advancement of these materials with respect to the state of the art is briefly tackled in the following paragraphs. Bone tissue regeneration: possible limitations of the polymers currently used for bone regeneration include lack of bioactivity and poor mechanical properties; an ideal scaffold for bone tissue regeneration should be able to promote osteoblasts proliferation and migration, and should have mechanical properties similar to that of bone. Moreover it should have a porous structure with interconnected pores and controlled size in order to allow an excellent osteointegration [Ann. of Biom. Eng. 2012, 40, 1628-40; Adv. Mater. 2012, 24, 4995-5013]. The use of CNSs in combination with biopolymers could implement scaffold properties by modulating mechanical strength and osteoinductivity [Int. J. Biol. Macromol. 2010, 46, 281-3]. Spinal Cord Injury treatment: SCI is a devastating clinical condition that significantly impacts the ability of affected individuals to produce functional movements and often results in paraplegia or quadriplegia [Nat. Rev. Neurosci. 2006, 7, 644-53]. Currently there are no therapies able to repair the damage of the spinal cord; recent strategies have involved the study of a plethora of curative interventions towards prevention of cell death, or towards stimulation of axonal re-growth, Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 142 enhancement of axonal transmission or amelioration of secondary damage [Nat. Rev. Neurosci. 2006, 7, 644-53; Spinal Cord 2005, 43, 134-61; Nat. Rev. Neurosci. 2006, 7, 628-43; Exp. Neurol. 2002, 174, 125-36; Exp. Neurol. 2012, 235, 100-9]. The use of bioactive biomaterials as synthetic bridging implants able to transmit electrical signals for SCI treatment has not yet been transferred into clinical trials: the ongoing SCI clinical trials continue to rely mainly on the pharmacological approach, with the only few exceptions of the stem cell-based therapies, which, however, have not provided so far convincing evidence of clinical efficacy. Applications of nanotechnology with potential clinical impact include the use of nano-engineered functional scaffold systems for promoting neural regeneration following both acute and chronic injury. These approaches attempt to create chemical, physical and biological environments that support/promote the function or regeneration of central axons. The polymeric materials employed for scaffold design provide a pure biomimetic environment: thus, the regeneration process is not based on the implementation of electrical signals. Hyaluronan-based materials have been tested in models of peripheral nerve and SCIs. The presence of a high molecular weight form of hyaluronic acid has been linked to scar-free wound healing, leading to a reduced glial scar response [Neurosci. Lett. 2012, 519, 103-14]. The rationale behind incorporating CNSs into a novel injectable/implantable biomaterial is that of overcoming the limits of conventional polymer-based scaffolds, such as the lack of electrical conductivity: it has been proposed that one of the main issues in neural tissue regeneration is the electrical conductivity of the biomaterial which would favor neural transmission and can improve mechanical and rheological properties of ECM-like structures [Nat. Nanotech. 2011, 6, 13-22]. CNSs moreover can affect cell behavior and promote attachment, growth, differentiation and long term survival of neurons [ACS Chem. Neurosci. 2012, 3, 611-18]. Objectives for the three years The main objective of the project is the preparation of biocompatible nanocomposites in the form of scaffolds or injectable matrices based on natural-based biopolymers (such as alginate, hyaluronic acid, chitosan and derivatives) and CNSs. This goal will be pursued through the following intermediate objectives: • optimization of the preparation of the nanocomposite systems; • physical‐chemical and mechanical characterization; • evaluation of in vitro biocompatibility and bioactivity. In case of promising in vitro results, in vivo tests will be considered to test the materials on suitable animal models. Objectives for the first year: Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 143 • literature survey on the most suitable components and solutions for the applications targeted by this project; • selection of the components among various polysaccharides and CNSs; • preparation and characterization of homogenous solutions and chemical/physical and rheological characterization; • preparation and characterization of homogenous hydrogels and scaffolds with desired chemical and physical features. Research project The research project foresees the production of different nanocomposites materials in form of injectable fillers or 3D scaffolds composed of a polysaccharide matrix and CNSs. Morphological, mechanical and physico-chemical characterizations will be performed. In addition, the effects on eukaryotic cells will be studied in vitro and a final in vivo study will be considered in case of encouraging in vitro results. The activities and tasks of this project are listed below: 1.Materials selection and analysis: • analysis and evaluation of physical‐chemical properties of the selected biopolymers (Viscosimetry, Nuclear Magnetic Resonance); • analysis of functionalized CNSs (TGA, SEM, TEM). 2.Design and characterization of the nanocomposite formulations: • preparation of the nanocomposite formulations; • characterization of the materials in the form of solutions, hydrogels and freeze‐dried scaffolds (rheological tests, mechanical tests, SEM, TEM, µ‐CT) 3.In vitro biological characterization: • biocompatibility and cytotoxicity assays of the materials (LDH, MTT); • evaluation of the material ability to promote axonal regeneration and synaptogenesis; • evaluation of the material ability to stimulate osteoblasts activity and inhibition of osteoclasts activity (Alamar Blue, Alizarin Red assays, Confocal Microscopy, SEM); 1st year Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 2nd year 3rd year 144 Materials selection and analysis Design and characterization of the nanocomposite formulations Biological characterization Educational Activity foreseen University courses: • Biomaterials, artificial organs and prostheses (prof. Sbaizero Orfeo; Master Degree in Process and Materials Engineering, 6 CFU) • Introduction to organic spectroscopy (prof. Felluga Fulvia; Bachelor Degree in Chemistry, 4 CFU) I will attend laboratory activities to improve my knowledge on: • in vitro and in vivo tests of biomaterials and nanocomposites; • Physical/chemical and mechanical characterization of nanocomposites; • preparation and characterization of nanostructured materials. I will attend the Interdisciplinary PhD Spring School (Udine, March 7 – 8, 2013) and other school and seminars. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 145 CANDIDATE PASQUALE SACCO Email: [email protected] Title of the thesis: Novel biomaterials for innovative therapies in the severe wounds treatment Laboratory: Department of Life Science, Ed. Q, First Floor, Room 105 Supervisor: Prof. Sergio PAOLETTI Tutors: Dr.ssa Eleonora MARSICH, Dr. Massimiliano BORGOGNA Research Activity foreseen State of the art and motivation Nonhealing wounds (such us diabetic and pressure ulcers) are wounds which have not undergone the normal process of healing because the three phases of healing (the inflammatory, proliferative and remodeling phases) have been prolonged or did not progress in an orderly fashion. Non-healing skin lesions are a fertile ground for bacteria proliferation that contribute to make the lesion worse, causing a massive and persistent inflammatory response [5]. Proper treatments of wounds require the employment of pro-regenerative and anti-inflammatory factors associated to antimicrobial agents such as antibiotics and antiseptics [6]. However, antibiotics topically applied often lead to the development of bacterial resistance and sensitization. In this direction, employment of alternative wide-spectrum antibacterial agents is preferred to antibiotics. Several metals including Silver (Ag) have shown efficacy for the treatment of infections by inhibiting Gram+ and Gramgrowth at very low concentrations [7]. Silver nitrate solutions [8] and silver sulfadiazine [9] are commonly used in the treatment of burns. Both of these solutions have drawbacks: Ag nitrate is caustic, thus its concentration should be very low in solution whilst sulfadiazine induces sensitization and bacterial resistance. Moreover both nitrate and sulfadiazine affect the healing process [10]. Nanotechnology has provided new chemical forms of silver, such as nanocrystalline silver, for the employment in biological systems. These formulations can be used to prepare creams, impregnated and advanced Ag-based medications. The employment of metals such as silver represents the future in the design of advanced medical systems with antiseptic activity. [5] Approccio terapeutico alle lesioni cutanee: la gestione della carica batterica - www.riparazionetissutale.it [6] Angela Peghetti, Matilde Mantovani, Giuliana Canova, Loretta Ferri “Le medicazioni avanzate per il trattamento delle ferite acute e croniche - Dalle evidenze della letteratura alla pratica quotidiana” – pagg. 9 e seguenti. Servizio Sanitario Regione Emilia Romagna – Febbraio 2012 [7] Andrea Travan et al “Non-cytotoxic Silver Nanoparticle-Polysaccharide Nanocomposites with Antimicrobial activity” Biomacromolecules 2009, 10, 1429–1435 1429 [8] Mayer C. Treatment of large human burns with 0.5% silver nitrate solution. Arch Surg 1965:90; 8120-820 [9] Fox C. silver sulfadiazine: a new topical therapy for Pseudomonas in burns. Arch Surg 1968:96; 1840-187 [10] Demling R, DeSanti L. Effect of silver on wound management. Wounds 2001:13 Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 146 This project aims to provide nano-structured biomaterials containing either biologically active ionic metal or nanostructured forms of silver embedded inside natural polymeric matrices in order to obtain an absolutely innovative multifunctional system activity. Objectives for the three years The aim of this project is to develop novel Ag-based systems suitable for the employment in advanced dressings for infected non-healing skin wounds. The main objectives for the three years are listed below: 1. Synthesis of nano-engineered polysaccharides conjugated with biological molecules to increase their bioactivity and biocompatibility 2. Physical-chemical characterization of conjugated compounds 3. Biological characterization of conjugated compounds 4. Development of polysaccharide-based system synthesized at step 1 containing silver ions and silver nanoparticles 5. Combinations of aforementioned conjugates with biologically active polysaccharide matrices, such as hyaluronic acid or other glycosaminoglycans to obtain three-dimensional networks 6. Study of antibacterial and tissue regeneration property of biomaterials developed from step 1 to 4 These novel matrices will constitute a new generation of devices in which they will combine synergistically the advantages of the individual components, namely: - Biological activity of molecules, such as lipoic acid and butyrate - Antiseptic activity of Silver - Skin regenerative activity of the polysaccharide matrices Objectives for the first year • Selection and synthesis of the components of polysaccharide derivatives • Preliminary biological studies on primary cells using derivates at different degrees of substitution and concentration • Set up of experimental procedures for the development of nano-engineered systems containing silver ions and silver nanoparticles. Research project Task1 Synthesis of nano-engineered polysaccharides conjugates Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 147 Natural polysaccharides such as hyaluronic acid will be nano-engineered by covalent grafting of bioactive molecules (butyrate and lipoate) with the aim to introduce additional bio-functional molecules and signals able to increase / modify the bioactivity of the polymer. Task 2 Physical-chemical characterization of conjugated compounds Functionalized conjugates will be characterized in order to define degree of substitution, purity, rheological properties, solubility and miscibility. Task 3 Biological characterization of conjugated compounds Primary human cells such as dermal fibroblasts and keratinocytes will be used to study the effects of the compounds. Cytotoxicity, proliferation, migration, expression of phenotypic markers and of extracellular matrix components will be considered. Moreover, the influence of the polymers on the expression and release of pro- and anti-inflammatory cytokines from monocytes and macrophages will be evaluated in order to clarify their effects on the inflammatory response. Task 4 Development of polysaccharide-based systems synthesized at step 1 containing silver ions and silver nanoparticles The polymers produced in Task 1 will be used as soluble support matrices for silver ions and/or for silver nanoparticles in order to develop a system endowed with antibacterial activity. Particular attention will be devoted to characterize dimensions, dispersion and stability of the nanoparticles in the polymeric colloidal solutions. Task 5 Combinations of conjugates with biologically active polysaccharide matrices, such as hyaluronic acid or other glycosaminoglycans to obtain three-dimensional networks Three dimensional matrices will be obtained combining bioactive/biocompatible polymers with gelling properties with the silver-containing polymers. Task 6 Study of antibacterial properties and cytotoxicity of biomaterials Antibacterial tests will be performed both on silver-containing polymeric solutions and on threedimensional matrices using bacterial strains directly involved in skin infections (Staphylococcus aureus, Staphylococcus epidermidis and Pseudomonas aeruginosa). The effect will be evaluated Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 148 both on bacterial planctonic forms and on bacterial biofilms. Particular attention will be provided to study the possible cytotoxic effects by silver nanoparticles. 1st year 2nd year 3rd year Synthesis of nano-engineered polysaccharides conjugates Physical-chemical characterization of conjugated compounds Biological characterization of conjugated compounds Development of polysaccharide-based systems containing silver ions and silver nanoparticles Combinations of conjugates with biologically active polysaccharide matrices Study of antibacterial properties of biomaterials Educational Activity foreseen In the first year my educational activity will regard: Participation to seminars, conferences Study of scientific literature “Biomateriali e Ingegneria Tissutale”, course of the Master Degree in Medical Biotechnology, Dr. Gianluca Turco (56 hours) Other courses or school activities Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 149 FRANCESCA SCOGNAMIGLIO Email: [email protected] Title of the thesis: “Nano-engineered adhesive biomaterials for biomedical applications” Laboratory: 113, building Q Supervisor: Prof. Sergio PAOLETTI Tutors: Andrea TRAVAN, Ivan DONATI. Research Activity foreseen State of the art and motivation Polysaccharide-based adhesive systems Adhesive systems are largely investigated for several biomedical applications; several innovative approaches are based on molecular strategies engineered at the nano-scale. An ideal adhesive system for medical use should allow a proper adhesion between the biomaterial and the biological tissue avoiding both sliding effects on wet surfaces and adverse reactions. Adhesion can be achieved through the establish of covalent bonds between the material and a biological surface, or by exploiting hydrophobic/hydrophilic features of both of them. In general, given the different composition of the two interacting surfaces, several applications require the of glues and sealants that allow the proper adhesion. Polysaccharide molecules represent an ideal substrate for the achievement of biological glues, since they can be easily modified through the addition of chemical reactive groups. For instance, chitosan, alginate and dextran are prone to be modified at the nanoscale level for the development of nano-engineered biocompatible adhesive systems. Biopolymeric membranes for colorectal applicartions During this research project, biopolymeric membranes will be developed and characterised as a new biomaterial for anastomotic leakage prevention, in cases of colorectal cancer (CRC) resection. Colorectal cancer (CRC) is the second most common form of cancer in Europe and its treatment is mainly based on surgical intervention, with the resection of the affected bowel and the suture of the extremities to restore the normal bowel transit1. The site at which the bowel continuity is restored is called anastomosis. The most frequent post-operative complication is the Anastomotic Leakage (AL) which occurs when no proper and rapid regeneration of the intestinal tissue occurs at the site of the anastomosis2. Both systemic and surgical factors contribute to the onset of AL leading to clinical consequences such as generalized peritonitis (requiring abdominal reoperation), increasing in local recurrence of cancer and decreasing in long term patient survival3. For these raisons, it has been proposed the use of an external reinforcement that wraps the anastomosis and trigs the tissue healing4. In this regard, this project aim to develop a material that wraps the anastomosis and promote the physiological process of tissue regeneration. This material will be applied by surgeons to the staple line as an external reinforcement. According to Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 150 laparoscopic techniques, the material should be produce in form of an adhesive patch, biocompatible, water swellable, easy to handle, and it should not lead to adverse reactions, such as inflammation, citotoxicity and infection, or causing adhesion between viscera and abdominal walls. The introduction of nano-fillers and reinforcement will be studied in order to modulate the mechanical properties of the patches. An additional feature of such material would be its antibacterial activity. Polysaccharide-based adhesive for restorative dentistry Polysaccharide-based adhesive systems are suitable to be employed in dental field. Several materials based on polysaccharides are investigated for this medical application. Given the high incidence of oral diseases such dental caries, there is a strong need to restore the dental structure, thus preventing the onset of secondary ones. At present, materials used for dental restoration are based on resin composites that are bound to the collagen dentin through an adhesive system. Such adhesive systems form a hybrid layer on the dental surface that ensures a micromechanical interlocking. However, the creation of a stable bond between dentin collagen and restorative material is challenging, given the action of degradation phenomena5 and the lack of chemical bond between collagen fibrils and resin. On these basis, this research project aims also to develop a new adhesive system that allows proper interaction between the two surfaces. The adhesion strategy will be based on the modification at nanoscale level of chitosan, a polysaccharide that has intrinsic bioadhesive features. Objectives for the three years The final goal of this PhD is to develop new nano-engineered adhesive solutions based on natural polysaccharides for two different applications: one for internal surgery and the second one for dentistry applications. The first research line will aim at the development of an engineered bioresorbable biomaterial that will be used for the prevention of the AL. The biomaterial will be based on natural polysaccharides such as alginate and Hyaluronic acid (HA), polymers already used in several medical applications. Moreover, HA conjugated with butyric acid (HABut) will be inserted into the formulation, since butyric acid has been reported to reduce the AL on rat models7. The second research line points at the development of an adhesive system able to interact with both dentin collagen and the restorative material used mainly for dental disease. To achieve this goal, chitosan will be modified in order to obtain a nano-engineered polymer with a double functionalisation. In this regard, we aim at modifying chitosan through the introduction of both methacrylate groups and glutamine residues, able to interact with both the dentin collagen and the resin-based composites, thus creating an hybrid layer that resist to degradation phenomena. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 151 The final goals will be reached through the following intermediate objectives: ¾ Mechanical and physico-chemical characterization of the developed materials; ¾ Definition of adhesive strategies to allow a proper tissue-material adhesion; ¾ In vitro tests for the evaluation of biocompatibility, cell vitality and viability, proliferation, adhesion and other biological effects; ¾ In vivo studies of the biomaterials on animal models (for the intestinal membrane research line). Objectives for the first year The objectives to be achieved during the first year are the following: ¾ Literature survey on the state of the art about the research topics proposed; ¾ As to the first research line, definition of adhesive strategies to allow a proper tissuematerial bondage. The strategies will be based on the analysis of the adhesive systems already used in surgical intervention, as well as the development on new ones, based on the modification at nanometric scale and functionalisation of the polysaccharide matrix, in order to allow the conjugation with other chemical compounds. Sealants already available for medical applications will be tested, as well as the use of nano-engineered polysaccharides; ¾ As to the second research line, a suitable functionalization of the polysaccharide (chitosan) will be tackled in order to endow the polymer with adhesive properties towards both restorative resin and collagen fibers; ¾ Phisical, chemical and mechanical characterisation of the biomaterials; ¾ In vitro biological tests in order to investigate the biological activity of the patches. ¾ In vitro biological tests to evaluate the biocompatibility of the functionalized-chitosan adhesive system. Research project Line 1: Development of nano-structured adhesive patches for colorectals applications The biomaterial that will be developed will be based on a mixture of polysaccharides, such as alginate and hyaluronic acid, polymers that are already use in several medical applications. In addition, butyrate will be added in a conjugated form with HA (hyaluronic acid butyric ester), to confer additional properties to the material. Each polymer exerts a specific biological function and Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 152 represent an alternative to synthetic polymers or to proteins such as collagen which can be associated to a severe risk of biological contamination. The patches will be obtained through the freeze drying procedure and designed to adhere to the intestinal serosa and to remain in situ for a sufficient period to achieve the cicatrisation and remodelling of the anastomosis (approximately two weeks). The proper adhesion of the patch to the intestinal epithelium is required in order to trigger the biological healing processes. The absence of a proper adhesion may lead to poor biological response. Thus, the development of an efficient strategy to ensure a proper adhesion is a fundamental aspect for this biomedical applications. In order to improve the adhesion of the patch to the external intestine walls, several strategies will be pursued. Furthermore, this material should possess adequate mechanical properties (which can be tailored upon addition of nanofillers and micro/nano fibres) and should not cause adverse reactions. The activities and tasks of this project are listed below: 1. Development of adhesion strategies that allow the proper adhesion of the patch to the intestinal epithelium. In order to improve the adhesion of the patch to the external intestine walls, several strategies will be pursued. • Development of an adhesive system based on molecular strategies that ensure a proper tissue-material bondage at the nanoscale level. Various approaches will be pursed, including the possibility to obtain covalent bonding between the polysaccharide matrix and the tissue. The polysaccharide matrix will be functionalised to allow the conjugation with adhesive molecules such as dopamine; • A combination of already existing adhesion strategies, such as fibrin glue, gelatine based tissue adhesive, chitosan sealant will be tested; • The adhesivness of the different formulations will be tested on intestinal pig ephitelium. 2. Polysaccharide chemical functionalization. Polymers used to develop the patches will be chemically modified in order to modulate the adhesive properties of the biomaterial. These molecules will be functionalised through the introduction of specific pendent groups that will be chemically bound on polysaccharide backbones, thus creating polymers modified at nano-scale level. This strategy aims to the formation of side chains that will be able to bind covalently to tissues. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 153 3. Mechanical and physical-chemical characterisation. The patches should posses adequate mechanical properties in order to withstand handling and positioning stress, to withstand the peristaltic movements and should not cause stenosis at the anastomosis site upon material stiffening. These aspects will be characterised through mechanical tests considering ultimate strength, Young’s Modulus, deformation at break of patches in both wet and dried conditions. 4. Introduction of a structural reinforcement in the polysaccharide matrix. • Various options for the reinforcement of the patches will be investigated, in order to improve its mechanical performances in physiological conditions. The introduction of nanofiller and nanofibers capable of increasing mechanical properties will be studied. 5. In vitro biological tests will assay: • Cytocompatibility of the components by LDH and MTT assays. • Cell viability and activity after incubation of cells with the patch (AlamarBlue, MTT assays); • Biocompatibility of the patches by exposing human monocytes to the sterile patch for a predeterminated length of time and evaluation of inflammation response through the detection of cytokines into the medium by MultiPlex beads; • Cell growth, apoptosis, differentiation, synthesis of extracellular matrix quantified through RT- PCR and western blot analysis. 6. In vivo studies of patches on animal models. These tests will be performed by a research partner of the EU project AnastomoSEAL (University of Maastricht); results will be shared and anlyzed by the whole project consortium, allowing to gather information about the behaviour of the developed membranes in an animal model (pig). The Gantt chart of this research line is sketched in the following table. 1st year 2nd year 3rd year Survey literature on adhesive systems Material selection Material development (chemical, mechanical and structural characterisation) In vitro biological tests In vivo tests Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 154 Line 2: Development of nano-structured adhesive patches for restorative dentistry In order to improve the adhesion between the dental surface and the restorative material we aim to develop a nano-engineered dental adhesive system capable to form covalent chemical bonds with both the dentin collagen and the resin. This system will be based on a natural polysaccharide (chitosan) that will be modified in order to bear both methacrylate groups and glutamine residues. Methacrylate groups guarantee the bound between the adhesive and the restorative material by a photopolymerisation process, while glutamine residues are able to bind the exposed dentin collagen through crossilinking reaction catalysed by transglutaminase enzymes. The activities and tasks of this project are listed below: 1. Synthesis of the adhesive system and mechanical, physical and chemical characterisation. • Introduction of flanking methacrylate and glutamine residues on the polysaccharide chain; • Morphological characterisation through the use of microscopy techniques (SEM), and infrared spectroscopy (ATR-FTIR); • 2. Viscosity and solubility chracterization of the adhesive system; In vitro biological tests • Biocompatibility (LDH, MTT) using fibroblasts cell lines as well as primary cultures of gingival and pulp fibroblast and odontoblasts; • Analysis of the effect on metalloproteinase activity. The Gantt chart of this research line is sketched in the following table. 1st year 2nd year 3rd year Synthesis of the adhesive and physical-chemical characterization Material development (mechanical and structural characterisation of the adhesive interface) In vitro biological tests Educational Activity foreseen Nanobiotechnology ( Modulus B course of the degree in Medical Biotechnology) Interdisciplinary PhD Spring School on nanotechnology Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 155 Other schools and courses Laboratory activities aimed to improve the knownledge in the field of chemistry, engineereing and biology field. Reference list 1 Rajput Ashwani and Bullard Dunn Kelli, "Surgical Management of Rectal Cancer,"in 34 ed.2007), pp.241-249. 2 Y. H. Ho and M. A. Ashour, "Techniques for colorectal anastomosis," World J Gastroenterol. 16(13), 1610 (2010). Ref Type: Journal 3 C. S. McArdle, D. C. McMillan, and D. J. Hole, "Impact of anastomotic leakage on long-term survival of patients undergoing curative resection for colorectal cancer," Br. J Surg 92(9), 1150 (2005). Ref Type: Journal 4 J. Hoeppner, et al., "Small intestinal submucosa for reinforcement of colonic anastomosis," Int J Colorectal Dis 24(5), 543 (2009). Ref Type: Journal 5 L. Breschi et all. “Dental adhesion review: aging and stability of the bonded interface”. Dent Mater 2008 24 (1), 90-101 Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 156 Candidate CRISTIAN SVETINA Email: [email protected] Title of the thesis: Photon beam studies and characterization for EUV/Soft X-ray coherent imaging of nano-structures using coherent FEL radiation Laboratory: ELETTRA-Sincrotrone Trieste Supervisor: Dr. Marco Zangrando Tutors (if any): Research Activity foreseen State of the art and motivation Fermi@Elettra is the first seeded Free Electron Laser in the EUV/Soft Xray energy range. Based on a High Gain Harmonic Generation (HGHG) scheme, this FEL generates Fourier transform limited sub-picosecond pulses, with a high photon flux (up to 1014 photon/pulse), and variable polarization [1]. This unique radiation source will be used for time-domain spectroscopy and coherent imaging experiments, therefore paving the way for studying the dynamics of systems out of equilibrium or for the microscopy of nanoobjects by coherent imaging techniques using variable polarization fully coherent soft X-ray ultrashort pulses. The Diffraction and Projection Imaging (DiProI) beamline is one of the four end-stations operating with the FERMI@Elettra. In particular, DiProI is devoted to the imaging of both fixed and free-standing nano-objects of various nature [2]. In the first operating stage of FERMI, DiProI will perform Coherent Diffraction Imaging (CDI), in-line and Fourier transform holography of nanostructures, while projection imaging and stereo imaging are planned to be implemented in the next future. One of the DiProI main goals is to perform resonant CDI, with dichroic contrast obtained by varying the FEL wavelength and polarization, suitable for magnetism studies. In CDI the real- space information of the specimen is extracted from the far field diffraction pattern by an iterative phase retrieval algorithm. The main advantage of using FEL pulses, instead of a synchrotron source, arises from the possibility of acquiring instantaneously the information of the local electron density in the sample or its magnetic images (using variable polarization) with a very high spatial resolution (~1μm) during the time duration of the FEL pulses (~100 fs). The detection of the pulses will be provide by a technique called Command Detector Interface that has been validated by A. Barty and coworkers [3] in an experiment at the Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 157 FLASH FEL of DESY. Furthermore, in a recent work C. Gutt and coworkers have performed x-ray magnetic scattering on a Co/Pt multilayer film by tuning the FEL wavelength radiation across the Co absorption edge [4]. In order to be able to achieve these goals, DiProI needs to focus the FEL Gaussian photon beam below 10 μm (FWHM), with high spatial coherence and fluence. For reaching such a behavior two solutions could be adopted: implement a focusing lens (i.e., a Fresnel zone plate) or use focusing mirrors with suitable profiles. In the first case the resolution is mainly imposed by the limited quality of the used optical elements in full field and scanning X-ray microscopy. Moreover, the lenses can be easily damaged by the high fluence emitted by the FEL. The lensless CDI by means of focusing mirrors, on the other hand, has been demonstrated to be a powerful microscopy method [5] and, nowadays, has become the commonly used solution for FEL sources, allowing to resolve nano-structures with high resolution [6]. For these reasons the DiProI focusing system consists of a set of Kirkpatrick- Baez (KB) active mirrors [7] capable of modifying the focused beam dimensions, the focal length and, in principle, the wavefront quality, providing high resolution CDI. The diagnostics of focused photon beams is of great interest in the FEL community since they are essential for reaching the needed spot qualities and it is the core of the proposed project. Moreover, the optimization of the spot properties can be done by exactly knowing the effects of the focusing mirrors on the radiation. For this reason an accurate metrology, ex-situ and in-situ, is very important in general, and for DiProI in particular, for optimizing the light spot on the sample. References [1] E. Allaria et al., “Highly coherent and stable pulses from the FERMI seeded free-electron laser in the extreme ultraviolet”, Nature Photonics 6, 699–704 (2012) [2] E. Pedersoli et al., “Multipurpose modular experimental station for the DiProI beamline ofFermi@Elettra free electron laser”, Rev. Sci. Instrum. 82, 043711 (2011) [3] A. Barty et al., “Ultrafast single-shot diffraction imaging of nanoscale dynamics”, Nature Photonics 2 415–19 (2008) [4] C. Gutt, et al., “Single-pulse resonant magnetic scattering using a soft x-ray free-electron laser”, Physical Review B 81 100401 (2010) [5] J. Miao et al., ”Extending the methodology, of X-ray crystallography to Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 158 allow imaging of micrometre-sized non-crystalline specimens,”, Nature 400, 342-344 (1999) [6] H. N. Chapman et al., “Femtosecond Diffractive Imaging with a SoftX-ray Free-Electron Laser”, Nature Physics 2, 839-843 (2006) [7] L. Raimondi et al., “Microfocusing of the FERMI@Elettra FEL beam with a K-B active optics system: spot size predictions by application of the WISE code”, NIM-A special issue IWXM, Article in Press (2012) Objectives for the three years We plan to investigate the active KB system performances in terms of metrology measurements, focusing simulations, and actual measurements using the FERMI FEL radiation. The metrology part will be divided into ex-situ and in-situ metrology. The former will be carried out at the Elettra metrology laboratory by means of a Long Trace Profiler (LTP) and an interferometer, while the latter will be pursued by applying the pencil beam and the lateral shearing imaging techniques, using the FEL radiation. The results obtained during the metrological investigations will be used for predicting the KB performances at the DiProI beamline. These simulations will be done using ray tracing and wavefront propagation codes. During the measurements with the FEL radiation we plan to apply different techniques that allow the determination of the focused spot dimensions and the wavefront, like the Hartmann sensor, some phase retrieval methods, the ablation of some suitable samples (like PMMA and Silicon), and the direct imaging by means of YAG crystals and phosphorous screens. Finally, a significant part of the project work will be dedicated to the first experiments performed by the advanced optical devices described above, characterized and optimized by the proponent of this thesis. Objectives for the first year We plan to perform the first ex-situ metrological investigation of the active KB mirrors in order to measure the best reachable longitudinal profiles. We plan to simulate the optical performances of the active KB system using ray tracing and wavefront propagation codes. We will begin to characterize the FEL radiation focused with the active KB by means of a wavefront sensor and PMMA/Si ablation. Research project The research activities will be divided into two different categories: Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 159 active KB mirrors figure optimization measurement of the focused radiation in terms of spot size and shape The figure optimization will be performed by means of metrology measurement techniques, both involving ex-situ and in-situ metrology: ex-situ metrology will be carried out in the Elettra metrology laboratory in-situ metrology will performed using the FERMI FEL radiation The FEL focused spot will be characterized in the DiProI end-station by means of the following techniques: Wavefront Hartmann sensor detector direct imaging of YAG and Phosphorous screens PMMA and Silicon ablation Phase retrieval methods Educational Activity foreseen Attend the annual meetings and seminars organized by the School of nanotechnology Attend some seminars related to the FEL optics and diagnostics Support at the ELETTRA metrology laboratory Study of several FEL optics books and review articles Attend some International conferences about FEL optics and diagnostics Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 160 SIMONE VELARI Email: [email protected] Title of the thesis: “Modeling the atomic scale properties of simple biomolecules at surfaces: from the role of solvent to small structured peptides” Laboratory: / Supervisor: Alessandro De Vita Tutors (if any): / Research Activity foreseen State of the art and motivation The control of a large number of processes in living organisms is based on the recognition of small organic molecules by large molecules (such as proteins, enzymes or antibodies) through a specific interaction site. For this reason, the design of short, peptide-based artificial receptors capable of highly specific recognition is one of the goals of biotechnology. For instance, small synthetic peptides have been recently designed as biosensor transducers, and their functionality is intimately related to their conformation, in particular their secondary structure (such as α-helix or β-sheet), since it is known to allow for intermolecular self-organization of the sensing peptides over the sensor surface. In the perspective of an atomic scale investigation of biomolecules by SPM, it is crucial, although not trivial, to be able to deposit the molecules on a surface while preserving their secondary structure, as evident from the above discussion. A simple deposition method, albeit poorly tested up to now with respect to the preservation of the secondary structure, could be the deposition from solvent drop in ambient conditions. However, regardless of the chosen method, the role of the solvent upon interaction with the surface cannot be neglected, and must be thoroughly investigated. Preliminary STM experiments at liquid helium temperature, carried out within the group of Prof. Giovanni Comelli by Dr. Carlo Dri at the IOM-CNR TASC Laboratory in Basovizza, show evidence that solvent molecules create complex self-assembly structures upon adsorption, that in some cases even mimic the structural properties of small peptides. Theoretical modeling using the ab-initio computational approach is crucial in order to successfully address these questions, to provide insight not experimentally available due to the fundamental limitation of STM, i.e. the lack of chemical resolution. The aim of this project is to provide a theoretical model that could help rationalise the experimental data. Objectives for the three years To formulate a well-defined adsorption model for different solvent molecules (e.g. DMSO, TFE, acetonitrile, phosphate buffer, etc.), all the interactions between surface and solvent, and the possible inter-molecular bonds have to be explored. In particular, the relative importance of hydrogen bonding and dispersive interactions for the self-assembly have to be assessed. Moreover, the role and the presence of water molecules must be evaluated, that could indeed be stabilized by Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 161 coadsorpion within the observed structures. Such a complex pattern of chemical and physical interactions can be accounted for only by means of quantum mechanical computational techniques, which are able to correctly model the characteristics of inter-atomic bonds and electrostatic interactions. Density-functional theory (DFT) therefore represents the ideal choice when dealing with systems of such size and complexity. The Quantum Espresso code based on DFT, plane waves basis sets and pseudopotentials will be used for these ab-initio calculations. As a second step, the adsorption of simple, small synthetic peptides at surfaces with well-defined secondary structure (e.g. α-helices or β-sheets) will also be modeled with different and larger scale computational techniques, such as classical Molecular Dynamics or Kinetic Monte Carlo Methods. The adsorption of different aminoacid sequences will be explored, aiming at highlighting the effects of peptide size, charge distribution within the peptide structure and chemical affinity of specific residues with the substrate. For each step of the project, theoretical simulation of the STM images will be carried out, within suitable frameworks and approximations, on tAhe basis of the obtained computational results, in order to directly compare the theoretical models with the experimental data. The long-term goal of this project will be the study of the interactions between our prototypical biomolecules (starting from solvents, amino acids up to small peptides) and a variety of other surfaces with different physical and chemical properties, e.g., insulating thin films grown on metal substrates such as NaCl @Cu(111), to explore the range of functionalities achievable by our target peptide-based nanostructures in view of their possible use in bio-nanotechnology. Objectives for the first year • Define the problem, study the literature and understand the theoretical background of the STM experiment. • Choose the more useful computational techniques to understand the experimental data. • Model DMSO molecule, find through some tests the more suitable parameters and pseudopotentials. Try to model the DMSO - Water interaction. • Optimize the lattice constant of Gold, comparing the results of different pseudopotentials; create an Au (111) surface, optimize all the simulation parameters. • Create and study a DMSO - Au(111) adsorption model exploring different configurations and simulation parameters. • Try to replicate the self - assembled structures observed in STM images. • Evaluate the possible presence of water at the interface through classical and quantum methods. • Simulate STM images to compare the theoretical model to the experimental data. Research project 1) Interact with the experimental group 2) Optimize the metal surface Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 162 •Optimize the lattice constant •Create a slab and optimize the simulation parameters 3) Model the DMSO adsorption on metal surface •Compare different pseudopotenzials and optimize the simulation parameters •Model DMSO •Create an ab-initio adsorption model for a DMSO molecule •Create an ab-initio model for DMSO self-assembly •Simulate STM images of the system •Perform a QM/MM Dynamics on the Gold-DMSO system 4) Model the TFE adsorption on metal surface •Compare different pseudopotenzials and optimize the simulation parameters •Model TFE •Create an ab-initio adsorption model for a TFE molecule •Create an ab-initio model for TFE self-assembly •Simulate STM images of the system •Perform a QM/MM Dynamics on the Gold-TFE system 5) Model the adsorption of amino-acids on metal surface 6) Model small peptides adsorption on metal surface 7) Model other surfaces with different chemical properties Educational Activity foreseen • Participate in a Winter School of QM/MM Molecular Dynamics held at ICTP in Grignano. • Learn QM/MM codes like AMBER and LAMMPS. • Attend a course on Intermolecular forces and potentials, organized by Prof. Scoles. • Attend a course on electron microscopy techniques. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 163 5.Elenco dei componenti del collegio docenti Componente Ente AFRICH Cristina IOM‐CNR Dipartimento Not assigned BARALDI University Trieste Department of Physics ‐ DF Alessandro BERTI Federico University Trieste Department of Chemical and Pharmaceutical Science ‐ DSCF BIASIOL Giorgio IOM‐CNR Advanced Technology and Nanoscience ‐ TASC INFM BONIN Serena University Trieste Clinical Department of Medical Science, Surgery and Health ‐ DCSMCS BRESCHI University Trieste Clinical Department of Medical Lorenzo Science, Surgery and Health ‐ DCSMCS CADENARO University Trieste Clinical Department of Medical Milena Science, Surgery and Health ‐ DCSMCS CASALIS Elettra Not assigned Loredana Synchrotron Spa CESARO Attilio University Trieste Department of Life Science ‐ DLS COJOC Dan Advanced Technology and Nanoscience ‐ TASC INFM University Trieste Department of Physics ‐ DF SSD FIS/03 ASS FIS/03 RU CHIM/06 RU RIC MED/34 RU Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 Ruolo Collegio External expert Exclusive Member Member Member non academic Exclusive Member MED/28 PA Exclusive Member MED/28 PA Exclusive Member RIC CHIM/04 PO IOM‐CNR COMELLI Giovanni DA ROS Tatiana University Trieste Department of Chemical and Pharmaceutical Science ‐ DSCF DE VITA University Trieste Department of Engineering and Alessandro Architecture ‐ DIA DI LENARDA University Trieste Clinical Department of Medical Roberto Science, Surgery and Health ‐ DCSMCS FASSINA University Padova Not assigned Ambrogio FERMEGLIA University Trieste Department of Engineering and Maurizio Architecture ‐ DIA FIRRAO University Udine Department of Biology and Plant Giuseppe Protection ‐ DBPP (UD) FORNASIERO University Trieste Department of Chemical and Paolo Pharmaceutical Science ‐ DSCF FRALEONI Elettra Not assigned Alessandro Synchrotron Spa FRONZONI University Trieste Department of Chemical and Giovanna Pharmaceutical Science ‐ DSCF Qualifica RIC FIS/03 PO CHIM/08 RU ING‐ PA IND/22 MED/28 PO Member non academic Exclusive Member Member non academic Exclusive Member Exclusive Member Exclusive Member Exclusive Member MED/08 PO Member ING‐ IND/24 AGR/12 PO Director PA Member CHIM/03 PA RIC CHIM/02 PA Exclusive Member Member non academic Exclusive Member 164 Componente Ente Dipartimento SSD Qualifica GAMINI Amelia University Trieste Department of Life Science ‐ DLS CHIM/04 RU GIRALDI Tullio University Trieste Department of Life Science ‐ DLS BIO/14 KISKINOVA Maya LAZZARINO Marco LUGHI Vanni Elettra Synchrotron Spa IOM‐CNR MACOR Paolo PO Not assigned RIC Advanced Technology and Nanoscience ‐ TASC INFM University Trieste Department of Engineering and Architecture ‐ DIA University Trieste Department of Life Science ‐ DLS RIC MARSI Stefano University Trieste Department of Engineering and Architecture ‐ DIA MARZARI University Trieste Department of Life Science ‐ DLS Roberto MORGANTE University Trieste Department of Physics ‐ DF Alberto ONESTI Silvia Elettra Not assigned Synchrotron Spa PASQUATO University Trieste Department of Chemical and Lucia Pharmaceutical Science ‐ DSCF PASSAMONTI University Trieste Department of Life Science ‐ DLS Sabina PRATI Ubaldo Fund. Tommaso Not assigned Campanella PRICL Sabrina University Trieste Department of Engineering and Architecture ‐ DIA RUBINI Silvia IOM‐CNR Advanced Technology and Nanoscience ‐ TASC INFM SBAIZERO Orfeo University Trieste Department of Engineering and Architecture ‐ DIA SCAINI Denis Elettra Not assigned Synchrotron Spa SCHMID Chiara University Trieste Department of Engineering and Architecture ‐ DIA SERGO Valter University Trieste Department of Engineering and Architecture ‐ DIA STANTA Giorgio University Trieste Clinical Department of Medical Science, Surgery and Health ‐ DCSMCS TOFFOLI CRO Aviano Not assigned Giuseppe TORMEN IOM‐CNR Advanced Technology and Massimo Nanoscience ‐ TASC INFM Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 ING‐ RIC IND/22 MED/04 RIC ING‐ INF/01 BIO/06 RU FIS/01 PA PO RIC CHIM/06 PA BIO/10 RIC P.Osp ING‐ IND/24 PA RIC ING‐ IND/22 PO RIC ING‐ PA IND/22 ING‐ PO IND/22 MED/08 PA P.Osp RIC Ruolo Collegio Exclusive Member Member non academic Member non academic Member non academic Exclusive Member Exclusive Member Exclusive Member Exclusive Member Vice Director Member non academic Exclusive Member Exclusive Member Member non academic Exclusive Member Member non academic Exclusive Member Member non academic Exclusive Member Exclusive Member Member Member non academic Member non academic 165 Componente UGO Paolo VACCARI Lisa Ente University Venezia Elettra Synchrotron Spa Dipartimento SSD Qualifica Not assigned CHIM/01 PA Not assigned RIC Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 Ruolo Collegio Exclusive Member Member non academic 166 6. Produzione scientifica del collegio docenti 2007-2012 Personale di ruolo nelle università italiane e INAF 1. BARALDI Alessandro • SAVIO L, GERBI A, VATTUONE L, BARALDI A., COMELLI G, ROCCA M (2006). Monitoring super- and subsurface oxygen on Ag(210) by high energy resolution X-ray photoelectron spectroscopy: Subsurface diffusion and segregation. JOURNAL OF PHYSICAL CHEMISTRY. B, CONDENSED MATTER, MATERIALS, SURFACES, INTERFACES & BIOPHYSICAL, vol. 110; p. 942-, ISSN: 1520-6106 • WESTSTRATE C.J, BAKKER J.W, RIENKS E.D.L, VINOD C.P, LIZZIT S, PETACCIA L, BARALDI A., NIEUWENHUYS B.E (2006). Synchrotron XPS and desorption study of the NO chemistry on a stepped Pt surface. SURFACE SCIENCE, vol. 600; p. 1991, ISSN: 0039-6028 • BIANCHETTIN L, BARALDI A., DE GIRONCOLI S, LIZZIT S, PETACCIA L, VESSELLI E., COMELLI G, ROSEI R (2006). Geometric structure of the N/Rh(100) system by core-level photoelctron spectroscopy: Experiment and theory. PHYSICAL REVIEW. B, CONDENSED MATTER AND MATERIALS PHYSICS, vol. 74; p. 045430-, ISSN: 10980121, doi: 10.1103/PhysRevB.74.045430 • F. BUATIER DE MONGEOT, A. TOMA, A. MOLLE, S. LIZZIT, L. PETACCIA, BARALDI A. (2006). Carbon monoxide dissociation on Rh nanopyramids. PHYSICAL REVIEW LETTERS, vol. 97; p. 56103, ISSN: 0031-9007 • BIANCHETTIN L, BARALDI A., VESSELLI E, DE GIRONCOLI S, LIZZIT S, PETACCIA L, COMELLI G., ROSEI R (2007). Experimental and Theoretical Surface Core Level Shift Study of the S-Rh(100) Local Environment. JOURNAL OF PHYSICAL CHEMISTRY. C, NANOMATERIALS AND INTERFACES, vol. 111; p. 4003-, ISSN: 1932-7447 • BARALDI A., BIANCHETTIN L, VESSELLI E, DE GIRONCOLI S, LIZZIT S, PETACCIA L, ZAMPIERI G, COMELLI G., ROSEI R (2007). Highly under-Coordinated Atoms at Rh Surfaces: Interplay of Strain and Coordination Effects on Core Level Shift. NEW JOURNAL OF PHYSICS, vol. 9; p. 143-, ISSN: 1367-2630 • BUATIER DE MONGEOT F, TOMA A, MOLLE A, LIZZIT S, PETACCIA L, BARALDI A. (2007). Self-organised synthesis of Rh nanostructures with tunable chemical reactivity. NANOSCALE RESEARCH LETTERS, vol. 2; p. 251, ISSN: 1931-7573 • BARALDI A., VESSELLI E., BIANCHETTIN L, COMELLI G, LIZZIT S, PETACCIA L, DE GIRCONCOLI S, LOCATELLI A, MENTES O.T, ABALLE L, WEISSENRIEDER J, ANDERSEN J.N (2007). The (1x1)-> hexagonal phase transition on Pt(100) studied by high resolution core level photoemission. THE JOURNAL OF CHEMICAL PHYSICS, vol. 127; p. 164702-, ISSN: 0021-9606, doi: 10.1063/1.2794344 • DING X, DE ROGATIS L, VESSELLI E, BARALDI A., COMELLI G, ROSEI R, SAVIO L, VATTUONE L, ROCCA M, FORNASIERO P, ANCILOTTO F, BALDERESCHI A, PERESSI M. (2007). Interaction of carbon dioxide with Ni(110): a combined experimental and theoretical study. PHYSICAL REVIEW. B, CONDENSED MATTER AND MATERIALS PHYSICS, vol. 76; p. 195425-(1-12), ISSN: 1098-0121, doi: 10.1103/PhysRevB.76.195425 • TAIT S.L, WANG Y, LIN N, COSTANTINI G, BARALDI A., ESCH F, LIZZIT S, PETACCIA L, KERN K (2008). MetalOrganic coordination interactions in Fe-Teraphthalic acid networks on Cu(100). JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, vol. 130; p. 2108-2113, ISSN: 0002-7863 • BARALDI A. (2008). Structure and chemical reactivity of transition metal surfaces as probed by synchrotron radiation core-level photoelectron spectroscopy. JOURNAL OF PHYSICS. CONDENSED MATTER, vol. 20; p. 93001, ISSN: 0953-8984 • L. BIANCHETTIN, BARALDI A., S. DE GIRONCOLI, E. VESSELLI, S. LIZZIT, L. PETACCIA, G. COMELLI, R. ROSEI (2008). Core level shifts of under-coordinated Pt atoms. THE JOURNAL OF CHEMICAL PHYSICS, vol. 128; p. 114706-, ISSN: 0021-9606 • E. VESSELLI, L. BIANCHETTIN, BARALDI A., A. SALA, G. COMELLI, L. PETACCIA, S. LIZZIT, S. DE GIRONCOLI (2008). The Ni3Al(111) surface structure: experiment and theory. JOURNAL OF PHYSICS. CONDENSED MATTER, vol. 20; p. 195223-, ISSN: 0953-8984 • T. STAUDT, A. DESIKUSUMASTUTI, M. HAPPEL, E. VESSELLI, BARALDI A., S. GARDONIO, S. LIZZIT, F. ROHR AND J. LIBUDA (2008). Modelling NOx storage meterials: a high-resolution photoelectron spectroscopy study on the interaction of NO2 with Al2O3/NiAl(110) and BaO/Al2O3/NiAl(110). JOURNAL OF PHYSICAL CHEMISTRY. C, NANOMATERIALS AND INTERFACES, vol. 112; p. 9835-, ISSN: 1932-7447 • VESSELLI E, CAMPANIELLO M, BARALDI A., BIANCHETTIN L, AFRICH C, ESCH F, LIZZIT S, COMELLI G. (2008). A Surface Core Level Shift Study of Hydrogen-Induced Ordered Structures on Rh(110). JOURNAL OF PHYSICAL CHEMISTRY. C, NANOMATERIALS AND INTERFACES, vol. 112; p. 14475-, ISSN: 1932-7447 • VESSELLI E, DE ROGATIS L, DING X, BARALDI A., SAVIO L, VATTUONE L, ROCCA M, FORNASIERO P, PERESSI M., BALDERESCHI A, ROSEI R, COMELLI G (2008). Carbon Dioxide Hydrogenation on Ni(110). JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, vol. 130(34); p. 11417-11422, ISSN: 0002-7863, doi: 10.1021/JA802554G • S. LIZZIT, Y. ZHANG, K.L. KOSTOV, L. PETACCIA, BARALDI A., R. LARCIPRETE, D. MENZEL, K. REUTER (2009). O- and H- induced surface core level shifts on Ru(0001): prevalence of the additivity rule. JOURNAL OF PHYSICS. CONDENSED MATTER, vol. 21; p. 134009, ISSN: 0953-8984 • M. BIANCHI, D. CASSESE, A. CAVALLIN, R. COMIN, F. ORLANDO, L. POSTREGNA, E. GOLFETTO, S. LIZZIT, BARALDI A. (2009). Clean and oxygen induced surface core level shift on Ir(111). NEW JOURNAL OF PHYSICS, vol. 11; p. 063002, ISSN: 1367-2630 • BIANCHETTIN L, BARALDI A., DE GIRONCOLI S, VESSELLI E, LIZZIT S, COMELLI G., ROSEI R (2009). Surface Core Level Shift: High Sensitive Probe to Oxygen-Induced Reconstruction of Rh(100). JOURNAL OF PHYSICAL CHEMISTRY. C, NANOMATERIALS AND INTERFACES, vol. 113; p. 13192-, ISSN: 1932-7447 • S. LIZZIT, BARALDI A., CH. GRÜTTER, J.H. BILGRAM, PH. HOFMANN (2009). The surface phase transition and low temperature phase of α-Ga(010) studied by SPA-LEED. SURFACE SCIENCE, vol. 603; p. 3222, ISSN: 00396028 Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 167 • P. LACOVIG, M. POZZO, D. ALFÈ, P. VILMERCATI, BARALDI A., S. LIZZIT (2009). Growth of dome-shaped carbon nanoislands on Ir(111): the intermediate between carbidic clusters and quasi free-standing graphene. PHYSICAL REVIEW LETTERS, vol. 103; p. 166101, ISSN: 0031-9007 • DE ROGATIS L, VESSELLI E, BARALDI A., CASULA M.F, MONTINI T, COMELLI G, GRAZIANI M, FORNASIERO P. (2009). Charge Redistribution at the Embedded Rh-Alumina Interface. JOURNAL OF PHYSICAL CHEMISTRY. C, NANOMATERIALS AND INTERFACES, vol. 113(42); p. 18069-18074, ISSN: 1932-7447, doi: 10.1021/JP905736Q • GOLFETTO E., BARALDI A., POZZO M., ALFÈ D., SALA A., LACOVIG P., VESSELLI E., LIZZIT S., COMELLI G., ROSEI R. (2010). Determining the chemical reactivity trends of Pd/Ru(0001) pseudomorphic overlayers: core level shift measurements and DFT calculations. JOURNAL OF PHYSICAL CHEMISTRY. 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RIFERIMENTI NORMATIVI DM.224 Nota DM.50/2010 /99 art.2 MIUR Programmazio ne 2010-2012 n.640/2 INDICATORI E RANGE GIUDIZI INDIRI ZZI MIUR 011 punti a) b) ‐ comma 3 lett. a), b), c) (ovvero 1° - 2° - 3° Requisit o) punto c) comma 3 lett. d) (ovvero 4° Requisit o) punto B12 1 Qualità scientifi ca, elevati requisit i di struttur ee risorse per la ricerca 2 Impatt o dottora to – mondo produtt ivo a) Composizione collegio docenti N docenti esclusivi nei SSD del corso b) Produzione scientifica del collegio docenti Valutazione c) Pubblicazioni scientifiche dei dottorandi Valutazione d) Iniziative di pubblicizzazione delle tesi di dottorato Valutazione POSITIVO / NEGATIVO (è obbligatorio per tutti OpenstarTS) e) Disponibilità risorse e strutture Valutazione INSUFF – SUFF – BUONO ‐ OTTIMO f) Livello di soddisfazione dei dottorandi % soddisfatti questionario dottorandi 2010 />= 50% INSUFF 35%< =/ <50% SUFF 20%<= / <35% BUONO /<20% OTTIMO a) Inserimento lavorativo dottori di ricerca (monitoraggio annuale inviato al NV) % dottori con inserimento lavorativo connesso al titolo ultimi 6 anni %<=30 o non fornito => INSUFF 30< % <=50 => SUFF 50< % <=70 => BUONO % >70 => OTTIMO b) Cofinanziamento delle borse previsto per il XXVII ciclo % borse finanziate con fondi privati italiani e stranieri % <= 10 BASSO 10 < % <= 30 MEDIO % > 30 ALTO c) Fonte di finanziamento dei progetti di ricerca attivi nei dipartimenti proponenti % di fondi provenienti da privati italiani e stranieri Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 N >= min => ADEGUATO N < min => NON ADEGUATO INSUFF – SUFF – BUONO ‐ OTTIMO INSUFF – SUFF – BUONO ‐ OTTIMO % <= 10 BASSO 10 < % <= 30 MEDIO % > 30 ALTO 204 RIFERIMENTI NORMATIVI DM.224 Nota /99 art.2 MIUR n.640/2 011 punto d) DM.50/20 INDICATORI E RANGE GIUDIZI INDIRIZZI MIUR 10 Program mazione 20102012 punto B12 3 a) Attrattività dottorato Razionalizza zione dei corsi b) Attrattività dottorato sulle altre sedi comma 3 lett. b) (ovvero 2° Requisit o) c) Apertura sede N candidati presenti alla prova/ N posti con borsa banditi N candidati laureati altro ateneo presenti alla prova / N totale candidati presenti alla prova N iscritti dottorato provenienti da altri atenei / N iscritti totali d) Dimensione prevista del dottorato N posti ordinari XXVII e) Dimensione effettiva del dottorato media degli iscritti negli ultimi 3 cicli (confrontata con posti e borse previsti) comma 2 comma 3 lett. a), e) (ovvero 1° - 5° Requisit o) punto e) ‐ 4 Ampiezza delle tematiche scientifiche con riferimento a discipline riconoscibili a livello internazional e a) Denominazione chiara e traducibile Valutazione b) Coerenza tra tematiche scientifiche e denominazione Valutazione c) Ampiezza tematiche scientifiche N SSD di riferimento del corso d) Adeguata formulazione delle tematiche scientifiche e degli obiettivi formativi Valutazione Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 N < 2 BASSA 2 <= N <= 4 MEDIA N > 4 ALTA % <= 10 BASSA 10 < % <= 25 MEDIO‐BASSA 25 < % <= 45 MEDIA 45 < % <= 60 MEDIO‐ALTA % > 60 ALTA % <= 10 BASSA 10 < % <= 25 MEDIO‐BASSA 25 < % <= 45 MEDIA 45 < % <= 60 MEDIO‐ALTA % > 60 ALTA ADEGUATA – NON ADEGUATA (con riferimento al tipo corso e agli iscritti effettivi) ADEGUATA – NON ADEGUATA (con riferimento al tipo corso e al numero delle borse) ADEGUATA – NON ADEGUATA SI – NO ADEGUATA se N >= 3 NON ADEGUATA se N < 3 ADEGUATA – NON ADEGUATA 205 RIFERIMENTI NORMATIVI INDICATORI E RANGE GIUDIZI INDIRIZZI MIUR DM.224 Nota DM.50/20 /99 art.2 MIUR 10 n.640/2 Program 011 mazione 20102012 comma 3 lett. d) (ovvero 4° Requisit o) punto f) ‐ 5 Internaziona lizzazione a) Convenzioni con soggetti esteri per attività formative dottorandi b) Fonte di finanziamento dei progetti di ricerca attivi nei dipartimenti proponenti c) Presenza di iscritti stranieri d) Sito web del dottorato Valutazione PREVISTE – NON PREVISTE % di fondi provenienti da soggetti stranieri N iscritti stranieri / N iscritti totali Valutazione % <= 20 BASSO 20 < % <= 40 MEDIO % > 40 ALTO % < 10 BASSO 10 <= % < 20 MEDIO % > =20 ALTO INSUFFICIENTE ‐ SCARSO – SUFFICIENTE – DISCRETO – BUONO – MOLTO BUONO – OTTIMO comma 3 lett. f) ‐ (ovvero 6° Requisit o) ‐ 6 Adozione di sistemi di valutazione Valutazione ADEGUATO – NON ADEGUATO Sistemi di Valutazione Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 206 8. Giudizi dei referee esterni per dottorandi ammessi all’esame finale aprile 2013 Di seguito sono riportati i referee esterni scelti dal collegio per ciascuno dei dottorandi: Studente Supervisore AMBROSINI RUBINI Stefano Silvia Titolo Reviewers Growth and characterization Anna Fontcuberta i Morral, École of nanostructures. polytechnique fédérale de Lausanne Helge Weman, Norwegian University of Science and Technology CHEN Yan FORNASIE Nanostructured Titanium Giovanni Zangari, University of Xin RO Paolo Dioxide Based Materials for Virginia Photocatalysis and Hansjörg Grützmache, ETH Zürich Phototelectrocatalysis BIDOGGIA PASQUATO Mixed-monolayers Fabrizio Mancin, Università degli Silvia Lucia protected gold nanoparticles Studi di Padova, for applications in medicine Durand Grégory, University d’Avignon, GANAU SCOLES Nanotechnology Milan Skrap, Università di Udine Mario Giacinto applications in quantitative Francesco Stellacci, EPFL, Lausanne, neuroscience: proteomic Switzerland analyses of malignant gliomas GIORGIS ROMANAT Design, fabrication and Filiberto Bilotti, Università di Roma 3 Valentina O Filippo characterization of Jakub Dostalek, Austrian Institute of metamaterials inspired Technology plasmonic structures for sensing application LUCAFO' SAVA Study of carbon Christian Gaiddon, Centre National de Marianna Gianni nanostructures as carriers la Recherche Scientifique, France for drugs for cancer Paul J Dyson, EPFL, Lausanne, chemotherapy. Switzerland MARSICH SERGO Design and synthesis of Peter HIldebrandt, Technische Lucia Valter functionalized metal Universitaet Berlin nanoparticles for bio- Freek Ariese,Vrije Universiteit analysis with Surface- Amsterdam Enhanced Raman Scattering (SERS) PERONIO COMELLI Single-molecule Gian Paolo Brivio, Università' Angelo Giovanni heterogeneous catalysis Bicocca di Milano. Saw Wai Hla, Argonne National Laboratory SAMMITO ROMANAT Integration of plasmonic Theodoros Dimopoulos, Austrian Davide O Filippo gratings into optoelectronic Institute of Technology devices Emiliano Descrovi, Poitecnico di Torino ZANUSSO TOFFOLI Nanotechnologies and Enrico Mini, Università di Firenze. Chiara Giuseppe oncology: pharmacokinetics Emilio Clementi, Università di Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 207 and pharmacogenomics to Milano. optimize the antitumor therapies Vedi dettaglio negli allegati. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 208 9.Presentazioni dei dottorandi al congesso del gennaio 2013 Le presentazioni PPT dei dottorandi al congresso del gennaio 2012 sono riportate negli allegati. Scuola di dottorato di ricerca in Nanotecnologie: attività 2013 209