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Transparent Nanostructured Metal Oxides for Chemical Biosensors: Towards Point-Of-Care Environments

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Transparent Nanostructured Metal Oxides for Chemical Biosensors: Towards Point-Of-Care Environments Transparent nanostructured metal oxides for chemical biosensors: towards point-of-care environments Raquel Pruna Morales ADVERTIMENT. La consulta d’aquesta tesi queda condicionada a l’acceptació de les següents condicions d'ús: La difusió d’aquesta tesi per mitjà del servei TDX (www.tdx.cat) i a través del Dipòsit Digital de la UB (diposit.ub.edu) ha estat autoritzada pels titulars dels drets de propietat intel·lectual únicament per a usos privats emmarcats en activitats d’investigació i docència. No s’autoritza la seva reproducció amb finalitats de lucre ni la seva difusió i posada a disposició des d’un lloc aliè al servei TDX ni al Dipòsit Digital de la UB. No s’autoritza la presentació del seu contingut en una finestra o marc aliè a TDX o al Dipòsit Digital de la UB (framing). Aquesta reserva de drets afecta tant al resum de presentació de la tesi com als seus continguts. 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On having consulted this thesis you’re accepting the following use conditions: Spreading this thesis by the TDX (www.tdx.cat) service and by the UB Digital Repository (diposit.ub.edu) has been authorized by the titular of the intellectual property rights only for private uses placed in investigation and teaching activities. Reproduction with lucrative aims is not authorized nor its spreading and availability from a site foreign to the TDX service or to the UB Digital Repository. Introducing its content in a window or frame foreign to the TDX service or to the UB Digital Repository is not authorized (framing). Those rights affect to the presentation summary of the thesis as well as to its contents. In the using or citation of parts of the thesis it’s obliged to indicate the name of the author. Transparent nanostructured metal oxides for chemical biosensors: towards point-of-care environments Autor: Director y tutor: Raquel Pruna Morales Dr. Manuel L´opez de Miguel Memoria presentada para optar al grado de doctor por la Universidad de Barcelona Programa de doctorado en Ingenier´ıay Ciencias Aplicadas Departamento de Ingenier´ıaElectr´onica y Biom´edica Facultad de F´ısica Universidad de Barcelona Barcelona, junio de 2019 “All you need is faith, trust and a little bit of pixie dust.” Peter Pan Acknowledgements En primer lugar no podr´ıa estar otro que el director, tutor y gran responsable de esta tesis, Manel L´opez: me enga˜n´oal empezar, sigui´oenga˜n´andome durante los a˜nos de m´aster y tesis y finalmente parece que hemos sacado algo de verdad. Muchas gracias por aguantarme, ayudarme y empujarme hasta llegar al final. Al resto del equipo, Fran Palacio y Fernando Arreza. Sin vosotros (y vuestra pa- ciencia), todo esto no hubiera sido posible. Part del temps que ha durat aquesta tesi l’he passat a l’ICMAB, aix´ıque gr`acies als professors Francesc Teixidor i Clara Vi˜nas (i equip) per obrir-me les portes de casa seva i tractar-me com a una m´es del grup. Val a dir que no tot el temps l’hem dedicat a treballar, ja ´es mala sort haver coincidit en una `epoca tan convulsa... (o no? Ho hem passat molt b´e!). Muchas gracias al mayor pecador de la pradera que he conocido, el profesor Abdel- hamid Errachid. Thanks as well to the rest of the ISA team; it was a pleasure to stay at Lyon those months. Special thanks to the jamoncito Abdel: all your knowledge, ideas and comments were also very helpful, and without them this work wouldn’t have been possible. You manage! Gracias al resto de compa˜neros de estos a˜nos, en especial a Mauri por su apoyo y ayuda, caf´es,charletas... A Angel´ Di´eguez, por prestarme su firma. A Oriol Monereo, por todas las horas de caf´esy tertulia, y por revisar este manuscrito. A todos los que de alg´un modo hab´eis contribuido a esta tesis o me hab´eis acompa˜nado estos a˜nos: Catalina, Juan Pablo, Miriam, M`onica Mart´ınez, Oriol Bl´azquez, Rom´en... Gracias a todos. A les nenes del Masnou, per ser-hi sempre i des de sempre. Manel Bosch, tu tamb´e hi ets des de (gaireb´e)sempre, bien qu’on ne se voie pas souvent... Por el apoyo incondicional a lo largo de los a˜nos quiero agradecer a mis padres, Jordi y Feli; a mi hermano, Aitor; als avis i tieta Eli; a todos los que est´an un poqu´ınm´as lejos, y a los que ya no est´an. A mi segunda familia, Montse y Jose. Gracias por tanto. A Urf, mi paz y mi equilibrio (a veces... otras veces me das la vida m´artir, salao ). Qu´ea˜nos te he dado con esto, ¿eh? Y ah´ıhas estado, haciendo de cada d´ıa una aventura, en todos los lugares donde hemos estado, siempre sonriendo. Y lo que queda. “T´utan s´olo ilum´ıname con tu presencia cada d´ıa”. v Contents Acknowledgements v Contents vii 1 Introduction 1 1.1 Motivation: towards a very early-stage detection using smart biosensors 1 1.1.1 Medical diagnosis along history: a brief overview . 1 1.1.2 Medical diagnosis today: the concept of biomarker and early de- tection................................. 4 1.1.3 Towards point-of-care assistance: biosensors and lab-on-a-chip . 5 1.1.4 New horizons in biosensing: environmental care and food analysis 7 1.2Aboutthiswork............................... 8 1.2.1 Hypothesisandobjectives...................... 8 1.2.2 Dissertationsummary........................ 9 1.2.2.1 Specificcontributions................... 11 1.2.3 Organisationofthethesis...................... 12 1.2.4 Listofpublications.......................... 13 2 Theoretical background 15 2.1 Part I: The sensing material. Indium tin oxide . 16 2.1.1 Propertiesofindiumtinoxide.................... 16 2.1.1.1 Physical and structural properties . 16 2.1.1.2 Chemicalproperties.................... 20 2.1.2 Commonpreparationmethods................... 21 2.1.2.1 Chemical vapour deposition (CVD) . 22 2.1.2.2 Spraypyrolysis....................... 22 2.1.2.3 Sputtering......................... 22 2.1.2.4 Atomiclayerdeposition(ALD).............. 23 2.1.2.5 Electron beam (vacuum) evaporation . 23 2.1.2.6 Others........................... 23 2.1.3 ITO nanowire growth by vapour-liquid-solid (VLS) mechanisms . 25 2.1.3.1 TheVLSmethod..................... 25 2.1.3.2 The self-catalyzed VLS method . 26 2.1.4 ApplicationsofITOfilms...................... 26 2.2 Part II: The methodology. Electrochemistry . 30 2.2.1 Variables affecting the rate of electrode reactions . 31 2.2.1.1 Masstransfer........................ 31 2.2.1.2 External variables: thermodynamics of electrochemical cells............................. 31 2.2.1.3 Electricalvariables..................... 33 2.2.1.3.1Voltagestep..................... 34 2.2.1.3.2Voltagesweep.................... 34 vii Contents viii 2.2.1.4 Electrode and solution variables . 35 2.2.2 Kinetics of electrode reactions. Processes occurring at the electrode-solutioninterface..................... 37 2.2.2.1 Preliminary considerations . 37 2.2.2.2 The Butler-Volmer model of electrode kinetics: one-step, one-electronprocesses................... 39 2.2.3 Mott-Schottky analysis of the semiconductor electrode . 40 2.2.4 Electrochemical techniques and potentiostatic configurations . 42 2.2.4.1 Potentiometry....................... 43 2.2.4.2 Linearsweepvoltammetry................ 43 2.2.4.3 Electrochemical impedance spectroscopy . 44 2.3PartIII:Theapplication.Biosensors.................... 47 2.3.1 Classification of biosensors and state-of-the-art . 48 2.3.1.1 Bioreceptor and transducer-wise classifications of biosen- sors............................. 48 2.3.1.2 ITO-based biosensors: the state-of-the-art . 52 2.3.2 Strategies for surface modification and detection of species . 53 2.3.2.1 Crosslinkers for electrode derivatization . 53 2.3.2.1.1Silanecouplingagents............... 53 2.3.2.1.2 Diazonium salt electroaddressing (grafting reac- tions)........................ 57 2.3.2.1.3 Thiolation of surfaces . 58 2.3.2.2 Transductionmechanisms................. 58 2.3.2.2.1Impedance..................... 59 2.3.2.2.2Current....................... 61 2.3.3 Assaysofinterestusedinthiswork................. 63 2.3.3.1 Bovineserumalbumine.................. 63 2.3.3.2 Biotin–streptavidin.................... 63 2.3.3.2.1 Biotinylation and signal amplification . 65 2.3.3.3 Tumour necrosis factor α ................. 66 3 Study of the viability of nanostructured ITO as electrode for electro- chemistry 67 3.1 Thin film versus nanostructured indium tin oxide . 67 3.1.1 Article I: Electrochemical characterization of organosilane - func- tionalized nanostructured ITO surfaces ............... 69 3.2 Nanostructuration of ITO by electron beam evaporation . 77 3.2.1 Influence of substrate temperature and study of the electrical dou- blelayer................................ 77 3.2.1.1 Article II: Tuning the deposition parameters for optimiz- ing the faradaic and non-faradaic electrochemical perfor- mance of nanowire array-shaped ITO electrodes prepared by electron beam evaporation ..............
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