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Colloidal Gold Nanoparticles: a Study of Their Drying-Mediated Assembly

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Colloidal Gold Nanoparticles: a Study of Their Drying-Mediated Assembly UNIVERSITY OF HAUTE-ALSACE 2011 A Dissertation Submitted to the Graduate Faculty In Partial Fulfillment of the Requirements For the Degree Doctor of Philosophy in Physical Chemistry Colloidal Gold Nanoparticles: A study of their Drying-mediated Assembly in mesoscale aggregation patterns and of their AFM-assisted Nanomanipulation on model solid surfaces Samer DARWICH December 14, 2011 Examination committee: Prof. Serge STOLL (Principal Examiner) Dr. Hendrik HÖLSCHER (Principal Examiner) Prof. Claudine FILIATRE (Examiner) Dr. Enrico GNECCO (Examiner) Dr. Karine MOUGIN (Co-Advisor) Dr. Hamidou HAIDARA (Supervisor) University of Haute-Alsace A Dissertation Submitted to the Graduate Faculty in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in Physical Chemistry Colloidal Gold Nanoparticles: A Study of their Drying-Mediated Assembly in Mesoscale Aggregation Patterns and of their AFM Assisted Nanomanipulation on Model Solid Surfaces Examination Committee: Prof. Serge STOLL Samer Darwich Dr. Hendrik HÖLSCHER 14 December 2011 Prof. Claudine FILIATRE Dr. Enrico GNECCO Dr. Karine MOUGIN Dr. Hamidou HAIDARA Institut de Science des Matériaux de Mulhouse “Anything which can be counted is finite and will come to an end” Ali Al-Mortadhâ (A) To those who had opened to me the door to live, to learn, to love and to be loved; my father Hassan and my mother Zahra My love for you is uncountable “Yestarday I was with you; today I have become the object of a lesson for you, and tomorrow I shall leave you...” Ali Al-Mortadhâ (A) First of all, I would like to thank Dr. Hamidou Haidara who gave me the opportunity to join his group (“PMA” of the Institut de Science des Matériaux de Mulhouse) and who opened to me the prospects of research world. I am grateful for every discussion we had together, and for every lesson that lights me the way to knowledge. I express my gratitude to his rich humility, his humanity and his great attitude... I am indebted to my co-adviser Dr. Karine Mougin for his help at every step on the road of experimental work. I am thankful for his optimism, his patience and his trust in me. I would also like to thank her because she gave me the opportunity to work in the FANAS project (ESF) which showed me research life in different European countries and which allowed me to meet marked researchers. I would like to thank all the European partners Dr. Enrico Gnecco, Dr. Hendrick Höshler, Dr. Akshata Rao, Dr. Rogerio Colaço, Dr. Mykhaylo Evstigneev, Dr. André Schirmeisen, Dr. Rynno Lohmus, Dr. Guido Paolicelli, Dr. Andrzej Kulik, Dr. Santiago Casado, Dr. Sergei Vlassov, Ms. Patrizia Paradiso and Mr. Tobias Meier to all their near or far contributions in this work especially in the subject of the FANAS project (AFM manipulation of nanoparticles). I am thankful to the examination committee members Dr. Serge Stoll, Prof. Claudine Filiatre, Dr. Enrico Gnecco and Dr. Hendrick Höshler for accepting to evaluate my PhD work. I would like to thank the Director of our institute Dr. Catie Vix for being supportive to each personnel of the institute. I am grateful to all the technical and administrative personnel of the laboratory to their technical support, in particular, Dr. Loïc Vidal (TEM), Mr. Hugues Bonnet and Dr. Ludovic Josien (SEM), Mr. Simon Grée (SERS and UV-VIS), Dr. Aissam Airoudj and Dr. Jean-luc Bubendorff (AFM), Mrs. Marie-Paule Hirn (Centrifugation), Mr. Philippe Kunemann (Contact angle measurements system), Mr. Eric Ehrhard (informatics), Mr. Patrick Lamielle (Plant), Mr. Stéphan Knopf (Store), Mrs. Fabienne Sorgato (Secreteria), Mrs. Natalina Muller, Mrs. Joëlle Dangy and Louisa Idiri (Accounting), Mrs. Nathalie Castelein (Library) and Mrs. Sylvie Forget (Reception). Many thanks to Sylvie to the special time and discussions we had in the hallways of the institute. Many thanks to all of them to the social time shared with them. I am also thankful to all the researchers of the institute to each social and scientific time and discussion shared with them. Particularly I would like to thank Dr. Laurent Vonna, Dr. Vincent Roucoules, Dr. Govindasamy Chandrasekar and Dr. Bassel Haidar... I would like to thank all Ph-D students with whom I shared great moments of a social, scientific and personal perspective. In particular, Enormous thanks to Jalal Bacharouche, Mathieu Wagner, Carine Diebold, Jean-Nicolas Munsch, Patrice Brender, Sébastien Schlinger, Emilien Buet, Judith Böhmler, Guillaume Colombe, Arnaud Bach, Philippe Bernardo, Alexandre Geissler, Marie Palmieri, Mohammad Rajab, Houssam Hamie, Ahmad Fahs, Emilia Kulaga, Nicolas Ducruet, Helena Marques Da Silva, Christine De Saint-Aubin, Alicia Henry and Dorris Moura Campus... I am thankful to my friend Abdallah Ghaddar and to my family, my father Hassan, my mother Zahra and my brothers Mohammad, Alaa’ and Waël. Contents General Introduction 1 Part 1: Presentation of the nanomaterials: Suspension of nanoparticles/ Self-Assembled Monolayers 5 Introduction 6 Chapter 1: Gold Colloidal NPs 11 1.1.0. Introduction 12 a.Methods of preparation 13 b.Modes of stabilization 15 1.1.1. Gold nanospheres 16 a.Synthesis of gold colloidal nanospheres 20 b.Functionnalization of gold colloidal nanospheres 24 c.Characterization of Au NPs suspensions 26 1.1.2. Gold nanorods 29 a.Preparation of gold nanorods 32 b.Functionnalization of gold nanorods 33 c.Characterization of gold nanorods 34 1.1.3. Conclusion 39 Chapter 2: Self assembled monolayers 44 1.2.0. Introduction 45 1.2.1. Elaboration procedure 46 a.Cleaning and surface activation of the substrate 47 b.General preparation procedure of SAMs 47 1.2.2. Homogeneous molecular surfaces 49 a.Preparation of the molecular films 49 b.Characterizations 52 c.Conclusion 55 1.2.3. Heterogeneous molecular surfaces 56 1.2.4. Conclusion 59 Conclusion 61 Part 2: Drying-mediated assembly of gold NPs in mesoscale structures on model solid surfaces 63 Introduction 64 Chapter 1: Complex aggregation patterns issued for drying nanocolloidal suspensions 68 2.1.0. Introduction 69 2.1.1. Theoritical point of view vs. experimental 73 2.1.2. Complex drying patterns of “as-synthesized” Au NPs solution-Dependence of structure formation and aggregate stability on NPs 78 1.Experimental methods 78 2.Results and discussion 79 3.Conclusion 90 2.1.3. The role of salts in the formation of the complex NPs-based structures 91 1.Experimental methods 91 2.Results and discussion 93 3.Conclusion 103 2.1.4.General conclusion 104 Chapter 2: Nanobubbles and nanodroplets template growth of particles nanorings 106 2.2.0. Introduction 107 2.2.1. Experimental methods 111 2.2.2. Results and discussion 112 2.2.3. Conclusion 128 Chapter 3: Drying-mediated assembly structurs of binary solutions of (NPs/biopolymer) mixtures 130 2.3.0. Introduction 131 2.3.1. Experimental methods 137 2.3.2. Results and discussion 139 a.Structural characterization of samples 140 b.The surface microscopic complex aggregation patterns 141 c.Nanoscale aggregation structures 165 2.3.3. Conclusion 172 Conclusion 174 Part 3: Aging of the aggregation structures vs NPs mobility 177 Introduction 178 Chapter 1: Aging of complex NP-based structures 180 3.1.0. Introduction 181 3.1.1. Aging of the complex structures induced by drying of pure colloidal NPs 182 a.Experimental methods 182 b.Results and discussion 183 c.Conclusion 192 3.1.2. Aging of the complex structures induced by drying of mixed (alginate/NPs) solutions 193 3.1.3. Conclusion 198 Chapter 2: AFM Manipulation of NPs on Model Surfaces- a tentative account of the surface mobility and dislocation of aging NPs structures 199 3.2.0. Introduction 200 3.2.1. Experimental methods 203 3.2.2. Results and discussion 205 a.Influence of the size and the shape of NP 205 b.Influence of the chemistry of NP 210 c.Influence of the temperature 211 d.Organization effects 212 e.Influence of the relative humidity 213 f.Influence of the topography of the substrate 219 g.Influence of scan velocity 221 3.2.3. Conclusion 223 Conclusion 225 General conclusion 227 General Annexe: Combined electrostatic-covalent building of gold nanoparticles multilayers, and their size enhanced cohesive and SERS properties A1 General Introduction The development and the structuring of materials at the nanoscale can address new physics but also can perform features that are operating on original principles. This originality is determined by the unique properties of nanomaterials. These properties are used in particular for new technological applications in many fields: medicine, energy, electronics, optics, catalysis... The critical parameter in most of these properties is the small size of the material itself or of the unit object composing the nanomaterial (typically from 1 nm to 100 nm) that causes an increase in the (surface / volume) ratio. This work deals with the study of the drying-mediated assembly of colloidal gold nanoparticles (Au NPs) in mesoscale aggregation patterns and their manipulation by atomic force microscopy (AFM) on model surfaces. The objective of this work is twofold. First, it is aimed at understanding and controlling the genesis of original drying structures and patterns NPs based complex fluids. And secondly, we seek to understand and relate the stability of the NP-based structures (cohesion and dislocation/ desaggregation) to the intrinsic mobility of the constitutive unit NPs on various substrates. First, we will discuss the synthesis of two nanostructured materials. These materials are the basis of systems development at the mesoscopic scale, but also of the fundamental understanding of phenomena and physical parameters that are acting at the nanoscale. These materials are the Au NPs and the self-assembled molecular surfaces (SAMs) on rigid substrates, which are the supports for the assembly and the structuring of NPs. The morphology (size and shape) and the surface chemistry (functionality of grafted molecules) of NPs are adjusted during their chemical synthesis to control the physical and the chemical properties of the studied nano-objects.
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