Evaporation Induced Self-Assembly (EISA)

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Table of contents

1. Chapter I. Bibliographical introduction
1.1. Electrified interface between two immiscible electrolyte solutions
1.1.1. Liquid – liquid interface structure
1.1.2. Charge transfer reactions at the ITIES
1.1.2.1. Simple ion transfer reaction
1.1.2.2. Assisted/facilitated ion transfer
1.1.2.3. Electron transfer across ITIES
1.1.2.4. Electrochemically induced interfacial adsorption
1.1.3. Potential window and limiting current
1.1.4. Electrochemical instability at the electrified liquid – liquid interface in the presence of ionic surfactants
1.1.5. Miniaturization of the ITIES
1.2. Sol – Gel Process of Silica employing Template Technology
1.2.1. Nomenclature and physicochemical properties of silicon and silicon containing compounds
1.2.2. The Sol – Gel process of silica
1.2.2.1. Hydrolysis
1.2.2.2. Condensation
1.2.2.3. Dissolution
1.2.2.4. Curing
1.2.3. Templates – towards surface engineering
1.2.4. A soft template for a Sol-Gel process of mesoporous silica thin films
1.2.5. Functionalized mesoporous silica films prepared by Sol-Gel processing
1.3. Liquid – liquid interface modification
1.3.1. Metals at the electrified liquid – liquid interface.
1.3.1.1. Au deposition at the ITIES
1.3.1.2. Ag deposition at the electrified ITIES
1.3.1.3. Pd and Pt deposition at the electrified ITIES
1.3.2. Phospholipids at the electrified liquid – liquid interface
1.3.3. Organic polymers at the polarized liquid – liquid interface
1.3.4. Carbon based materials at/near polarized liquid – liquid interface
1.3.5. Silica modified liquid – liquid interface
1.3.5.1. Three phase junction systems
1.3.5.2. Neat, non-polarized liquid – liquid interface in situ modification with silica material..
1.3.5.3. Electrified Interface between Two Immiscible Electrolyte Solutions modification with silica materials
1.3.5.3.1. Ex situ modification
1.3.5.3.2. In situ modification
2. Chapter II. Experimental part
2.1. Chemicals
2.2. Electrochemical set-ups
2.3. Composition of electrochemical cells. The aqueous and the organic phase preparation
2.4. Instrumentation
2.5. Protocols
2.5.1. Preparation procedure of BTPPA+TPBCl-
2.5.2. Preparation procedure of CTA+TPBCl-
2.5.3. Preparation procedure of TBA+TPBCl-
2.5.4. Preparation procedure of PH+TPBCl-
2.5.5. Protocol of organic counter electrode preparation
2.5.6. Single pore microITIES protocol of preparation
2.5.7. Protocol of preparation of trimethylbenzhydrylammonium iodide
3. Chapter III. Templated Sol – Gel process of silica at the electrified liquid – liquid interface
3.1. Results and discussion
3.1.1. Electrochemical study
3.1.2. Characterization of silica deposits electrogenerated at the ITIES
3.1.3. Spectroscopic analysis
3.1.4. BET analysis
3.1.5. Morphological characterization
3.2. Conclusion
4. Chapter IV. Silica electrodeposition using cationic surfactant as a template at miniaturized ITIES
4.1. Electrochemical and morphological study of silica deposits at the array of microITIES
4.1.1. Surfactant-template assisted Sol-Gel process of silica at the microITIES
4.1.1.1. Factors affecting silica deposition at the array of microITIES
4.1.1.1.1. Influence of [CTA+]org and [TEOS]aq
4.1.1.1.2. Influence of the pore center-to-center distance
4.1.1.1.3. Influence of the scan rate
4.1.2. Morphological study
4.1.3. Spectroscopic and electrochemical characterization of deposits
4.1.4. Conclusion
4.2. In situ confocal Raman spectroscopy study of interfacial silica deposition at microITIES
4.2.1. Raman spectroscopy analysis of the liquid – liquid interface at open circuit potential
4.2.2. Ion transfer followed by Raman spectroscopy
4.2.3. Interfacial silica deposition followed by Raman spectroscopy
4.2.4. Conclusions
4.3. Electrochemical evaluation of microITIES modified with silica deposits
4.3.1. Blank experiment before and after modification
4.3.2. Single charge ion transfer before and after modification
4.3.3. Multicharged ion transfer before and after modification
4.3.4. Electroanalytical properities of microITIES modified with silica deposits
4.3.5. Conclusion
5. Chapter V. Local pH change at the ITIES induced by ion transfer and UV photolysis
5.1. Synthesis and characterization of trimethylbenzhydrylammonium iodide
5.2. Electrochemical characterization of PH+ transfer at macroITIES
5.3. Study of photodecomposition of PH+ species
5.4. Local pH change induced by electrochemical transfer and photodecomposition of PH+ species
5.5. Silica deposition induced by local pH decrease
5.6. Conclusion
6. General conclusions
7. Further directions
7.1. Silica deposits – SECM characterization
7.2. Silica deposits functionalization
7.3. Interfacially active base
8. References
Appendix I. Nanopipette preparation and silanization
Appendix II. Protocol of preparation of 3-azidopropyltrimethoxysilane