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Table of contents
Introduction
Chapter 1 State of the art
1.1. Introduction
1.2. Surface modification
1.2.1 Thiols
1.2.2 Diazonium salts
1.2. Dynamic investigations
1.2.2 Characterization at the macro/microscale
1.2.3 Characterization at the nanoscale
1.3. Electrochemical tip-enhanced Raman spectroscopy
1.3.1 First TERS developments
1.3.2 TERS developments in air
1.3.3 TERS in liquid and under electrochemical conditions
Chapter 2 STM-TERS under electrochemical conditions – Experimental developments & implementation
2.1. Introduction
2.2. Elaboration of TERS-active bulk metal probes
2.2.1 Design of plasmonic amplifiers
2.2.2 TERS probe from etched gold wires
2.3. Raman and STM coupling: technical implementation
2.3.1 Optical construction of the Raman microscope
2.3.2 SPM/ Raman coupling platform and choice of the illumination geometry ..
2.4. EC-STM-TERS analyses: setups and modus operandi
2.4.1 First prototype of the EC-STM-TERS setup
2.4.2 Optimization of the EC-STM-TERS setup
2.4.3 EC-STM-TERS analyses – Step-by-step implementation
2.4.4 Assessment of the TERS signal stability with the potential
2.5. Conclusion
Chapter 3 Study of a complex reduction mechanism on a model sample
3.1. Introduction
3.2. 4-NBM as model system
3.2.1 SAM sample preparation
3.2.2 Electrochemical measurements
3.3. EC-STM-TERS: real-time following of the reduction mechanism
3.3.1 EC-TERS experimental conditions
3.3.2 Mapping at fixed potential
3.3.3 Deciphering of the reaction mechanism by real-time TERS
3.4. Discussions and conclusions
Chapter 4 Diazonium-based structures: influence of the thickness on the electrochemical reactivity
4.1. Introduction
4.2. Elaboration of functionalized surfaces by controlling diazonium chemistry
4.2.1 Electrochemical grafting of 4-NB radicals on gold
4.2.2 Control of 4-NBD layer growth with a redox cross-inhibitor
4.2.3 Characterization of the grafted layers
4.2.4 STM-TERS mapping in air
4.3. Surface reactivity screening by EC-TERS mapping
4.3.1 Measurement setup
4.3.2 TERS mapping under polarization
4.3.3 Structure-reactivity relationships
4.4. Conclusions
Conclusions and perspectives
Annexes
Comparison of ChA and DPPH performances as inhibitors
Abbreviations
Bibliography
