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Tip-Enhanced Raman Spectroscopy (TERS) under electrochemical conditions : towards the in situ characterization of functional nanomaterials

Abstract : The objective of this work has been to expand developments that were further performed in STM towards AFM ones to broaden the range of systems which can be studied such as nanoparticles, 2D materials on conductive or insulating substrates or low-conductivity (multi) layers, passive layers and semiconductor materials among others, as mentioned earlier. Also, the thesis objective is to expand previous TERS development under electrochemical conditions, which has been achieved in the LISE laboratory in 2018, in the STM mode using partially isolated TERS active STM probes, with the new development in the AFM mode. The latter could broaden the range of possible systems which can be studied in the air and liquid and under electrochemical conditions, using hand-made TERS active AFM probes, initiated in this work as well. The initial step in this thesis was the optimization of manufacturing procedure of hand-made AFM-TERS probes, which were further used as the main tool for AFM imaging performances and TERS mapping. The measurements were implemented in the air and in liquid environment, whereas the TERS implementation in liquid, using point spectra, has been demonstrated for the first time using bulk metal AFM probes. Additionally, TERS mapping performances on nano-objects in the air have been performed as well, where the TERS molecule signature and the topography of the nano-particle have been obtained simultaneously. The challenge and core of this work is dedicated to the characterization of developed electroactive system by EC-AFM-TERS. The focus is on the electrochemical reduction of 4-nitrobenzene mercaptan (4-NBM) self-assembled monolayer in acidic and alkaline medium in two different configurations; upright and inverted. Thanks to the new design proposed for the bottom-illumination of AFM-TERS setup, the reduction of a 4-NBM monolayers could be followed in situ. The new setup was used for the first time to evaluate the reactivity of an electroactive (Raman non-resonant) molecular layer obtained by self-assembled monolayer of 4-NBM on gold.
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Submitted on : Thursday, November 24, 2022 - 11:48:11 AM
Last modification on : Friday, November 25, 2022 - 4:12:01 AM

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  • HAL Id : tel-03869392, version 1

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Aja Ana Pavlič. Tip-Enhanced Raman Spectroscopy (TERS) under electrochemical conditions : towards the in situ characterization of functional nanomaterials. Theoretical and/or physical chemistry. Sorbonne Université, 2022. English. ⟨NNT : 2022SORUS264⟩. ⟨tel-03869392⟩

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