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Preparation of Silica Thin Films for Analytical Chemistry Applications

Abstract : Oriented mesoporous silica-based film on FTO electrode was prepared via electrochemically-assisted self-assembly approach (EASA). A potential of -1.5V was applied to the FTO electrode containing a prehydrolyzed silica precursor, (e.g. tetraethyl orthosilicate), in the presence of a template (e.g. cetrimonium bromide) and electrolyte. This approach could generate vertically-aligned silica nanochannels with pore sizes adjustable between 2 and 3 nm, depending on the template. This work showed the voltammetric behavior and the selectivity of the mesoporous silica film towards various positively-charged cations of different nature, size, and charge. Results showed an accumulation and selectivity favoring the least positive charged ion: MB⁺ > PQ²⁺ > DQ²⁺ > Ru(bpy)₃²⁺ > Ru(NH₃)₆³⁺. The enhancement of the voltammetric signals relative to the bare FTO electrode was strongly dependent on the probe type. The accumulation of the different redox probe is attributed to the due to the vertical orientation of the nanochannel favoring fast transport and diffusion unto the electrode surface. Further electrochemical characterization showed an interplay of the suface-controlled and diffusion-controlled process, wherein adsorbed species is more prominent in diluted media. Results showed that changing the debye length and electrokinetic radius of the silica nanochannel due to the ionic strength or nanochannel diameter also affects the transport and electrochemical detection of the paraquat analyte. Mesoporous silica films having different pore size, prepared using different alkyl ammonium bromide as template, yield different sensitivities, which could be due to the difference in electrochemical charge of the silica surface, as well as the distribution of ions in the nanochannel. Finally, an attempt to modify the surface of silica wall using zirconia was also made to study the transport of cations, which could pave a way for an improved stability of the mesoporous film.
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https://hal.univ-lorraine.fr/tel-03356710
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Submitted on : Tuesday, September 28, 2021 - 12:26:00 PM
Last modification on : Sunday, June 26, 2022 - 3:13:59 AM

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  • HAL Id : tel-03356710, version 1

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Deomila Basnig. Preparation of Silica Thin Films for Analytical Chemistry Applications. Chemical Sciences. Université de Lorraine, 2021. English. ⟨NNT : 2021LORR0102⟩. ⟨tel-03356710⟩

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