CFM 2019

Digitizing porous gold electrodes using FIB-SEM analysis
Anthony Baux  1@  , Guillaume Couégnat  2@  , Olivier Caty  3@  , Didier Lasseux  4@  , Nicolas Mano  5@  , Alexander Kuhn  6@  , Gérard Vignoles  7@  
1 : Laboratoire des Composites Thermostructuraux  (LCTS)
Université Sciences et Technologies - Bordeaux 1, Commissariat à l'énergie atomique et aux énergies alternatives : DAMLe Ripault, Snecma-SAFRAN group, Centre National de la Recherche Scientifique : UMR5801
2 : Laboratoire des Composites ThermoStructuraux  (LCTS)  -  Site web
Safran Ceramics, CNRS : UMR5801
3 allée de la Boétie 33600 Pessac -  France
3 : Laboratoire des Composites Thermostructuraux  (LCTS)  -  Site web
CEA, CNRS : UMR5801, Université Sciences et Technologies - Bordeaux I, SAFRAN (FRANCE)
3 allée de la Boétie 33600 PESSAC -  France
4 : Institut de Mécanique et d'Ingénierie de Bordeaux  (I2M)  -  Site web
Institut polytechnique de Bordeaux, Arts et Métiers ParisTech, CNRS : UMR5295, Université Sciences et Technologies - Bordeaux I
Site Site ENSAM Esplanade des Arts et Métiers 33405 TALENCE -  France
5 : Centre de recherches Paul Pascal  (CRPP)  -  Site web
CNRS : UPR8641
115, Av Albert Schweitzer 33600 PESSAC -  France
6 : Institut des Sciences Moléculaires  (ISM)
Université Montesquieu - Bordeaux 4, Université Sciences et Technologies - Bordeaux 1, École Nationale Supérieure de Chimie et de Physique de Bordeaux (ENSCPB), Centre National de la Recherche Scientifique : UMR5255
Bâtiment A 12 351 cours de la Libération 33405 TALENCE CEDEX -  France
7 : Laboratoire des Composites Thermostructuraux  (LCTS)
CNRS : UMR5801, CEA, Université de Bordeaux (Bordeaux, France), SAFRAN (FRANCE)

This project is dedicated to a bottom-up approach to optimize the design of porous electrode materials devoted to biofuel cells and biosensors. These devices operate on the basis of complex enzymatic electrochemical redox reactions coupled to mass transfer of substrates (glucose and O2) and electron transfer within the pores of the structure and from/to the pore surfaces. The advantage of using porous materials for these devices lies in the very large internal surface area (where electron exchange takes place) to overall material volume ratio, yielding much larger current densities than on a bare solid electrode. Some very interesting techniques, based on templating silica beads on gold substrate with a Langmuir-Blodgett deposition [1] step followed by electroplating of gold [2] and beads dissolution have been elaborated to synthetize pure gold porous materials having a typical spherical pore size of the order of one micrometer. The objective of the project is to model the porous structure of the electrode. First, a determination of the geometrical characteristics can be achieved through image acquisition and analysis. The structure not only contains a gradient of hollow spherical pore radii, but also some degree of disorder due to local arrangement defects; the radii of the windows separating the pores is also locally variable. Since pore window dimensions are lying around 100 nm, Focused Ion Beam-Scanning Electron Microscopy (FIB-SEM [3]) has been performed to have a 3D reconstruction of the porous media (fig. 1). Segmentation and binarization of the images are made both manually and automatically using Fiji and Python software. More than 600 SEM (SE) images (25 nm between 2 images) allow having a 3D image of a part of the electrode (fig. 2). The shape of the connections between spheres, the distances between spheres and the sphere diameters have been analysed.


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