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An In Situ SEM-FIB-Based Method for Contrast Enhancement and Tomographic Reconstruction for Structural Quantification of Porous Carbon Electrodes

Published online by Cambridge University Press:  04 August 2014

Santhana K. Eswara-Moorthy ,
Prasanth Balasubramanian ,
Willem van Mierlo ,
Jörg Bernhard ,
Mario Marinaro ,
Margret Wohlfahrt-Mehrens ,
Ludwig Jörissen  and
Ute Kaiser
Santhana K. Eswara-Moorthy*
Affiliation:
Département Science et Analyse des Matériaux (UIS), Centre de Recherche Public – Gabriel Lippmann, 41, rue du Brill, L-4422 Belvaux, Luxembourg Central Facility of Electron Microscopy, Group of Electron Microscopy of Material Science, Universität Ulm, 89081 Ulm, Germany
Prasanth Balasubramanian
Affiliation:
Central Facility of Electron Microscopy, Group of Electron Microscopy of Material Science, Universität Ulm, 89081 Ulm, Germany
Willem van Mierlo
Affiliation:
Central Facility of Electron Microscopy, Group of Electron Microscopy of Material Science, Universität Ulm, 89081 Ulm, Germany
Jörg Bernhard
Affiliation:
Central Facility of Electron Microscopy, Group of Electron Microscopy of Material Science, Universität Ulm, 89081 Ulm, Germany
Mario Marinaro
Affiliation:
Zentrum für Sonnenenergie- und Wasserstoff-Forschung Baden-Württemberg, 89081 Ulm, Germany
Margret Wohlfahrt-Mehrens
Affiliation:
Zentrum für Sonnenenergie- und Wasserstoff-Forschung Baden-Württemberg, 89081 Ulm, Germany
Ludwig Jörissen
Affiliation:
Zentrum für Sonnenenergie- und Wasserstoff-Forschung Baden-Württemberg, 89081 Ulm, Germany
Ute Kaiser
Affiliation:
Central Facility of Electron Microscopy, Group of Electron Microscopy of Material Science, Universität Ulm, 89081 Ulm, Germany
*
*Corresponding author. eswara@lippmann.lu
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Abstract

A new in situ Scanning Electron Microscope-Focused Ion Beam-based method to study porous carbon electrodes involving Pt filling of pores from gaseous precursors has been demonstrated to show drastically improved image contrast between the carbon and porous phases when compared with the Si-resin vacuum-impregnation method. Whereas, the latter method offered up to 20% contrast, the new method offers remarkably higher contrast (42%), which enabled fast semi-automated demarcation of carbon boundaries and subsequent binarization of the images with very high fidelity. Tomographic reconstruction of the porous carbon electrode was then obtained from which several morphological parameters were quantified. The porosity was found to be 72±2%. The axial and radial tortuosites were 1.45±0.04 and 1.43±0.04, respectively. Pore size, which is defined to be the distance from the medial axis of the pore to the nearest solid boundary, was quantified. Average pore size determined from the pore size distribution was 90 nm and the corresponding 1 sigma ranges from 45 to 134 nm. Surface-to-volume ratio of the carbon phase was 46.5 µm−1. The ratio of total surface area to the total volume of electrode including pores (i.e., specific surface area) was 13 µm−1.

Keywords

porous carbon electrodePt fillingSEM-FIBtomographystructural quantification
Type
Instrumentation and Techniques Development
Information
Microscopy and Microanalysis , Volume 20 , Issue 5 , October 2014 , pp. 1576 - 1580
Copyright
© Microscopy Society of America 2014 

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