In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays: High Resolution Imaging at Ambient Pressure and Elevated Temperature

A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin electro...

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Bibliographic Details
Published in:Microscopy and microanalysis 2016-02, Vol.22 (1), p.178-188
Main Authors: Baier, Sina, Damsgaard, Christian D., Scholz, Maria, Benzi, Federico, Rochet, Amélie, Hoppe, Robert, Scherer, Torsten, Shi, Junjie, Wittstock, Arne, Weinhausen, Britta, Wagner, Jakob B., Schroer, Christian G., Grunwaldt, Jan-Dierk
Format: Article
Language:English
Subjects:
Catalysis
Gold
Heating
High temperature
Hot Temperature
Hydrostatic Pressure
Materials Applications
Microscopy
Microscopy - instrumentation
Microscopy - methods
Oxidation
X-Ray Diffraction - instrumentation
X-Ray Diffraction - methods
X-rays
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Summary:A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin electron transparent window and allows heating. Two gold-based systems, 50 nm gold particles and nanoporous gold as a relevant catalyst sample, were used for studying the feasibility of the cell. Measurements showing a resolution around 40 nm have been achieved under a flow of synthetic air and during heating up to temperatures of 933 K. An elevated temperature exhibited little influence on image quality and resolution. With this study, the potential of in situ hard X-ray ptychography for investigating annealing processes of real catalyst samples is demonstrated. Furthermore, the possibility to use the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample.
ISSN:1431-9276
1435-8115
DOI:10.1017/S1431927615015573