4.5 Article

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

Journal

MICROSCOPY AND MICROANALYSIS
Volume 22, Issue 1, Pages 178-188

Publisher

CAMBRIDGE UNIV PRESS
DOI: 10.1017/S1431927615015573

Keywords

ptychography; X-ray microscopy; in situ; heterogeneous catalysis; synchrotron radiation; annealing; nanoporous gold

Funding

  1. Stiftung der Deutschen Wirtschaft
  2. Alexander von Humboldt Foundation
  3. BMBF [05K10VK1/05K10OD1, 05K13VK2/05K13OD4]
  4. virtual institute In-situ Nano Imaging of Biological and Chemical Processes [VI-403]
  5. Helmholtz Research Program Science and Technology of Nanosystems (STN)
  6. Danish National Research Foundation's Center for Individual Nanoparticle Functionality [DNRF54]
  7. Danish Instrumentation Centre (DanScatt)

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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-chip (TM) 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.

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