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A versatile nanoreactor for complementary in situ X-ray and electron microscopy studies in catalysis and materials science

Fam, Yakub ; Sheppard, Thomas L. ; Becher, Johannes ; Scherhaufer, Dennis ; Lambach, Heinz ; Kulkarni, Satishkumar ; Keller, Thomas F. ; Wittstock, Arne ; Wittwer, Felix and Seyrich, Martin , et al. (2019) In Journal of Synchrotron Radiation 26. p.1769-1781
Abstract

Two in situ 'nanoreactors' for high-resolution imaging of catalysts have been designed and applied at the hard X-ray nanoprobe endstation at beamline P06 of the PETRA III synchrotron radiation source. The reactors house samples supported on commercial MEMS chips, and were applied for complementary hard X-ray ptychography (23 nm spatial resolution) and transmission electron microscopy, with additional X-ray fluorescence measurements. The reactors allow pressures of 100 kPa and temperatures of up to 1573 K, offering a wide range of conditions relevant for catalysis. Ptychographic tomography was demonstrated at limited tilting angles of at least ±35° within the reactors and ±65° on the naked sample holders. Two case studies were selected... (More)

Two in situ 'nanoreactors' for high-resolution imaging of catalysts have been designed and applied at the hard X-ray nanoprobe endstation at beamline P06 of the PETRA III synchrotron radiation source. The reactors house samples supported on commercial MEMS chips, and were applied for complementary hard X-ray ptychography (23 nm spatial resolution) and transmission electron microscopy, with additional X-ray fluorescence measurements. The reactors allow pressures of 100 kPa and temperatures of up to 1573 K, offering a wide range of conditions relevant for catalysis. Ptychographic tomography was demonstrated at limited tilting angles of at least ±35° within the reactors and ±65° on the naked sample holders. Two case studies were selected to demonstrate the functionality of the reactors: (i) annealing of hierarchical nanoporous gold up to 923 K under inert He environment and (ii) acquisition of a ptychographic projection series at ±35° of a hierarchically structured macroporous zeolite sample under ambient conditions. The reactors are shown to be a flexible and modular platform for in situ studies in catalysis and materials science which may be adapted for a range of sample and experiment types, opening new characterization pathways in correlative multimodal in situ analysis of functional materials at work. The cells will presently be made available for all interested users of beamline P06 at PETRA III.

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publishing date
type
Contribution to journal
publication status
published
keywords
catalysis, electron microscopy, hard X-ray ptychography, nanoreactors, porous, X-ray microscopy
in
Journal of Synchrotron Radiation
volume
26
pages
13 pages
publisher
International Union of Crystallography
external identifiers
  • scopus:85071778567
  • pmid:31490169
ISSN
0909-0495
DOI
10.1107/S160057751900660X
language
English
LU publication?
no
id
95ca1cd9-02f2-46d6-ad93-93c67c872445
date added to LUP
2019-10-12 12:51:33
date last changed
2024-10-02 14:23:27
@article{95ca1cd9-02f2-46d6-ad93-93c67c872445,
  abstract     = {{<p>Two in situ 'nanoreactors' for high-resolution imaging of catalysts have been designed and applied at the hard X-ray nanoprobe endstation at beamline P06 of the PETRA III synchrotron radiation source. The reactors house samples supported on commercial MEMS chips, and were applied for complementary hard X-ray ptychography (23 nm spatial resolution) and transmission electron microscopy, with additional X-ray fluorescence measurements. The reactors allow pressures of 100 kPa and temperatures of up to 1573 K, offering a wide range of conditions relevant for catalysis. Ptychographic tomography was demonstrated at limited tilting angles of at least ±35° within the reactors and ±65° on the naked sample holders. Two case studies were selected to demonstrate the functionality of the reactors: (i) annealing of hierarchical nanoporous gold up to 923 K under inert He environment and (ii) acquisition of a ptychographic projection series at ±35° of a hierarchically structured macroporous zeolite sample under ambient conditions. The reactors are shown to be a flexible and modular platform for in situ studies in catalysis and materials science which may be adapted for a range of sample and experiment types, opening new characterization pathways in correlative multimodal in situ analysis of functional materials at work. The cells will presently be made available for all interested users of beamline P06 at PETRA III.</p>}},
  author       = {{Fam, Yakub and Sheppard, Thomas L. and Becher, Johannes and Scherhaufer, Dennis and Lambach, Heinz and Kulkarni, Satishkumar and Keller, Thomas F. and Wittstock, Arne and Wittwer, Felix and Seyrich, Martin and Brueckner, Dennis and Kahnt, Maik and Yang, Xiaogang and Schropp, Andreas and Stierle, Andreas and Schroer, Christian G. and Grunwaldt, Jan Dierk}},
  issn         = {{0909-0495}},
  keywords     = {{catalysis; electron microscopy; hard X-ray ptychography; nanoreactors; porous; X-ray microscopy}},
  language     = {{eng}},
  month        = {{09}},
  pages        = {{1769--1781}},
  publisher    = {{International Union of Crystallography}},
  series       = {{Journal of Synchrotron Radiation}},
  title        = {{A versatile nanoreactor for complementary in situ X-ray and electron microscopy studies in catalysis and materials science}},
  url          = {{http://dx.doi.org/10.1107/S160057751900660X}},
  doi          = {{10.1107/S160057751900660X}},
  volume       = {{26}},
  year         = {{2019}},
}