A versatile nanoreactor for complementary in situ X-ray and electron microscopy studies in catalysis and materials science.
J Synchrotron Radiat
; 26(Pt 5): 1769-1781, 2019 Sep 01.
Article
in En
| MEDLINE
| ID: mdl-31490169
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 (23â
nm spatial resolution) and transmission electron microscopy, with additional X-ray fluorescence measurements. The reactors allow pressures of 100â
kPa and temperatures of up to 1573â
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 923â
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.
Key words
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Microscopy, Electron
/
Catalysis
/
Materials Science
Language:
En
Journal:
J Synchrotron Radiat
Journal subject:
RADIOLOGIA
Year:
2019
Type:
Article
Affiliation country:
Germany