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A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions

DOI: 10.1107/S1600577521013576 DOI Help

Authors: Julia E. Parker (Diamond Light Source) , Miguel Gomez-Gonzalez (Diamond Light Source) , Yolanda Van Lishout (Johnson Matthey) , Husn Islam (Johnson Matthey) , Desiree Duran Martin (Johnson Matthey) , Dogan Ozkaya (Johnson Matthey) , Paul D. Quinn (Diamond Light Source) , Manfred E. Schuster (Johnson Matthey)
Co-authored by industrial partner: Yes

Type: Journal Paper
Journal: Journal Of Synchrotron Radiation , VOL 29

State: Published (Approved)
Published: March 2022
Diamond Proposal Number(s): 20036 , 22509

Open Access Open Access

Abstract: To improve the understanding of catalysts, and ultimately the ability to design better materials, it is crucial to study them during their catalytic active states. Using in situ or operando conditions allows insights into structure–property relationships, which might not be observable by ex situ characterization. Spatially resolved X-ray fluorescence, X-ray diffraction and X-ray absorption near-edge spectroscopy are powerful tools to determine structural and electronic properties, and the spatial resolutions now achievable at hard X-ray nanoprobe beamlines make them an ideal complement to high-resolution transmission electron microscopy studies in a multi-length-scale analysis approach. The development of a system to enable the use of a commercially available gas-cell chip assembly within an X-ray nanoprobe beamline is reported here. The novel in situ capability is demonstrated by an investigation of the redox behaviour of supported Pt nanoparticles on ceria under typical lean and rich diesel-exhaust conditions; however, the system has broader application to a wide range of solid–gas reactions. In addition the setup allows complimentary in situ transmission electron microscopy and X-ray nanoprobe studies under identical conditions, with the major advantage compared with other systems that the exact same cell can be used and easily transferred between instruments. This offers the exciting possibility of studying the same particles under identical conditions (gas flow, pressure, temperature) using multiple techniques.

Diamond Keywords: in situ; sample environments; multi-length scales; X-ray nanoprobes; transmission electron microscopy (TEM); synchrotrons; micro-electro-mechanical systems (MEMS)

Subject Areas: Chemistry, Technique Development

Instruments: I14-Hard X-ray Nanoprobe

Added On: 16/02/2022 10:12

Journal of Synchrotron Radiation - 2022 - Parker - A cell design for correlative hard X%E2%80%90ray nanoprobe and electron.pdf

Discipline Tags:

Physical Chemistry Technique Development - Chemistry Catalysis Chemistry

Technical Tags:

Diffraction Imaging Spectroscopy X-ray Fluorescence (XRF) X-ray Absorption Spectroscopy (XAS)