A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions
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 cha...
| Main Authors: | , , , , , , , |
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| Format: | Article |
| Language: | English |
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International Union of Crystallography
2022-03-01
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| Series: | Journal of Synchrotron Radiation |
| Subjects: | |
| Online Access: | http://scripts.iucr.org/cgi-bin/paper?S1600577521013576 |
| _version_ | 1830228194853126144 |
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| author | Julia E. Parker Miguel Gomez-Gonzalez Yolanda Van Lishout Husn Islam Desiree Duran Martin Dogan Ozkaya Paul D. Quinn Manfred E. Schuster |
| author_facet | Julia E. Parker Miguel Gomez-Gonzalez Yolanda Van Lishout Husn Islam Desiree Duran Martin Dogan Ozkaya Paul D. Quinn Manfred E. Schuster |
| author_sort | Julia E. Parker |
| collection | DOAJ |
| description | 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. |
| first_indexed | 2024-12-18T10:09:38Z |
| format | Article |
| id | doaj.art-ae8d7d29c30746a385c048c7130c2937 |
| institution | Directory Open Access Journal |
| issn | 1600-5775 |
| language | English |
| last_indexed | 2024-12-18T10:09:38Z |
| publishDate | 2022-03-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | Journal of Synchrotron Radiation |
| spelling | doaj.art-ae8d7d29c30746a385c048c7130c29372022-12-21T21:11:27ZengInternational Union of CrystallographyJournal of Synchrotron Radiation1600-57752022-03-0129243143810.1107/S1600577521013576ye5016A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditionsJulia E. Parker0Miguel Gomez-Gonzalez1Yolanda Van Lishout2Husn Islam3Desiree Duran Martin4Dogan Ozkaya5Paul D. Quinn6Manfred E. Schuster7Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE, United KingdomDiamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE, United KingdomJohnson Matthey Technology Centre, Johnson Matthey, Blounts Court, Sonning Common, Berkshire RG4 9NH, United KingdomJohnson Matthey Technology Centre, Johnson Matthey, Blounts Court, Sonning Common, Berkshire RG4 9NH, United KingdomJohnson Matthey Technology Centre, Johnson Matthey, Blounts Court, Sonning Common, Berkshire RG4 9NH, United KingdomJohnson Matthey Technology Centre, Johnson Matthey, Blounts Court, Sonning Common, Berkshire RG4 9NH, United KingdomDiamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE, United KingdomJohnson Matthey Technology Centre, Johnson Matthey, Blounts Court, Sonning Common, Berkshire RG4 9NH, United KingdomTo 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.http://scripts.iucr.org/cgi-bin/paper?S1600577521013576in situsample environmentsmulti-length scalesx-ray nanoprobestransmission electron microscopy (tem)synchrotronsmicro-electro-mechanical systems (mems) |
| spellingShingle | Julia E. Parker Miguel Gomez-Gonzalez Yolanda Van Lishout Husn Islam Desiree Duran Martin Dogan Ozkaya Paul D. Quinn Manfred E. Schuster A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions Journal of Synchrotron Radiation in situ sample environments multi-length scales x-ray nanoprobes transmission electron microscopy (tem) synchrotrons micro-electro-mechanical systems (mems) |
| title | A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions |
| title_full | A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions |
| title_fullStr | A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions |
| title_full_unstemmed | A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions |
| title_short | A cell design for correlative hard X-ray nanoprobe and electron microscopy studies of catalysts under in situ conditions |
| title_sort | cell design for correlative hard x ray nanoprobe and electron microscopy studies of catalysts under in situ conditions |
| topic | in situ sample environments multi-length scales x-ray nanoprobes transmission electron microscopy (tem) synchrotrons micro-electro-mechanical systems (mems) |
| url | http://scripts.iucr.org/cgi-bin/paper?S1600577521013576 |
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