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High throughput in situ EXAFS instrumentation for the automatic characterization of materials and catalysts

High throughput in situ EXAFS instrumentation for the automatic characterization of materials and catalysts
High throughput in situ EXAFS instrumentation for the automatic characterization of materials and catalysts
An XAS data acquisition and control system for the in situ analysis of dynamic materials libraries under control of temperature and gaseous environment has been developed. It was integrated at the SRS in Daresbury, UK, beamline 9.3, using a Si (220) monochromator and a 13 element solid state Ge fluorescence detector. The core of the system is an intelligent X, Y, Z, θ positioning system coupled to multi-stream quadrupole mass spectrometry analysis (QMS). The system is modular and can be adapted to other synchrotron radiation beamlines. The entire software control was implemented using Labview and allows the scan of a variety of library sizes, in several positions, angles, gas compositions and temperatures with minimal operator intervention. The system was used for the automated characterization of a library of 91 catalyst precursors containing ternary combinations of Cu, Pt, and Au on γ-Al2O3, and for the evaluation and structural characterization of eight Au catalysts supported on A12O3 and TiO2. Mass spectrometer traces reveal conversion rate oscillations in 6wt % Au/γAl2O3 catalysts. The use of HT experimentation for in situ EXAFS studies demonstrates the feasibility and potential of HT in situ XAFS for synchrotron radiation studies.
high throughput, combinatorial chemistry, xas, catalysis, Au, ?-Al203, sbs standard
9780735403734
1739-1742
Tsapatsaris, Nikolaos
2f279771-c8da-4e97-9e7c-39c9988e9ee9
Beesley, A.M.
39f30de5-300a-4089-aac5-414578a5622a
Weiher, Norbert
b80730e2-01a5-40c2-9244-dbe44547e5f1
Tromp, Moniek
48c1ebbb-579c-42b6-83bb-7188c668b322
Evans, John
05890433-0155-49fe-a65d-38c90ea25c69
Dent, A.J.
b5cc5c9e-ae74-45f2-8ac1-685bbcc1f074
Harvey, Ian
c7d85326-0c7a-47b5-a50b-fd6bfebbe3cd
Schroeder, Sven L.M.
8e7ce7d1-2bfd-48fe-aff6-e79961d3444c
Tsapatsaris, Nikolaos
2f279771-c8da-4e97-9e7c-39c9988e9ee9
Beesley, A.M.
39f30de5-300a-4089-aac5-414578a5622a
Weiher, Norbert
b80730e2-01a5-40c2-9244-dbe44547e5f1
Tromp, Moniek
48c1ebbb-579c-42b6-83bb-7188c668b322
Evans, John
05890433-0155-49fe-a65d-38c90ea25c69
Dent, A.J.
b5cc5c9e-ae74-45f2-8ac1-685bbcc1f074
Harvey, Ian
c7d85326-0c7a-47b5-a50b-fd6bfebbe3cd
Schroeder, Sven L.M.
8e7ce7d1-2bfd-48fe-aff6-e79961d3444c

Tsapatsaris, Nikolaos, Beesley, A.M., Weiher, Norbert, Tromp, Moniek, Evans, John, Dent, A.J., Harvey, Ian and Schroeder, Sven L.M. (2007) High throughput in situ EXAFS instrumentation for the automatic characterization of materials and catalysts. AIP Conference Proceedings, 879 (1), 1739-1742. (doi:10.1063/1.2436404).

Record type: Article

Abstract

An XAS data acquisition and control system for the in situ analysis of dynamic materials libraries under control of temperature and gaseous environment has been developed. It was integrated at the SRS in Daresbury, UK, beamline 9.3, using a Si (220) monochromator and a 13 element solid state Ge fluorescence detector. The core of the system is an intelligent X, Y, Z, θ positioning system coupled to multi-stream quadrupole mass spectrometry analysis (QMS). The system is modular and can be adapted to other synchrotron radiation beamlines. The entire software control was implemented using Labview and allows the scan of a variety of library sizes, in several positions, angles, gas compositions and temperatures with minimal operator intervention. The system was used for the automated characterization of a library of 91 catalyst precursors containing ternary combinations of Cu, Pt, and Au on γ-Al2O3, and for the evaluation and structural characterization of eight Au catalysts supported on A12O3 and TiO2. Mass spectrometer traces reveal conversion rate oscillations in 6wt % Au/γAl2O3 catalysts. The use of HT experimentation for in situ EXAFS studies demonstrates the feasibility and potential of HT in situ XAFS for synchrotron radiation studies.

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More information

Published date: 19 January 2007
Additional Information: Print ISSN 0094-243X; Online ISSN 1551-7616
Venue - Dates: Synchrotron Radiation Instrumentation: Ninth International Conference on Synchrotron Radiation, 2006-05-28 - 2006-06-02
Keywords: high throughput, combinatorial chemistry, xas, catalysis, Au, ?-Al203, sbs standard

Identifiers

Local EPrints ID: 46745
URI: http://eprints.soton.ac.uk/id/eprint/46745
ISBN: 9780735403734
PURE UUID: f3b41144-c99a-443d-91dc-97714bb939fa

Catalogue record

Date deposited: 18 Jul 2007
Last modified: 25 Nov 2019 17:30

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