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High Throughput In Situ EXAFS Instrumentation for the Automatic Characterization of Materials and Catalysts

DOI: 10.1063/1.2436404 DOI Help

Authors: Nikolaos Tsapatsaris (University of Manchester) , A. M. Beesley (University of Manchester) , Norbert Weiher (University of Manchester) , Moniek Tromp (Southampton University) , John Evans (University of Southampton) , A. J. Dent (Diamond Light Source Ltd) , Ian Harvey (Daresbury Laboratory) , Sven L. M. Schroeder (The University of Manchester)
Co-authored by industrial partner: No

Type: Conference Paper
Conference: Ninth International Conference on Synchrotron Radiation Instrumentation
Peer Reviewed: No

State: Published (Approved)
Published: June 2006

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, ? 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 ??Al2O3, and for the evaluation and structural characterization of eight Au catalysts supported on Al2O3 and TiO2 Mass spectrometer traces reveal conversion rate oscillations in 6wt % Au/?Al2O3 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.

Journal Keywords: High Throughput; Combinatorial Chemistry; Xas; Catalysis; Au; Gamma Al(2) O(3); Sbs Standard

Subject Areas: Chemistry

Facility: Daresbury