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

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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