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In-situ Diffraction of Time-Resolved Processes: Application of Quantitative Phase Analysis to Large Data Sets

Daniel P. Riley 1Erich H. Kisi 2

1. The Univeristy of Melbourne (UNIMELB), Grattan Street, Melbourne 3052, Australia
2. The University of Newcastle, University Drive, Newcastle 2308, Australia

Abstract

With the development of high-flux neutron diffractometers (D20, ILL; GEM, ISIS; WOMBAT-HIPD, OPAL) has come the capability for investigating in-situ time-resolved processes. This technique may be applied to resolve either reversible (stroboscopic mode) or irreversible (e.g. chemical reactions) processes at time resolutions as low as 80ms (see Figure 1). Developments that have allowed for this research include the design of wide angular acceptance position sensitive detectors (PSDs), rapid data acquisition electronics, customisable reaction chambers, 3-dimensional visualisation programs (e.g. LAMP, ILL) and most importantly Quantitative Phase Analysis (QPA). A remaining challenge for this research is the application of QPA to large data sets; presently a time consuming and potentially inaccurate activity. To place this in perspective, it should be noted that typical in-situ investigations produce between 100 – 10000 sequential diffraction patterns, for which independent Rietveld refinements and QPA must be performed. Alternately, attempts at automating these analysis methods often result in inaccuracies in phase quantification at low concentrations and identification of low intensity diffraction features (e.g. superlattice reflections). It is the intended aim to present an overview of QPA as applied to large data sets; detailing limitations of this process and providing examples of relevant research. 

 

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Related papers

Presentation: Oral at 11th European Powder Diffraction Conference, Microsymposium 7, by Daniel P. Riley
See On-line Journal of 11th European Powder Diffraction Conference

Submitted: 2008-08-07 16:09
Revised:   2009-06-07 00:48