Journal
CHEMICAL COMMUNICATIONS
Volume 52, Issue 96, Pages 13865-13868Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c6cc08133a
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Funding
- Engineering and Physical Sciences Research Council (U.K.) [EP/P505216/1]
- Diamond Light Source Ltd
- European Union [FP7-NMP4-LA-2012-280983]
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We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi5Ti3Fe0.5Cr0.5O15 at 950 degrees C in molten Na2SO4 we observe the progression of numerous metastable phases. Using sequential multi-phase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.
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