Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.
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, Bi5Ti3Fe0.5Cr0.5O15at 950 °C in molten Na2SO4we observe the progression of numerous metastable phases. Using sequential multiphase 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.
Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk.
Saul J
SJ
Moorhouse
Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk.
Yue
http://orcid.org/0000-0003-2874-8267
Y
Wu
Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk.
Hannah C
HC
Buckley
Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk.
Dermot
D
O'Hare