Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

Autor: Moorhouse SJ; Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk., Wu Y; Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk., Buckley HC; Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk., O'Hare D; Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford, OX1 3TA, UK. dermot.ohare@chem.ox.ac.uk.
Jazyk: angličtina
Zdroj: Chemical communications (Cambridge, England) [Chem Commun (Camb)] 2016 Nov 24; Vol. 52 (96), pp. 13865-13868.
DOI: 10.1039/c6cc08133a
Abstrakt: 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, Bi 5 Ti 3 Fe 0.5 Cr 0.5 O 15 at 950 °C in molten Na 2 SO 4 we 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.
Databáze: MEDLINE