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Synthesis and structural characterisation using Rietveld and pair distribution function analysis of layered mixed titanium-zirconium phosphates |
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| Authors: | Victoria A. Burnell Chiu C. Tang Stephen P. Thompson |
| Affiliation: | a School of Chemistry, The University of Birmingham, Edgbaston, Birmingham B15 2TT, UK b Diamond Light Source Ltd., Diamond House, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE, UK |
| Abstract: | Crystalline metal (IV) phosphates with variable zirconium-to-titanium molar ratios of general formula (Ti1−xZrx)(HPO4)2·H2O have been prepared by precipitation of soluble salts of the metals with phosphoric acid and heating the amorphous solids in 12 M H3PO4 in an autoclave. The new materials are structurally characterised by Rietveld analysis of synchrotron X-ray powder diffraction data and pair distribution function (PDF) analysis of high energy synchrotron X-ray total scattering data. A broad range of zirconium-titanium phosphate solid solutions were formed showing isomorphous substitution of titanium by zirconium in the α-titanium phosphate lattice and vice versa for titanium substitution into the α-zirconium phosphate lattice. In both cases the solubility is partial with the coexistence of two substituted phases observed in samples with nominal compositions between the solubility limits. |
| Keywords: | Layered phosphates Titanium Zirconium Pair distribution function analysis Solid solution |
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