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Synthesis and structural characterisation using Rietveld and pair distribution function analysis of layered mixed titanium-zirconium phosphates

DOI: 10.1016/j.jssc.2010.07.028 DOI Help

Authors: Victoria Burnell (University of Birmingham) , Jenny Readman (University of Birmingham) , Chiu Tang (Diamond Light Source) , Julia Parker (Diamond Light Source) , Stephen Thompson (Diamond Light Source) , Joe Hriljac (University of Birmingham)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Journal Of Solid State Chemistry , VOL 183 (9) , PAGES 2196-2204

State: Published (Approved)
Published: September 2010

Abstract: Crystalline metal (IV) phosphates with variable zirconium-to-titanium molar ratios of general formula (Ti1-xZrx)(HPO4)(2)center dot 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 alpha-titanium phosphate lattice and vice versa for titanium substitution into the a-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.

Journal Keywords: Layered phosphates; Titanium; Zirconium; Pair distribution function analysis; Solid solution

Subject Areas: Chemistry

Instruments: I11-High Resolution Powder Diffraction