Solid state synthesis and structural refinement of polycrystalline phases: Ca1−2xZr4M2xP6−2xO24 (MMo, x = 0.1 and 0.3)

The structure of molybdenum substituted Polycrystalline calcium zirconium phosphate (CZP) was determined on the basis of crystal data of solid solutions. It was found that up to ∼5.81 wt.% (∼1.74 mol%), molybdenum could be loaded into CZP formulations without significant changes of the three-dimensional framework structure. The crystal chemistry of Ca1−2xZr4M2xP6−2xO24 (MMo, x = 0.1 and 0.3) phases has been investigated using General Structure Analysis System (GSAS) programming. The Mo substituted CZP phases crystallize in the space group R-3 and Z = 6. Powder diffraction data have been subjected to Rietveld refinement to arrive at a satisfactory structural convergence of R-factors. The PO4 stretching and bending vibrations in the Infra red (IR) region have been assigned. Morphology and compositional analysis have been carried out by scanning electron microscopy (SEM) and Energy Dispersive X-ray Analysis (EDAX) of the specimens.