Abstract
Rapid synthesis of Pb 5(VO 4) 3I, a potential immobilisation host for iodine radioisotopes, was achieved in an open container by microwave dielectric heating of a mixture of PbO, PbI 2, and V 2O 5 at a power of 800 W for 180 s (at 2.45 GHz). The resulting ceramic bodies exhibited a zoned microstructure, differentiated by inter-granular porosity and phase assemblage, as a consequence of the inverse temperature gradient characteristic of microwave dielectric heating. Liquid PbI 2 within the interior of microwave processed ceramics assisted formation of Pb 5(VO 4) 3I, and reduced inter-granular porosity. In contrast, the exterior of microwave processed ceramics comprised poorly sintered Pb 5(VO 4) 3I with the presence of minor reagent relics. Quantitative microanalysis, electron diffraction and Rietveld analysis, confirmed the synthesis of stoichiometric Pb 5(VO 4) 3I within precision. The crystal structure of Pb 5(VO 4) 3I was found to adopt space group P6 3/m with a = 10.4429(3) Å and c = 7.4865(2) Å.
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