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b s t r a c tDeuteride phases in the zirconium-deuterium system in the temperature range 25e286 C have been studied in-situ by high resolution neutron diffraction. The study primarily focused on observations of d/g transformation at 180 C, and the peritectoid reaction a þ d 4 g at 255 C in commercial grade Zr powder that was deuterated to a deuterium/Zr ratio of one to one. A detailed description of the zirconium deuteride preparation route by high temperature gas loading is also described. The lattice parameters of a-Zr, d-ZrD x and ε-ZrD x were determined by whole pattern crystal structure analysis, usingRietveld and Pawley refinements, and are in good agreement with values reported in the literature. The controversial g-hydride phase was observed both in-situ and ex-situ in deuterated Zr powder after a heat treatment at 286 C and slow cooling.