Effect of lattice defects and temperature transition rates on the deuteride (hydride) particle morphology and phase transformation thermal hysteresis in niobium

Small-angle neutron scattering (SANS) measurements have been performed to investigate deuteride particle morphology and the phase transformation temperature hysteresis in low-concentration Nb–D alloys. Deformation either by cold rolling and or by previous deuteride cycling induced a coarse deuteride particle distribution. This observation is attributed to a more heterogeneous precipitation process facilitated by the dislocation defects and/or dislocation substructure. Deuteride precipitation in the deformed samples was observed immediately upon crossing the incoherent solvus during temperature reduction, again consistent with dislocationaided nucleation. Deuteride dissolution was observed at the very onset of heating for the coldrolled material, an observation unique among the samples characterized here. This is attributed to the availability of elastic accommodation energy for deuteride particles embedded in the severely work-hardened host matrix. In other words, the elastic energy assists dissolution, consistent with a theoretical model developed by Puls (1984 Acta Metall. 32 1259–69). The effect of temperature reduction transition rates was also investigated. Rapid, direct cooling (at 2–3 K min−1) resulted in a much finer deuteride particle distribution—a factor of 200 increase in the particle number density and a factor of ten reduction in characteristic particle size compared to well annealed single crystal Nb. The thermal hysteresis was also affected by the temperature transition rates, with a significant reduction of the hysteresis for the slowest cooling rates. This implies that at least part of the recorded hysteresis in the well annealed material is dependent on the temperature transition rate.