Zirconium Phase Transformation under Static High Pressure and ω-Zr Phase Stability at High Temperatures.

Abstract

High-purity Zr has been observed to undergo a phase transformation from the α-phase to the hexagonal ω-phase under high pressure generated either statically or by shock loading. The transition pressure from α-Zr to ω-Zr at 300 K is 2.10 GPa. The main aim of this research was to determine the conditions of α-Zr in ω-Zr transformation and the state of stresses after the high-pressure pressing and sintering of zirconium powders. Commercially acquired zirconium powders of 99.9% and 98.8% purity were used in this study. Qualitative and quantitative phase analysis of the materials was carried out using X-ray diffraction. The materials were statically pressed and sintered using a Bridgman-type toroidal apparatus at under 4.0 and 7.8 GPa. After pressing, the transformation proceeded for the zirconium powder containing 98.8% purity (with hydrides admixture) but did not occur for the high-purity zirconium powders with 99.9% purity. The zirconium powders were sintered using the HPHT (High Pressure—High Temperature) method at temperatures of 1273 K and 1473 K. The transformation proceeded for both powders. The highest contribution of the ω-Zr phase was obtained in the zirconium (98.8% purity with the hydrides contents) sintered for 1 min at a temperature of 1473 K and a pressure of 7.8. The ω-phase content was 87 wt.%. The stress measurement was performed for the pressed and sintered materials using the sin2ψ X-ray diffraction method. The higher sintering temperature resulted in a decrease of the residual stresses in the ω-Zr phase for the sintered zirconium. The higher levels of stress limited the transformation of the α-Zr phase into the ω-Zr phase. Investigated materials characterized by higher compressive macrostresses were also typical of the greater stability of the ω-Zr phase at high temperatures.