Phase Evolution and Deuterium Storage Properties of TiVNbZrCr High-Entropy Alloy: A Temperature-Resolved Synchrotron X-Ray Diffraction Study

TiVNbZrCr high-entropy intermetallic alloy was investigated as a deuterium storage material using gravimetric sorption measurements, thermogravimetric analysis, and temperature-resolved synchrotron X-ray diffraction during deuterium desorption. The as-prepared alloy had an experimentally determined composition of Ti17V19Zr19Nb22Cr23 and a density of 6.59 g·cm−3. Empirical alloy-design parameters indicate that the alloy is not a single-phase bcc solid solution, but rather a compositionally complex intermetallic alloy. The calculated hydrogen-affinity descriptors suggest a strong thermodynamic driving force for deuteride formation. Under 5 MPa D2, the alloy absorbed 3.28 wt.% D, corresponding to D/M = 1.1. After ex situ deuteration, additional diffraction reflections were indexed using tetragonal deuteride reference structures corresponding to ZrV2D2.35 and TiD2, while the Cr-rich bcc phase remained comparatively stable. Thermal desorption released 2.28 wt.% D up to 600 °C in three partially overlapping steps. These results demonstrate that deuterium storage in TiVNbZrCr is governed by phase-selective deuteride formation and decomposition rather than by homogeneous bcc lattice expansion.