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The multicomponent alloy HfNbTiVZr has been described as a single-phase high-entropy alloy (HEA) in the literature, although some authors have reported that additional phases can form during annealing. The thermal stability of this alloy has therefore been investigated with a combination of experimental annealing studies and thermodynamic calculations using the CALPHAD approach. The thermodynamic calculations show that a single-phase HEA is stable above about 830 °C. At lower temperatures, the most stable state is a phase mixture of bcc, hcp, and a cubic C15 Laves phase. Annealing experiments followed by quenching confirm the results from thermodynamic calculations with the exception of the Laves phase structure, which was identified as a hexagonal C14 type instead of the cubic C15 type. Limitations of the applied CALPHAD thermodynamic description of the system could be an explanation for this discrepancy. As-synthesized HfNbTiVZr alloys prepared by arc-melting form a single-phase bcc HEA at room temperature. In situ annealing studies of this alloy show that additional phases start to form above 600 °C. This indicates that the observed HEA is metastable at room temperature and stabilized by a slow kinetics during cooling. X-ray diffraction analyses using different cooling rates and annealing times show that the phase transformations in this HEA are slow and that completely different phase compositions can be obtained depending on the annealing procedure. In addition, it has been shown that the sample preparation method (mortar grinding, heat treatment, etc.) has a significant influence on the collected diffraction patterns and therefore on the phase identification and analysis.

In this study, we show that the phase formation of HfNbTiVZr high-entropy thin films is strongly influenced by the substrate temperature. Films deposited at room temperature exhibit an amorphous microstructure and are 6.5 GPa hard. With increasing substrate temperature (room temperature to 275 °C), a transition from an amorphous to a single-phased body-centred cubic (bcc) solid solution occurs, resulting in a hardness increase to 7.9 GPa. A higher deposition temperature (450 °C) leads to the formation of C14 or C15 Laves phase precipitates in the bcc matrix and a further enhancement of mechanical properties with a peak hardness value of 9.2 GPa. These results also show that thin films follow different phase formation pathways compared to HfNbTiVZr bulk alloys.

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