Due to TiAl alloys’ excellent properties, TiAl alloys have received widespread attention from researchers. However, the high energy consumption and lengthy process of traditional preparation methods have always limited the large-scale application of TiAl alloys. This article develops a new method for preparing TiAl-based alloy powder via the magnesium thermal reduction of TiO2 in AlCl3-KCl molten salt. In this study, the proportion of AlCl3&KCl molten salts was determined. We conducted phase analysis on the final product by studying the changes in temperature and time. It was found that the TiAl3 alloy powder could be obtained by being kept at 750 °C for 2 h, with an oxygen content of 3.91 wt%. The reaction process for the entire experiment was determined through thermodynamic calculations and experimental analysis, and the principles of the reduction process are discussed.
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