A new process of magnesium thermal reduction was successfully attempted to produce Zr–Ti alloy powder. A gas mixture of ZrCl4+TiCl4 was injected to molten magnesium, and the chloride components were reduced by magnesium, leading to the formation of MgCl2. The Zr and Ti atoms that were not reacted with magnesium were condensed to particle forms inside liquid magnesium and magnesium chloride. In the next stage, the magnesium and its chloride were fully removed by 1–5%HCl solution at room temperature. The target compositions of Zr–Ti alloy powder could be obtained in the ranges of Zr–(0–20 wt-%)Ti by controlling the mole fraction of each ZrCl4 and TiCl4 gas. Its purity was achieved to ∼99·4%, and the average particle size was almost found to be in the level of several micrometres.