A process to produce niobium-50mass% titanium alloy powder is proposed and its applicability is examined experimentally. The oxide mixture (Nb2O5+TiO2) was exposed to the reductant calcium, which can be applied thermodynamically as either the liquid or the gaseous form. Ca gas was favorable for the contamination of impurity such as carbon. The anhydrated co-precipitation from the aqueous solution involving Nb5+ and Ti4+ formed the better uniformity in the obtained alloy powder. The addition of CaCl2 reduced the residual oxygen to the level of 0.15mass pct because the by-product CaO partially dissolved in the molten CaCl2.