Abstract: Alloys comprising titanium and aluminum, or titanium, aluminum and at least one of the metals M, wherein M is vanadium, zirconium, chromium, niobium, tantalum and/or iron, are facilely prepared by reducing an alkali metal fluotitanate, or coreducing admixture of an alkali metal fluotitanate and at least one halide of a metal M, with aluminum, in the presence of an alkali metal oxide reactive flux, either Na.sub.2 O and/or K.sub.2 O; next solubilizing with water the fluorine compounds of reduction/coreduction which are in admixture of reduction/coreduction with dispersion of the aforesaid metals in metallic state; separating said dispersion of metals in metallic state from said admixture of reduction/coreduction; and then alloying by melting and cooling said separated dispersion of metals in metallic state.