Method of manufacturing pure titanium hydride powder and alloyed titanium hydride powders by combined hydrogen-magnesium reduction of metal halides

A method of manufacturing pure and alloyed titanium hydride powders by the combined hydrogen-magnesium reduction of metal halides, comprising:

• (a) filling a reaction retort with liquid metallic magnesium or with solid metallic magnesium and melting the solid magnesium, supplying hydrogen into the retort at 750-850° C., and dissolving the hydrogen into the liquid magnesium up to saturation,
• (b) supplying liquid titanium tetrachloride TiCl4 into the retort filled with liquid magnesium thereby producing titanium by reducing the titanium tetrachloride, and forming magnesium chloride as a byproduct,
• (c) introducing gaseous hydrogen and at least one component from the group consisting of titanium hydride powder, metal halides, individual metal powders, metal hydride powders other than titanium hydride powder, master alloy powders, or combinations thereof, together with liquid titanium tetrachloride TiCl4, in the form of a pulp into the retort, whereby the amount of any titanium hydride powder is in the range of 0.1-10 wt. % of the total amount of titanium product to be produced from the titanium tetrachloride for a single processing cycle,
• (d) dissociating any titanium hydride into titanium and hydrogen al 750-850° C., followed by forming hydrogen gas micro-bubbles, which bubble in both the liquid phases of magnesium and magnesium chloride, thereby increasing the rate of the reduction by increasing an effective surface area of reacting phases, destroying a magnesium chloride film on the surface of the molten magnesium, and generating a turbulent gas phase above the liquid in the retort,
• (e) dissolving hydrogen into the reduced titanium metal to the end of reduction reaction at 750-850° C., in an amount of 30-180 cm3 of hydrogen per 1 g of titanium and forming a block of spongc-likc titanium hydride, having a composition of TiHx, where x is in the range of 0.3-1,
• (f) vacuum separating the block of sponge-like titanium hydride at 1000-1050° C., homogenizing alloyed titanium hydride, and emitting additional hydrogen from the titanium hydride, thereby destroying closed pores of the block of sponge-like titanium hydride due to density differences of the titanium hydrides having varying hydrogen content, thereby effectively liberating and removing residual magnesium and magnesium chloride,
• (g) supplying additional cold hydrogen into the retort after the removal of a part of the magnesium and magnesium chloride, decreasing the temperature in the center of the retort to 600-640° C., thereby effecting a polymorphic transformation, additional hydrogenation of the block of sponge-like titanium hydride, and cooling of the retort from the outside,
• (h) at least partially crystallizing the metallic magnesium and magnesium chloride, resulting in additional stresses to the block of sponge-like titanium hydride, thereby resulting in at least a partial disintegration of the block of sponge-like titanium hydride, and providing for evaporation and the removal of magnesium and magnesium chloride during a subsequent step of vacuum separation,
• (i) raising the temperature of the block of sponge-like titanium hydride in the center of the retort to 1000-1050° C., by supplying hydrogen,
• (j) de-hydrogenating the block of sponge-like titanium hydride in a vacuum at 1000-1050° C., followed by hydrogenation at temperatures in the range of 600-640° C. to promote a destruction of the pores of the sponge-like titanium hydride due to changes in the lattice structures and bulk densities of the compositions formed in the sponge-like titanium hydride block due to phase transformation at different temperatures,
• (k) removing the magnesium chloride and the metallic magnesium from the block of sponge-like titanium hydride by vacuum separation,
• (l) cooling the block of sponge-like titanium hydride to room temperature and hydrogenating in a hydrogen atmosphere by purging hydrogen through the retort thereby increasing the brittleness of the block of sponge-like titanium hydride, while saving energy needed for disintegration of the block of sponge-like titanium hydride in the retort, and
• (m) mechanically disintegrating the block of sponge-like titanium hydride inside the retort after hydrogenation according to step (l), whereby the disintegration is carried out in an atmosphere selected from the group consisting of hydrogen, inert gas, and vacuum.