Adma Products, Inc.

Other

Andrey G Klevtsov

Vladimir S Moxson

Volodymyr A Duz

Mykhailo Matviychuk

Sergey A Kasparov

Jury Shuvalov

Viktor D Sukhoplyuyev

Mihajlo D Sopka

Aleksandr I Cheprasov

Yury V Shuvalov

Alexander Nikishin

The invention relates to energy-saving manufacturing of purified hydrogenated titanium powders or alloying titanium hydride powders, by metallo-thermic reduction of titanium chlorides, including their hydrogenation, vacuum separation of titanium hydride sponge block from magnesium and magnesium chlorides, followed by crushing, grinding, and sintering of said block without need for any hydro-metallurgical treatment of the produced powders. Methods disclosed contain embodiments of processes for manufacturing high purity high-purity powders and their use in manufacturing near-net shape titanium and titanium-alloy articles by sintering titanium hydride and alloyed titanium hydride powders produced from combined hydrogen-magnesium reduction of titanium chlorides, halides and hydrides of other metals. Additional titanium hydride powder introduced with titanium tetrachloride beneficially affects the kinetics of magnesium-thermic reduction due to formation of additionally-emitted atomic hydrogen, which helps to reduce presence of oxides, and so cleans inter-particle interfaces of the product and enhances diffusion between all components of the powder mixture.

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

The invention relates to the manufacture of titanium hydride powder using continuous or semi-continuous process, and using titanium slag or synthetic rutile as raw materials, while hydrogen, titanium tetrachloride, titanium trichloride, titanium dichloride, and hydrogen chloride are participate as intermediate reaction products. The continuous comprises: (a) reduction of TiClto low titanium chlorides followed by cooling a mixture, (b) separating of residual TiClfrom solid low chlorides by heating the mixture in argon or vacuum up to 150&#xb0; C. followed by removing the titanium tetrachloride from the mixture, (c) dissociation of TiClto TiClat 450&#xb0; C. in vacuum followed by removal of gaseous titanium tetrachloride from the reaction zone, condensation to the liquid, and returning back into the reaction retort, (d) dissociation of TiClin vacuum at 750-850&#xb0; C. to manufacture fine powder of metallic titanium and titanium tetrachloride, whereby hydrogen heated up to 1000&#xb0; C. is used to accelerate this reaction, and (e) saturation of the fine titanium powder by hydrogen at 400-640&#xb0; C. to manufacture final product of titanium hydride powder which is free of oxygen or nitrogen. The semi-continuous process includes the Kroll's process as the very first step.

Continuous and semi-continuous process of manufacturing titanium hydride using titanium chlorides of different valency

The cost-effective hydrogenated, purified titanium powder is manufactured by the semi-continuous process including: (a) magnesium-thermic reduction of titanium chlorides at 830-880&#xb0; C. in the hydrogen atmosphere characterized by the formation of a hollow porous block of the reaction mass having an open cavity in the center of the block, (b) full thermal-vacuum separation of the hollow block from excessive Mg and MgClat 850-980&#xb0; C. and residual pressure of 26-266 Pa using a multi-step cycle including: (i) purging hydrogen at 800-950&#xb0; C. into the reactor at the pressure 10 kPa to 24.5 kPa, (ii) directive squeezing-out of a separated liquid phase containing magnesium and magnesium chloride into an additional vessel, and (iii) application of alternate pressure to small portions of the liquid phase in porous titanium compound from different sides which provides removal of the liquid from small pores of the titanium compound and fast evaporation of said liquid, (c) simultaneous hydrogenation and cooling of the titanium sponge down to 600&#xb0; C. by purging cold hydrogen using multiple recirculation of hydrogen, (d) holding the hydrogenated porous titanium compound in the hydrogen atmosphere at 450-600&#xb0; C. for 20-70 minutes, (e) removing the hydrogenated porous titanium compound from the reactor, and (f) crushing and grinding the crushed hydrogenated porous titanium pieces into the powder having a predetermined particle size.

Semi-continuous magnesium-hydrogen reduction process for manufacturing of hydrogenated, purified titanium powder

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Moscow, Russia

Andrey G Klevtsov