Adma Products, Inc.

Other

Advanced Materials Products, Inc.

Advance Material Products, Inc

Advance Materials Products, Inc.

Vladimir S Moxson

Volodymyr A Duz

Eugene Y Ivanov

Orest M Ivasishin

Andrey G Klevtsov

Dmitro G Savvakin

Mykhailo Matviychuk

Vladimir Duz

Francis H Froes

Vladislav V Telin

Oleksiy P Yatsenko

Anatoli E Andreev

Aleksandr I Cheprasov

Yury V Shuvalov

Victor A Drozdenko

Mykola M Gumenyak

Aleksandr E Shapiro

Anatoli M Petrunko

Alexander E Shapiro

Viktor D Sukhoplyuyev

Alexander Nikishin

Jury Shuvalov

Mihajlo D Sopka

Sergey A Kasparov

Disclosed herein is a process that includes:

Manufacture of near-net shape titanium alloy articles from metal powders by sintering with presence of atomic hydrogen

The present invention relates to design and manufacture of multilayer sintered membranes made from metals and inorganic compounds (ceramics, silicate, clay, zeolites, phosphates, etc.). The membranes are designated for separation of water. They comprise at least one layer having nanopores commensurable with the size of water molecules. The membranes comprise: (a) supporting metallic layer having pore size 1-500 microns, (b) metallic interlayer having pore size &#x3c;2 micron, (c) sublayer with local regular protrusions of the interlayer into the supporting layer to increase service life of the membrane, and (d) one nanoporous ceramic or metallic top layer having pore size in the range of 1-15 angstroms. The invented design and method allow the manufacture of cost-effective multilayer membranes containing nanoporous layer with controlled pore sizes in each layer and optimal morphology of pores that provides selective transport of molecules during filtration and separation of liquids.

Multilayer, micro- and nanoporous membranes with controlled pore sizes for water separation and method of manufacturing thereof

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 is suitable for the manufacture of flat or shaped titanium matrix composite articles having improved mechanical properties such as lightweight plates and sheets for aircraft and automotive applications, heat-sinking lightweight electronic substrates, bulletproof structures for vests, partition walls and doors, as well as for sporting goods such as helmets, golf clubs, sole plates, crown plates, etc. A fully-dense discontinuously-reinforced titanium matrix composite (TMMC) material comprises (a) a matrix of titanium or titanium alloy as a major component, (b) ceramic and/or intermetallic hard particles dispersed in the matrix in the amount of &#x2266;50 vol. %, and (c) complex carbide- and/or silicide particles at least partially soluble in the matrix at the sintering or forging temperatures such as TiCrC, TiSiC, CrC, TiAlC, TiAlC, AlC, AlSiC, AlSiC, AlSiC, VC, (Ti,V)C, VCrC, and VCrCdispersed in the matrix in the amount of &#x2266;20 vol. %. The invention can be used to produce near-full density near-net shape parts from titanium matrix composite materials with acceptable mechanical properties without a hot deformation.

Fully-dense discontinuously-reinforced titanium matrix composites and method for manufacturing the same

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

The invention relates to manufacture of titanium articles from sintered powders. The cost-effective initial powder: 10-50 wt % of titanium powder having &#x2266;500 microns in particle size manufactured from underseparated titanium sponge comprising &#x2266;2 wt % of chlorine and &#x2266;2 wt % of magnesium; 10-90 wt % of a mixture of two hydrogenated powders A and B containing different amount of hydrogen; 0-90 wt % of standard grade refined titanium powder, and/or 5-50 wt % of alloying metal powders. The method includes: mixing powders, compacting the blend to density at least 60% of the theoretical density, crushing titanium hydride powders into fine fragments at pressure of 400-960 MPa, chemical cleaning and refining titanium powders by heating to 300-900&#xb0; C. and holding for &#x2266;30 minutes, heating in vacuum at 1000-1350&#xb0; C., holding for &#x2266;30 minutes, and cooling.

Cost-effective titanium alloy powder compositions and method for manufacturing flat or shaped articles from these powders

The method is suitable for the manufacture of flat or shaped titanium aluminide articles and layered metal matrix composites such as lightweight plates and sheets for aircraft and automotive applications, thin cross-section vanes and blades, composite electrodes, heat-sinking lightweight electronic substrates, bulletproof structures for vests, partition walls and doors, as well as for sporting goods such as helmets, golf clubs, sole plates, crown plates, etc. The method includes the following steps: (a) forming a porous preform of the reactive powder alloy or a porous multi-layer composite preform consisting of reactive powder metals and alloys by consolidation using at least one method selected from low-temperature loose sintering in vacuum, high-temperature loose sintering in vacuum, low-pressure sintering in an inert gas, cold pressing, direct powder rolling, isostatic or die pressing, and other means of room temperature and warm temperature consolidation, and/or combination thereof, to provide the density not less than 25% from the theoretical density of said reactive alloy; (b) hot consolidating by hot pressing said preform, hot rolling, hot isostatic pressing, or hot extrusion to obtain the density of 98-100% from the theoretical density of said reactive alloy; (c) additional sintering and/or annealing at the temperature being at least 900&#xb0; C. to decrease the residual porosity, control the microstructure, and improve the mechanical properties, especially ductility and/or plasticity of the resulting metal sheets or layered composites. The hot pressing is carried out at the temperature ranging 950-1700&#xb0; C., preferably at 1250-1450&#xb0; C., and at pressure ranging 50-350 kg/cm. The HIP is carried out at the temperature ranging 1250-1350&#xb0; C. and at pressure ranging 15000-40000 psi. The layered composite preform is manufactured by individual loose sintering, one layer of the composite at a time, and assembling them in the desired order. The composite consists of layers of titanium and/or titanium hydride, Ti-6Al-4V alloy, &#x3b1;-titanium aluminide alloy, &#x3b2;-titanium aluminide alloy, and &#x3b3;-titanium aluminide alloy in any combinations.

Method for manufacturing fully dense metal sheets and layered composites from reactive alloy powders

The invention relates to manufacturing of fully dense strips, plates, sheets, and foils from titanium alloys, titanium metal matrix composites, titanium aluminides, and flat multilayer composites of said materials by direct powder rolling of blended powders followed by sintering. The resulting titanium alloy flat products have properties that meet or exceed the conventional ingot metallurgy alloys and are suitable for aerospace, automotive, sporting goods, and other applications. The process includes: (a) providing C.P. titanium matrix powder and at least one powder of alloying components, (b) mechanical activation by attrition of all alloying components, (c) blending titanium powder with attrited alloying powders obtained in step (b), (d) cold direct powder rolling in a mill with horizontally-positioned rolls with different diameters to achieve density of the rolled strip of 60&#xb1;20% of the theoretical value with subsequent densification by re-rolling green strip, (e) densification by cold re-rolling of the green strip, (f) multiple cold re-rolling, and (g) sintering.

Process of direct powder rolling of blended titanium alloys, titanium matrix composites, and titanium aluminides

(a) The metal matrix composite is suitable for the manufacture of flat or shaped titanium aluminide, zirconium aluminide, or niobium aluminide articles and layered metal composites having improved mechanical properties such as lightweight plates and sheets for aircraft and automotive applications, thin cross-section vanes and airfoils, heat-sinking lightweight electronic substrates, bulletproof structures for vests, partition walls and doors, as well as sporting goods such as helmets, golf clubs, sole plates, crown plates, etc. The composite material consists of a metal (e.g., Ti, Zr, or Nb-based alloy) matrix at least partially intercalated with a three-dimensional skeletal metal aluminide structure, whereby ductility of the matrix metal is higher than that of the metal aluminide skeleton. The method for manufacturing includes the following steps: (a) providing an aluminum skeleton structure having open porosity of 50-95 vol. %, (b) filling said skeleton structure with the powder of a reactive matrix metal, (c) compacting the aluminum skeleton/matrix powder composite preform by cold rolling, cold die pressing, cold isostatic pressing, and/or hot rolling, (d) consolidating the initial or compacted composite preform by sintering, hot pressing, hot rolling, hot isostatic pressing, and/or hot extrusion to provide, at least partially, a reaction between aluminum skeleton and matrix metal powder, and (e) diffusion annealing followed by any type of heat treatment needed to provide predetermined mechanical and surface properties of the resulting metal matrix composite. The combination of ductile matrix and metal aluminide skeletal structure results in significant improvement of mechanical properties of the composite material, especially hot strength. This high-strength aluminide-based material can also be used as a core component in multilayer metal matrix composites.

High-strength metal aluminide-containing matrix composites and methods of manufacture the same

The cost-effective titanium powder is manufactured by (a) magnesium-thermic reduction of titanium chlorides characterized by the formation of a hollow block of the reaction mass having an open cavity in the center of the block, (b) thermal-vacuum separation of the hollow block from excessive Mg and MgCl at 850-950&deg; C. and residual pressure of 10  mm Hg, (c) cooling of obtained titanium hollow block in a H -contained atmosphere at an excessive hydrogen pressure, (d) crushing the hydrogenated titanium block, (e) grinding the crushed titanium pieces into the powder combined with a hydro-metallurgical treatment of obtained titanium powder in a diluted aqueous solution of at least one chloride selected from magnesium chloride, sodium chloride, potassium chloride, or titanium chloride, and (f) drying and, optionally dehydrating the titanium powder ground to a predetermined particle size. The formation of the hollow block of the reaction mass with the open cavity in the center of the block is carried out by accelerating the reaction mass on the inside surface of the reactor. The hydro-metallurgical treatment of titanium powder is carried out in the solutions having the total content of chlorides of 0.5-10 wt. %, at the powder-to-solution weight ratio from 1:1 to 1:4. The cooling of the titanium hollow block in the hydrogen-contained atmosphere is carried out to the temperature of 550-450&deg; C. at the excessive hydrogen pressure of 0.2 bar or higher. The productivity of the innovative process is higher, the energy consumption is lessened more than double, the duration of the processing cycle is decreased by 3. The shorter time of high-temperature stages results in significant improvement of titanium powder quality because it prevents the oxidation and nitrogenation of the metal. The powder dispersion is increased caused by porous and poorly sintered structure of the reaction mass. Cooling the block in the presence of hydrogen also increases the powder quality and the yield of fine powder fractions during the hydro-metallurgical treatment.

Manufacture of cost-effective titanium powder from magnesium reduced sponge

The lightweight bulletproof metal matrix macrocomposites (MMMC) contain (a) 10-99 vol. % of permeable skeleton structure of titanium, titanium aluminide, Ti-based alloys, and/or mixtures thereof infiltrated with low-melting metal selected from Al, Mg, or their alloys, and (b) 1-90 vol. % of ceramic and/or metal inserts positioned within said skeleton, whereby a normal projection area of each of said inserts is equal to or larger than the cross-section area of a bullet or a projectile body. The MMMC are manufactured as flat or solid-shaped, double-layer, or multi-layer articles containing the same inserts or different inserts in each layer, whereby insert projections of each layer cover spaces between inserts of the underlying layer. The infiltrated metal contains 1-70 wt. % of Al and Mg in the balance, optionally, alloyed with Ti, Si, Zr, Nb, V, as well as with 0-3 wt. % of TiB , SiC, or Si N sub-micron powders, to promote infiltrating and wetting by Al-containing alloys. The manufacture includes (a) forming the permeable metal powder and inserts into the skeleton-structured preform by positioning inserts in the powder followed by loose sintering in vacuum to provide the average porosity of 20-70%, (b) heating and infiltrating the porous preform with molten infiltrating metal for 10-40 min at 450-750&deg; C., (c) hot isostatic pressing of the infiltrated composite, and (d) re-sintering or diffusion annealing.

Bulletproof lightweight metal matrix macrocomposites with controlled structure and manufacture the same

Lightweight metal matrix composites containing a skeleton structure of titanium, titanium aluminide, or Ti-based alloy are manufactured by low temperature infiltration with molten Mg-based alloy or Mg&mdash;Al alloy at 450-750&deg; C., with molten In, Pb, or Sn at 300-450&deg; C., or with molten Ag and Cu at 900-1100&deg; C. The skeleton structure with a density of 25-35% is produced by loose sintering of Ti or Ti-based alloy powders. A primary deformation of the Ti skeleton structure before the infiltration is carried out by cold or hot rolling or forging to obtain a porous flat or shaped preform with a porosity <50% and pores drawn out in one direction such as the direction of future rolling of the composite plate. A secondary deformation of the infiltrated preform is carried out by multistage cold, or especially hot rolling, to refine the microstructure of the infiltrated skeleton structure and transform it into the textured microstructure strengthened by intermetallic phases such as TiAl, Ti Al, and TiAl . Subsequent re-sintering or diffusion annealing form a fully dense final structure of the resulting material having improved mechanical properties. The molten Mg-based infiltrate is alloyed with Al, Si, Zr, Nb, and/or V with the addition of TiB , SiC, and Si N sub-micron particles as infiltration promoters. The molten Agcomer- or Cu-based infiltrate can be alloyed with elements depressing its melting point. The method allows for control of the microstructure of composite materials by changing parameters of deformation, infiltration, and heat treatment. The method is suitable for the manufacture of flat or shaped metal matrix composites having improved ductility, such as lightweight bulletproof plates and sheets for aircraft and automotive applications, composite electrodes, heat-sinking lightweight electronic substrates, sporting goods such as helmets, golf clubs, sole plates, crown plates, etc.

Manufacture of lightweight metal matrix composites with controlled structure

A method of producing Iron-Silicon high density sintered articles of intricate design comprising: (a) the blending of compressible iron or low-carbon steel powder, silicon alloyed iron or silicon powder, or combination of silicon alloyed iron and silicon powder, and lubricant, (b) cold pressing said blended mixture with pressures of less than 50 tsi to form the structure of said article with the density up to 88% of the theoretical value and with uniformly distributed hard powder consisting of silicon and/or silicon alloyed particles among ductile iron powder, (c) low temperature stress relieving heat treatment of said formed article at the temperature range of 360-800.degree. C. followed by a cooling rate of less than 120.degree. C./min that relieves compression stress in said iron or low carbon steel particles and provides partial bonding of these iron/steel particles inside said formed article but does not allow the substantial diffusion of silicon from hard powder consisting of silicon and/or silicon alloyed particles into ductile iron or steel particles, (d) impregnation or lubrication of said formed articles which provide hydrostatic pressure and radial plastic flow of the porous metal in a subsequent pressing operation, (e) densification of said formed article, stress relieved, and impregnated article by cold pressing to the density not less than 91% of the theoretical density using the same pressure as in the previous pressing stage, and finally (f) sintering the said formed article to obtain a density greater than 96% of the theoretical value at the elevated temperature up to 1420.degree. C. from 1250.degree. C.

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Hudson, OH, United States of America

Vladimir S Moxson