WO2013022531A1 - Fabrication d'articles en alliage de titane de forme extrêmement précise à partir de poudres métalliques par frittage en présence d'hydrogène atomique - Google Patents

Fabrication d'articles en alliage de titane de forme extrêmement précise à partir de poudres métalliques par frittage en présence d'hydrogène atomique Download PDF

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Publication number
WO2013022531A1
WO2013022531A1 PCT/US2012/045170 US2012045170W WO2013022531A1 WO 2013022531 A1 WO2013022531 A1 WO 2013022531A1 US 2012045170 W US2012045170 W US 2012045170W WO 2013022531 A1 WO2013022531 A1 WO 2013022531A1
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Prior art keywords
around
titanium
green compact
powder
hydrogen
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PCT/US2012/045170
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English (en)
Inventor
Vladimir S. MOXSON
Dmitro G. SAVVAKIN
Orest M. Ivasishin
Mykola G. GUMENYAK
Vladimir A. DUZ
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Advance Material Products, Inc.
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Publication of WO2013022531A1 publication Critical patent/WO2013022531A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment

Definitions

  • Titanium alloys are known to exhibit light weight, high resistance to oxidation or corrosion, and the highest specific strength (the strength-to-weight ratio) of all metals except beryllium.
  • Articles of titanium alloys have been produced by melting, forming, and machining processes, or by certain powder metallurgy techniques.
  • the first method is not cost effective (although it provides high levels of desired properties of titanium alloys).
  • the second method is cost effective but as previously implemented cannot completely realize all of the desirable advantages of titanium alloys.
  • the method described in U.S. Pat. No. 4,432,795 includes grinding particles of light metals to a median particle size of less than 20 ⁇ , mixing them with particles of titanium based alloys having a median particle size larger than 40 ⁇ , and compacting the mixture by molding and sintering at temperatures less than that of a formation of any liquid phase.
  • This method allows the manufacture of the alloy having a density close to the theoretical value.
  • the resulting alloy contaminated by oxygen, iron, and other impurities, also exhibits insufficient mechanical properties.
  • U.S. Pat. No. 4,838,935 discloses the use of titanium hydride together with titanium powder in the primary mixture before molding and sintering to form tungsten-titanium sputtering targets.
  • the molded article is heated in a hot-press vacuum chamber to a temperature sufficient for the dehydration of TiH 2 to remove gases. Then, the article is heated to a second temperature of 1350-1500°C while maintaining the pressure and vacuum.
  • This method cannot completely prevent the oxidation of highly-reactive titanium powders during the second heating, because hydrogen is permanently out-gassing from the working chamber. Also, the method does not provide sufficient cleaning of titanium powder that resulted in deviations of final products from AMS and ASTM specifications. In addition, this method is not suitable for powdered mixtures containing low-melting metal and phases.
  • a preliminary partial sintering of titanium and titanium hydride powders with at least one powdered additive of alloying metals is disclosed in U.S. Pat. No. 3,950,166 (the contents of which are incorporated herein by reference).
  • the "mother” alloy obtained in such a way is pulverized and remixed with at least one of powdered titanium or titanium hydride, and optionally with powdered metals such as Mo, V, Zr, and Al-V alloys to achieve the final composition of titanium alloy.
  • This mixture is molded in a predetermined shape and sintered at 1000-1500°C in a vacuum. While the preliminary sintering partially resolves one technical problem (how to improve uniform distribution of alloying components), the process generates another problem (oxidation of the 'mother' powder during pulverization).
  • the disclosed methods relate to embodiments of processes for the manufacture of near-net shape titanium articles from sintered powders containing commercially pure (CP.) titanium and/or hydrogenated titanium powders, and/or titanium alloys with all required alloying elements.
  • CP. commercially pure
  • the embodiments of the methods disclosed herein resolve many or all of the problems related to high impurities, insufficient strength, irregular porosity, insufficient density, and cost reductions that have been described above, and that have not been solved by prior processes.
  • the process includes:
  • the process includes:
  • the initial mixture of metal powders can additionally comprise a powder prepared from underseparated titanium sponge, or alloying metal powders selected from master alloy powders, or alloy mixture of elemental powders, or pre-alloyed titanium powders, or combinations of these.
  • the powder blend can comprise, in addition to CP. titanium powder, only the hydrogenated titanium powders containing different amount of hydrogen in the range of 0.2- 3.9 wt. %.
  • the powder blend may contain only the hydrogenated titanium powders, or may exclude the CP. titanium powder, as indicated in the embodiment described above.
  • formation of the beta-phase titanium and releasing of atomic hydrogen from the hydrogenated titanium powder is carried out by slow heating, i.e., heating the green compact to a temperature ranging from about 250°C to about 600°C in an atmosphere of emitted hydrogen at the heating rate less than or equal to around 15°C/min to enhance the chemical reduction and cleaning effect of the emitted hydrogen and to release reaction water from titanium hydride and hydrogenated titanium powders.
  • consolidating of the powder blend can result from compaction, or from loose sintering.
  • Loose sintering can be used without use of room temperature consolidation.
  • a 40% to 90% dense sintered pre-form is further processed by high temperature deformation (forging, rolling, extrusion, etc.) to reach the required full theoretical density, which can be followed by the appropriate annealing or other stress relief operations.
  • Cleaning of titanium particles by emitted atomic hydrogen is facilitated in the loose-sintered green compact due to the developed porosity of the material.
  • the dehydrogenation taking place during sintering operations may be disrupted at a temperature above around 800°C before the completion of hydrogen evacuation in order to reserve residual hydrogen, which can be useful or necessary for reducing the deformation forces, grain refinements, and/or other positive effects such as additional cleaning of sintered titanium article during subsequent hot processing by forging, rolling, HIP, and/or extrusion.
  • the embodiments disclosed herein are particularly useful when forming parts having complex shapes, in particular when forming shapes with variations in their thickness that are being compacted in the thickness direction, and when the difference in green densities are very pronounced and cannot be avoided, because the use of hydrogenated titanium powders allows the disclosed process to reach near full density during sintering, which is impossible to achieve when non hydrogenated titanium powder is used.
  • the hydrogenated titanium powders are present in an amount of 10-90 wt. % of the powder blend, while other titanium powders (CP. titanium powder, underseparated titanium powder, etc.) is present in an amount of 5-20 wt. % of the powder blend. These titanium powders may be also hydrogenated prior to the blending operation.
  • the resulting sintered near-net shape titanium article desirably contains less than 0.2 wt. % of oxygen, less than 0.006 wt. % of hydrogen, less than 0.05 wt. % of chlorine, less than 0.05 wt. % of magnesium, less than 10 ppm of sodium, and desirably has a final porosity less than 1.5% at pore sizes less than 20 microns.
  • This low interstitial content achieved by our process makes the resulting titanium and titanium alloys weldable, which was not achievable by prior art.
  • initial heating is desirably performed at a slow rate, e.g., at a rate of less than or equal to 15°C/min.
  • the embodiments described herein are desirable because they can provide a method to manufacture near-net shape sintered titanium articles in a cost-effective way as a result of performing all process operations within one thermal cycle for one furnace run. This is, at least in part, the result of control of the purity and mechanical properties of sintered titanium alloys using (a) particularly desirable thermal processing of titanium, and hydrogenated titanium powders and control of atomic hydrogen emitted from the hydrogenated powders during heating in vacuum, (b) control of open porosity and hydrogen cleaning of titanium and titanium alloy particles at different steps of the thermal cycle during the sintering process, and (c) control of alpha-beta transformation of titanium in conjunction with porosity, cleaning, and densification of green compact depending on the presence, pressure, and activity of emitted hydrogen in the furnace chamber during the heating and sintering.
  • the terms “around” or “about” in connection with a numerical value denote a deviation from the numerical value of +/- 5%.
  • the term “hydrogenated titanium powders” includes titanium powders having hydrogen contents ranging from about 0.2 to about 3.9 wt %. This includes hydrogenated titanium particles nominally described as “titanium hydride” or “TiH 2 powder”, as well as other hydrogenated titanium particles having hydrogen contents within the indicated range, and combinations thereof, unless otherwise indicated.
  • this terminology can include hydrogenated titanium powder containing hydrogen in an amount ranging from 0.2 wt % up to and including 3.4 wt %, as well as hydrogenated titanium powder containing hydrogen in an amount above 3.4 wt % and up to and including 3.9 wt %, the latter being sometimes denominated as "titanium hydride" or "TiH 2 powder.”
  • the methods disclosed herein relate generally to the manufacture of sintered titanium and titanium alloys using elemental metal powders and titanium hydride and/or hydrogenated titanium powders as raw materials. It has been found that the atomic hydrogen emitted from titanium hydride and hydrogenated titanium powders before formation of molecular hydrogen plays a very important role in chemical reduction and cleaning of the titanium particles with respect to oxygen and other impurities such as chlorine, magnesium, sodium, and in preventing oxidation during heating and sintering, as well.
  • one or more of the hydrogenated titanium powders used was compacted to a relatively low density in the green samples (3.06 g/cm 3 ) as compared to green samples prepared from titanium powder alone (3.47 g/cm 3 ).
  • the converse was true, and the C.P.-Ti samples produced using hydrogenated titanium powder had a higher density (4.43 g/cm.sup.3, i.e. 98.2%) than those sintered from Ti powder alone (4.37 g/cm 3 , 97.0%).
  • This result confirms the advantage of using hydrogenated titanium powders to form the powder blend with respect to achieving higher sintered density, as shown in FIG.
  • the emitted atomic hydrogen beneficially affects sintering kinetics, helps to reduce any oxides that are usually located on the surface of powder particles, and by doing so, is cleaning inter-particle interfaces and enhancing the diffusion between all components of the powder mixture.
  • a characteristic feature of the hydrogenated titanium powders used in the methods disclosed herein is the ability to undergo a dehydrogenation process, i.e. a process of hydrogen evolution from the material, and the resulting significant shrinkage during vacuum heating above 320°C.
  • the temperature interval of dehydrogenation and corresponding changes in the phase composition depend on the heating rate and the rate of hydrogen evacuation from the heating chamber.
  • Relatively slow heating e.g., a heating rate of less than or equal to 15°C/mm (preferably ⁇ 7°C/min.) led to a phase change represented by TiH 2 ⁇ beta ⁇ alpha and which is a consequence of phase transformations, and completion of dehydrogenation at a temperature of about 800°C.
  • the intensity of hydrogen evolution varied within the mentioned temperature range and was determined by diffusion rate of hydrogen in the phases towards the powder particle surface.
  • the most intensive dehydrogenation with evolution of a major portion of hydrogen from the material was observed within a temperature range of about 400°C to about 600°C, and is believed to be due to the formation of the .beta.-phase, in which hydrogen diffusivity is the fastest.
  • FIG. 3 schematically illustrates a competition between two processes involving oxide films on the powder surfaces—either to be reduced by hydrogen or to be dissolved through diffusion of oxygen into the powder interior volume.
  • the second feature of the hydrogen cleaning process occurring in the methods disclosed herein is transformation of open porosity to closed porosity. It has been found that this also happens at temperatures of around 700°C. After this, products of reacting hydrogen with surface impurities will be located inside of the titanium material, and either the reaction will stop due to excessive pressure in the closed pore, or the reaction products will dissolve themselves in titanium instead of reacting with hydrogen at the surface. This relates especially to magnesium and magnesium chloride impurities that should evaporate at the higher temperature of sintering.
  • H 2 0 that we observed within the interval of hydrogen emission illustrated by FIG. 4, which shows mass-spectrometry curves of H 2 0 and H 2 0 gas release upon heating of titanium metal powdered compacts (curve Ti) and compacts prepared from hydrogenated titanium powders (curve TiH 2 ).
  • FIG. 4 shows mass-spectrometry curves of H 2 0 and H 2 0 gas release upon heating of titanium metal powdered compacts (curve Ti) and compacts prepared from hydrogenated titanium powders (curve TiH 2 ).
  • a low-temperature H 2 0 peak is present for both the TiH 2 and Ti compacts and, without wishing to be bound by theory, is believed to be related to the atmospheric moisture absorbed on the powders.
  • another H 2 0 peak was observed in the curve for the TiH 2 compact above 400°C, but absent from the curve for the Ti compact.
  • the oxide scales at powder surfaces are effective barriers for diffusion, which can prevent or limit the sintering of compacted particles.
  • sintering becomes possible above ⁇ 700°C when dissolution of Ti0 2 scales occurs due to diffusion of oxygen atoms from the surface deep into the titanium.
  • hydrogenated titanium powders hydrogen leaving a particle reduces the surface oxide scales (at least partially) before their dissolution and diffusion into the titanium particle, thus promoting a mass transfer between particles and decreasing oxygen content in dehydrogenated titanium.
  • the powder blend can comprise only hydrogenated titanium powders having the hydrogen contents described above, i.e., that contain different amounts of hydrogen in the range of 0.2-3.9 wt. %, for example, a powder blend that comprises three hydrogenated titanium powders with 0.2 wt. % of hydrogen, 2.0 wt. % of hydrogen, and 3.8 wt. % of hydrogen, respectively.
  • a powder having the lowest content of hydrogen becomes pure titanium powder due to dehydrogenation at an early point of the sintering process.
  • the resulting sintered articles have high mechanical properties such as tensile strength, yield strength, and elongation meet or exceed the requirements of the above specifications as indicated in the examples.
  • a powder blend of three hydrogenated titanium powders containing different amount of hydrogen was used: (1) 25% of hydrogenated titanium powder containing 0.5 wt. % of hydrogen, particle size ⁇ 45 microns, (2) 25% of hydrogenated titanium powder containing 2 wt. % of hydrogen, particle size ⁇ 100 microns, and (3) 50% of titanium hydride TiH.sub.2 powder containing 3.8 wt. % of hydrogen, particle size ⁇ 120 microns. These powders were mixed together, and the obtained mixed powder was compacted at 720 MPa to a low density green compact of 3.05 g/cm 3 .
  • the green compact having the thickness 12 mm, was heated to 250°C at a slow heating rate of ⁇ 7°C/min and held at this temperature for 40 min to release absorbed water from the titanium powder. Then, heating was continued at the heating rate of ⁇ 22°C/min to a temperature in the range of 480-500°C in the atmosphere of emitted hydrogen, and held at this temperature for 30 min to form beta-phase titanium and to release reaction water from the hydrogenated titanium powders.
  • the titanium plate was hot rolled to the thickness of 8 mm, followed by vacuum annealing at 750°C for 1.5 hours.
  • the measured contents of impurities in the final product were the following: oxygen ⁇ 0.15 wt. %, hydrogen ⁇ 0.005 wt. %, chlorine ⁇ 0.001 wt. %, magnesium ⁇ 0.003 wt. %, sodium ⁇ 10 ppm.
  • Standard specimens for mechanical testing were cut and machined from the titanium plate, which has a refined microstructure. Mechanical properties of the manufactured titanium plate were found to be: ultimate tensile strength 552-571 MPa, yield strength 489-510 MPa, and 21-23% elongation.
  • a powder blend of two types of powders was used: (1) 20% of CP titanium powder, which does not contain hydrogen at all, particle size ⁇ 150 microns, and (2) 80% of titanium hydride TiH 2 powder containing 3.5 wt. % of hydrogen, particle size ⁇ 100 microns.
  • the green compact having the thickness 24 mm was heated to 230.degree. C. at a slow heating rate of ⁇ 7°C/min and held at this temperature for 80 min to release absorbed water from the powder. Then, heating was continued at the heating rate of ⁇ 22°C/min to 560-580°C in the atmosphere of emitted hydrogen and held at this temperature for 25 min to form beta-phase titanium and release reaction water from the powder.
  • the diffusion- controlled chemical homogenization was carried out by heating of green compact to 830°C with the rate of 7°C/min and holding at this temperature for 20 min that was resulted in densification of green compact to 4.41 g/cm 3 due to complete dehydrogenation and active shrinkage of compact containing both titanium and titanium hydride components.
  • the titanium plate was hot rolled to the thickness of 20 mm followed by vacuum annealing at 720°C for 3.5 hours.
  • a powder blend of three types of powders was used: (1) 70 wt. % of titanium hydride powder TiH 2 containing 3.8 wt. % of hydrogen and having particle size less than 120 ⁇ , (2) 20% wt. % of CP titanium powder, which does not contain hydrogen, particle size ⁇ 150 microns, and (3) 10 wt. % of the 60A1-40V master alloy powder having particle size ⁇ 65 ⁇ .
  • the green compact having the thickness 16 mm was heated to 250°C at a slow heating rate of ⁇ 7°C/min and held at this temperature for 50 min to release absorbed water from the powders. Then, heating was continued at a heating rate of ⁇ 20°C/min to 580-600°C in the atmosphere of emitted atomic hydrogen and held at this temperature for 30 min to form beta-phase titanium and release reaction water from the powder.
  • the diffusion- controlled chemical homogenization was carried out by heating of green compact to 850°C with the rate of 7°C/min and holding at this temperature for 30 min that was resulted in densification of green compact to 4.47 g/cm 3 due to complete dehydrogenation and active shrinkage of the compact containing both titanium and hydrogenated titanium components.
  • the titanium alloy Ti-6A1-4V plate was hot rolled to the thickness of 12 mm followed by vacuum annealing at 750°C for 3 hours.
  • Measured contents of impurities in the final product were the following: oxygen ⁇ 0.15 wt. %, hydrogen ⁇ 0.0055 wt. %, chlorine ⁇ 0.001 wt. %, magnesium ⁇ 0.004 wt. %, sodium ⁇ 10 ppm.
  • Standard specimens for mechanical testing were cut and machined from the titanium alloy plate, which has a refined microstructure.
  • Mechanical properties of the manufactured titanium plate were: ultimate tensile strength 979-1041 MPa, yield strength 889-910 MPa, and elongation at break 15-18%. Due to low content of contaminants, the resulting titanium alloy plate is weldable using both GTAW and GMAW arc welding technique.
  • a powder blend of two types of powders was used: (1) 20 wt. % of underseparated titanium powder containing 2.0% chlorine and 0.8% of magnesium and having particle size ⁇ 100 ⁇ , and (2) 80 wt. % of titanium hydride TiH 2 powder containing 3.9 wt. % of hydrogen, particle size ⁇ 100 microns.
  • the green compact having a thickness 20 mm was heated to 250°C at a slow heating rate of ⁇ 7°C/min and held at this temperature for 70 min to release absorbed water from titanium powder. Then, the net-shaped green compacts were exposed to a temperature of 350°C for 60 min during heating in vacuum furnace for evacuation of chlorine and magnesium from the material.
  • the diffusion-controlled chemical homogenization was carried out by heating of green compact to 800-820°C with a heating rate of 6-7°C/min and holding at this temperature for 30 min that was resulted in densification of green compact to 4.42 g/cm 3 due to complete dehydrogenation and active shrinkage of compact containing both titanium and hydrogenated titanium components.
  • the titanium plate was hot rolled to the thickness of 15 mm followed by vacuum annealing at 750°C for 3 hours.
  • Measured contents of impurities in the final product were the following: oxygen ⁇ 0.16 wt. %, hydrogen ⁇ 0.005 wt. %, chlorine ⁇ 0.0015 wt. %, magnesium ⁇ 0.0048 wt. %, sodium ⁇ 10 ppm.
  • a powder blend of three types of base powders were used: (1) Crushed hydrogenated titanium sponge TG- 110 grade of Zaporozhye Titanium & Magnesium Corp., Ukraine, (2) Titanium hydride TiH 2 powder produced by a new "Non-Kroll” process combining reduction and distillation (ADMA hydrogenated powder), and (3) CP titanium powder manufactured by dehydration of TiH 2 . All powders had particle size ⁇ 100 microns, at the average particle size of 40 microns. Titanium hydride powder contained 3.5% of hydrogen.
  • the green compact having the thickness 18 mm was heated to 250°C at a slow heating rate of ⁇ 7°C/min and held at this temperature for 60 min to release absorbed water from the powder. Then, heating was continued at the heating rate of ⁇ 17°C/min to 550-570°C in the atmosphere of emitted hydrogen and held at this temperature for 30 min to form beta-phase titanium and release reaction water from the powder.
  • the diffusion- controlled chemical homogenization was carried out by heating of green compact to 840°C with the rate of ⁇ 7°C/min and holding at this temperature for 30 min that resulted in densification of the green compact to 4.43 g/cm 3 due to complete dehydrogenation and active shrinkage of the compact containing both CP titanium powder and hydrogenated titanium component.
  • the titanium plate was hot rolled to the thickness of 12 mm followed by vacuum annealing at 750°C for 2 hours.
  • a powder blend of four types of powder was used: (1) 20 wt. % of underseparated titanium powder containing 2.0% chlorine and 0.8% of magnesium and having particle size ⁇ 100 ⁇ , (2) 20 wt. % of underseparated and hydrogenated titanium powder containing 2% of hydrogen, (3) 20 wt. % of CP. titanium powder, (4) 30 wt. % of titanium hydride TiH 2 powder containing 3.4% of hydrogen, particle size ⁇ 100 microns, and (5) 10 wt. % of the 60A1-40V master alloy powder having particle size ⁇ 65 ⁇ .
  • the green compact having a thickness of 20 mm was heated to 250°C at slow heating rate ⁇ 7°C/min and held at this temperature for 70 min to release absorbed water from the powder. Then, net-shaped green compacts were exposed at 350°C for 60 min during heating in vacuum furnace for evacuation of chlorine and magnesium from the material.
  • the titanium plate was hot rolled to the thickness of 15 mm followed by vacuum annealing at 750°C for 3 hours.
  • FIG. 1 is a graph showing the relationship between compaction pressure used to produce a green compact, and the relative density of the sintered articles prepared from Ti powder alone and from Ti powder combined with hydrogenated titanium powder according to an embodiment disclosed herein.
  • FIG. 2 is a graph showing the relationship between change in free energy and temperature for different hydrogen pressures during sintering according to an embodiment disclosed herein.
  • FIG. 3 is a schematic diagram illustrating two mechanisms for disappearance of oxide films on surfaces of particles of Ti metal and hydrogenated titanium.
  • FIG. 4 is a graph showing mass spectrometry curves that illustrate the relationship between released water, hydrogen emission, and temperature for processing according to embodiments disclosed herein.

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Abstract

L'invention porte sur un procédé comprenant : (a) la formation d'un mélange de poudres par mélange de poudres de titane, (b) la consolidation du mélange de poudres par compactage pour obtenir un comprimé cru, (c) le chauffage du comprimé cru, ce qui libère de cette manière l'eau absorbée de la poudre de titane, (d) la formation de titane en phase bêta et le dégagement d'hydrogène atomique du titane hydrogéné par chauffage du comprimé cru dans une atmosphère d'hydrogène émis par le titane hydrogéné, (e) la réduction d'oxydes de surface présent sur les particules de la poudre de titane avec l'hydrogène atomique dégagé par chauffage du comprimé cru, (f) l'homogénéisation chimique du comprimé cru régulée par la diffusion et la densification du comprimé cru par chauffage suivi d'un maintien à température, ce qui a pour résultat une déshydrogénation totale ou partielle pour former un comprimé purifié et affiné, (g) le chauffage sous vide du comprimé cru purifié et affiné, ce qui fritte de cette manière le titane pour former un comprimé fritté dense et (h) le refroidissement du comprimé fritté dense pour former un article fritté de forme extrêmement précise.
PCT/US2012/045170 2011-08-08 2012-07-01 Fabrication d'articles en alliage de titane de forme extrêmement précise à partir de poudres métalliques par frittage en présence d'hydrogène atomique WO2013022531A1 (fr)

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CN105458296A (zh) * 2015-11-24 2016-04-06 四川大学 多段式氢化脱氢炉及低氧含量钛粉的制备方法
US9816157B2 (en) 2011-04-26 2017-11-14 University Of Utah Research Foundation Powder metallurgy methods for the production of fine and ultrafine grain Ti and Ti alloys
US11008639B2 (en) 2015-09-16 2021-05-18 Baoshan Iron & Steel Co., Ltd. Powder metallurgy titanium alloys
CN112941366A (zh) * 2021-01-25 2021-06-11 北京科技大学 一种超细钛粉制备高性能粉末冶金钛及钛合金的方法

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CN112941366A (zh) * 2021-01-25 2021-06-11 北京科技大学 一种超细钛粉制备高性能粉末冶金钛及钛合金的方法

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