WO2020009955A1 - Procédé et système de traitement de poudres métalliques, et articles produits à partir de celles-ci - Google Patents

Procédé et système de traitement de poudres métalliques, et articles produits à partir de celles-ci Download PDF

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Publication number
WO2020009955A1
WO2020009955A1 PCT/US2019/040053 US2019040053W WO2020009955A1 WO 2020009955 A1 WO2020009955 A1 WO 2020009955A1 US 2019040053 W US2019040053 W US 2019040053W WO 2020009955 A1 WO2020009955 A1 WO 2020009955A1
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Prior art keywords
particles
hydride
alloy
powder
plasma
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Ceased
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PCT/US2019/040053
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English (en)
Inventor
Mark Weaver
Justen SCHAEFER
Reshma P. THAKORE
Mikhail GERSHENZON
Deborah M. WILHELMY
Robert M. GASIOR
Jen C. Lin
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Howmet Aerospace Inc
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Arconic Inc
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Publication of WO2020009955A1 publication Critical patent/WO2020009955A1/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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/10—Pre-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • 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
    • B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
    • B22F12/70—Gas flow means
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the present disclosure relates to a method and a system for processing metal powders and to an article produced therefrom. In certain embodiments, the present disclosure relates to an additive manufacturing method and system.
  • the powder feedstocks have strict limits on properties like particle size (e.g average particle size,
  • the present disclosure provides a novel method for producing spheroidized metallic particles.
  • the method comprises passing powder comprising metal hydride particles through a plasma to spheroidize the particles and to also de-hydride metal hydride particles in the powder, providing spheroidized metallic particles.
  • the present disclosure provides a novel method for producing spheroidized metallic particles.
  • the method comprises passing powder comprising metal hydride particles having an irregular shape through a plasma to produce spheroidized metallic particles. More specifically, as the powder is passed through the plasma, a hydrogen content of at least a portion of the metal hydride particles is reduced and the metal hydride particles and any other particles present are spheroidized, providing spheroidized metallic particles.
  • the spheroidized metallic particles are substantially spherical.
  • the present disclosure provides novel spheroidized metallic particles.
  • the novel spheroidized metallic particles may be used as powder material in an additive manufacturing system or method to produce a part.
  • the present disclosure provides a method for producing an additively manufactured part.
  • the method comprises passing powder through a plasma to thereby spheroidize the powder and to de-hydride metal hydride particles in the powder, thereby providing spheroidized metallic particles. At least a portion of the spheroidized metallic particles are utilized as powder material in an additive manufacturing system or method to produce a part.
  • the present disclosure provides novel spheroidized metallic particles.
  • the method of manufacturing the spheroidized metallic particles comprises passing powder comprising metal hydride particles through a plasma to produce spheroidized metallic particles. Passing the powder through the plasma also frees hydrogen from (de-hydrides) metal hydride particles in the powder.
  • the spheroidized metallic particles may be used as powder material in an additive manufacturing system or method to produce a part.
  • FIG. l is a flow chart illustrating a non-limiting embodiment of a method to process powder according to the present disclosure
  • FIG. 2 is a schematic representation of a non-limiting embodiment of a system to process powder according to the present disclosure.
  • FIG. 3 presents photographs of non-limiting embodiments of experimental powder and experimental spheroidized metallic particles according to the present disclosure.
  • any numerical range recited herein includes all sub-ranges subsumed within the recited range.
  • a range of“1 to 10” includes all sub-ranges between (and including) the recited minimum value of 1 and the recited maximum value of 10, that is, having a minimum value equal to or greater than 1 and a maximum value equal to or less than 10.
  • Any maximum numerical limitation recited in this specification is intended to include all lower numerical limitations subsumed therein and any minimum numerical limitation recited in this specification is intended to include all higher numerical limitations subsumed therein. Accordingly, Applicant reserves the right to amend this specification, including the claims, to expressly recite any sub-range subsumed within the ranges expressly recited.
  • powder refers to a material comprising a plurality of particles. Powder may be used, for example, in a powder bed in an additive manufacturing system or process to produce a tailored alloy product via additive manufacturing.
  • “median particle size” refers to the diameter at which 50% of the volume of the particles have a smaller diameter than the given value (e.g Dso).
  • particle size was determined in accordance with ASTM standard B822.
  • substantially comprise means at least 50% by weight. In various embodiments, substantially comprise can be 50% to 100% by weight such as, for example, at least 60% by weight, at least 70% by weight, at least 80% by weight, at least 90% by weight, at least 95% by weight, or at least 99% by weight.
  • substantially free means no more than 1% by weight. In various embodiments, substantially free of can be 0 to 1% by weight such as, for example, less than 0.5% by weight, less than 0.1% by weight, less than 0.01% by weight, less than 0.001% by weight, or 0.
  • “substantially removed” means at least 50% by weight has been removed. In various embodiments,“substantially removed” can refer to removal of 50% to 100% by weight such as, for example, removal of at least 60% by weight, removal of at least 70% by weight, removal of at least 80% by weight, removal of at least 90% by weight, removal of at least 95% by weight, or removal of at least 99% by weight.
  • substantially spherical means a shape having a sphericity of at least 0.8, such as, for example, at least 0.85 or at least 0.92.
  • a metal or metal alloy source material e.g ., metal sponge, bar, etc.
  • the metal source material can be contacted with a gas containing hydrogen at an elevated temperature (e.g., 400°C to 700°C).
  • the resulting brittle metal hydride (i.e., a hydride of a metal or metal alloy) can be crushed to break the material into irregularly shaped metal hydride particles.
  • the irregularly shaped metal hydride particles are then de-hydrided to substantially remove hydrogen from the particles and increase ductility.
  • the metal hydride particles are heated at a temperature greater than 700°C.
  • the de-hydrided particles can then be milled to a desired particle size.
  • the milled material can be subjected to de-oxygenation, additional milling, and spheroidization to produce spheroidized metallic particles that can be
  • the process to produce spheroidized metallic particles having a low hydrogen content and that have a morphology generally suitable to flow in an additive manufacturing apparatus or system involves multiple energy-intensive steps such as heating and reducing pressure.
  • a method and system are provided that can reduce energy input requirements and increase the efficiency of producing spheroidized metallic particles having low or substantially no hydrogen content.
  • the de-hydriding process for freeing hydrogen from previously hydrided metals or metal alloys can be combined with spheroidization.
  • de-oxygenation can be combined with spheroidization/de-hydriding.
  • powder comprising metal hydride particles which may be generally irregularly shaped are passed through a plasma to thereby de-hydride metal hydride particles in the powder and to spheroidize the powder. This process results in spheroidized metallic particles, and the hydrogen content in the powder has been reduced.
  • a metal or metal alloy source material e.g, metal sponge, bar, etc.
  • the metal or metal alloy source material can comprise at least one of titanium, titanium alloy, aluminum, aluminum alloy, tantalum, tantalum alloy, niobium, niobium alloy, zirconium, zirconium alloy, hafnium, hafnium alloy, molybdenum, molybdenum alloy, vanadium, and vanadium alloy.
  • the metal source material can comprise at least one of titanium and a titanium alloy, for example, a titanium alloy comprising, in weight percentages based on total alloy weight, 87 to 91 titanium, 3.5 to 4.5 vanadium, 5.5 to 6.75 aluminum, and incidental impurities.
  • the metal source material can comprise Ti-6Al-4V alloy.
  • the metal source material can be hydrided to increase its hydrogen content and thereby convert the material to a metal hydride 102. This conversion embrittles the material.
  • a“metal hydride” refers to both a hydrided metal and a hydrided metal alloy.
  • the metal source material can be hydrided by heating the source material at an elevated temperature (e.g ., 400°C to 700°C) and exposing the heated material to a gas comprising hydrogen (i.e., a hydriding gas).
  • the resulting metal hydride can be or comprise titanium hydride, titanium alloy hydride, aluminum hydride, aluminum alloy hydride, tantalum hydride, tantalum alloy hydride, niobium hydride, niobium alloy hydride, zirconium hydride, zirconium alloy hydride, hafnium hydride, hafnium alloy hydride, molybdenum hydride, molybdenum alloy hydride, vanadium hydride, and vanadium alloy hydride.
  • the metal hydride comprises at least one of titanium hydride and titanium alloy hydride.
  • the metal hydride can comprise a titanium alloy hydride produced by hydriding a titanium alloy comprising, in weight percentages based on total alloy weight, 87 to 91 titanium, 3.5 to 4.5 vanadium, 5.5 to 6.75 aluminum, and incidental impurities.
  • the metal source material can be produced by hydriding a titanium alloy comprising Ti-6Al-4V alloy.
  • the metal hydride can comprise at least 2 weight % hydrogen, such as, for example, at least 4 weight % hydrogen or at least 5 weight % hydrogen.
  • the metal hydride can comprise a hydrogen content in a range of 2 weight % to 10 weight % hydrogen.
  • titanium hydride particles or titanium alloy hydride particles can comprise 4 weight % hydrogen.
  • niobium hydride particles or niobium alloy hydride particles can comprise 5 weight % hydrogen.
  • aluminum hydride particles or aluminum alloy hydride particles can comprise 10 weight % hydrogen.
  • the resulting metal hydride can be crushed to break up the material into smaller pieces (e.g., irregularly shaped metal hydride particles) 104.
  • Crushing can include various means of size reduction such as, for example, milling, grinding, pulverizing, and attriting.
  • the metal hydride particles can comprise a median particle size of less than 325 pm such as, for example, less than 300 pm, less than 275 pm, less than 250 pm, less than 225 pm, less than 200 pm, less than 175 pm, less than 150 pm, less than 125 pm, less than 100 pm, less than 90 pm, less than 70 pm.
  • the metal hydride particles can comprise a median particle size in a range of 5 pm to 100 pm, 10 pm to 100 pm, 105 pm to 180 pm, 20 pm to 50 pm, 10 pm to 50 pm, 60 pm to 90 pm, or 50 pm to 100 pm.
  • fractions of the crushed metal hydride having an undesirable particle size e.g ., too small, too large
  • the powder subjected to the succeeding steps can comprise or substantially comprise metal hydride particles.
  • the powder can consist of or consist essentially of metal hydride particles.
  • the powder comprises, substantially comprises, or consists essentially of particles have an irregular shape.
  • irregularly shaped powder may include at least one sharp edge having an acute exterior angle.
  • the metal hydride particles can be at least one of titanium hydride particles, titanium alloy hydride particles, aluminum hydride particles, aluminum alloy hydride particles, tantalum hydride particles, tantalum alloy hydride particles, niobium hydride particles, niobium alloy hydride particles, zirconium hydride particles, zirconium alloy hydride particles, hafnium hydride particles, hafnium alloy hydride particles, molybdenum hydride particles, molybdenum alloy hydride particles, vanadium hydride particles, and vanadium alloy hydride particles.
  • the metal hydride particles comprise at least one of titanium hydride particles and titanium alloy hydride particles.
  • the powder can comprise at least one additional material.
  • the powder can comprise non-hydride metallic particles, spheroidized metallic particles, a ceramic, or combinations of any of those materials.
  • the non-hydride metallic particles are metal or metal alloy particles that are substantially free of hydrogen.
  • the non-hydride metallic particles can comprise, for example, at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, tantalum particles, tantalum alloy particles, niobium particles, niobium alloy particles, zirconium particles, zirconium alloy particles, hafnium particles, hafnium alloy particles, molybdenum particles, molybdenum alloy particles, vanadium particles, and vanadium alloy particles, all of which are substantially free of hydrogen.
  • the non-hydride metallic particles can be produced from de-hydriding metal hydride particles, for example, or may be particles of material that was not previously subjected to a hydriding treatment.
  • the powder can comprise a blend of metal hydride particles and non-hydride metallic particles.
  • the powder is passed through a plasma to produce spheroidized metallic particles from the powder 106.
  • metal hydride particles within the powder that are subjected to the plasma can be de-hydrided and thus converted to non-hydride metallic particles.
  • the plasma treatment can both spheroidize and de-hydride metal hydride particles included in the powder.
  • particles within the powder have not been de-hydrided prior to passing the powder through the plasma.
  • powder is simultaneously de-hydrided and spheroidized in a single process while passing through the plasma, providing spheroidized metallic particles having a reduced ( e.g ., lowered or substantially no) hydrogen content as compared to the powder prior to passing the powder through the plasma.
  • the spheroidized metallic particles can be substantially spherical.
  • crushing the metal hydride to increase surface area thereof can enable a lower content of hydrogen and/or oxygen in the spheroidized metallic particles.
  • the spheroidized metallic particles can comprise less than 4 weight % hydrogen based on the total weight of the spheroidized metallic particles.
  • the hydrogen content of the spheroidized particles can be, for example, less than 2 weight %, less than 1 weight %, less than 0.1 weight %, or less than 0.01 weight %.
  • the spheroidized metallic particles can be substantially free of hydrogen.
  • passing the powder through the plasma can reduce a weight percentage hydrogen content of the powder by at least 30%, such as, for example, by at least 40%, by at least 50%, by at least 70%, or by at least 90%.
  • passing the powder through the plasma can reduce a weight percentage hydrogen content of the powder in a range of 40% to 90%, or 50% to 100%.
  • Passing the powder through the plasma also can reduce an oxygen content of the powder.
  • the spheroidized metallic particles can comprise less than 1 weight % oxygen or less than 0.5 weight % oxygen, based on the total weight of the spheroidized metallic particles.
  • the spheroidized metallic particles can be substantially free of oxygen.
  • passing the powder through the plasma can reduce a weight percentage oxygen content of the powder by at least 15%, such as, for example, by at least 30%, by at least 50%, by at least 70%, or by at least 90%.
  • passing the powder through the plasma can reduce a weight percentage oxygen content of the powder in a range of 40% to 90%, or 50% to 100%.
  • the spheroidized metallic particles can be passed through a plasma (e.g ., passed through the plasma a second time) 108, thereby reducing or further reducing a hydrogen content and/or an oxygen content in the spheroidized metallic particles.
  • the spheroidized metallic particles can be passed through a plasma a plurality of (i.e., two or more) times. The several passes through the plasma can reduce a weight percentage hydrogen content of the spheroidized metallic particles by at least 30%, such as, for example, by at least 40%, by at least 50%, by at least 70%, or by at least 90%.
  • the several passes through the plasma can reduce a weight percentage hydrogen content of the spheroidized metallic particles in a range of 40% to 90%, or 50% to 100%. In various embodiments, the several passes through the plasma can reduce a weight percentage oxygen content of the spheroidized metallic particles by at least 15%, such as, for example, by at least 30%, by at least 50%, by at least 70%, or by at least 90%. In some embodiments, the several passes through the plasma can reduce a weight percentage oxygen content of the spheroidized metallic particles in a range of 40% to 90%, or 50% to 100%. In various embodiments, the plurality of passes through the plasma can improve a spherical shape (e.g., sphericity) of the previously spheroidized metallic particles.
  • a spherical shape e.g., sphericity
  • Chamber 202 is provided with an inlet 204 and an outlet 206.
  • the inlet 204 is adapted to receive powder 208 and convey it into the chamber 202.
  • the inlet 204 also is adapted to receive an additional material such as, for example, a gas.
  • the chamber 202 is adapted to receive the powder 208 and convert the powder 208 to spheroidized metallic particles 210.
  • the chamber 202 can be configured to produce a plasma 212, and the powder 208 is brought into contact with the plasma 212 in the chamber 202.
  • the chamber 202 is adapted to operate with a pressure therein of at least atmospheric pressure (e.g, 1 atmosphere (atm) absolute).
  • the chamber 202 is adapted to operate with a pressure less than atmospheric pressure (e.g, less than 1 atm absolute) therein.
  • the spheroidization can reduce the number of faces, edges, and/or features otherwise out of round in the powder 208.
  • Spheroidized metallic particles 210 formed in the chamber 202 pass into outlet 206 and can be collected or, in certain embodiments of system 200, may be recycled by passing back into the chamber 202 where they are contacted by the plasma 212.
  • outlet 206 can be adapted to receive an additional material, such as, for example, an inert gas and/or one or more additional products of the reaction that occurs in the chamber 202.
  • the additional reaction product(s) can be, for example, hydrogen and/or water. Water may be produced in the chamber 202, for example, when hydrogen is freed from metal hydride particles in chamber 202 and reacts with oxygen from particles in the chamber 202 and/or present in the atmosphere provided in the chamber 202.
  • the plasma 212 also can facilitate removal of nitrides from powder 208.
  • the plasma 212 produced in chamber 202 can be generated by any of various means known in the art.
  • the plasma 212 can be any of a glow discharge plasma, a capacitive discharge plasma, a cascaded arc plasma, an inductively coupled plasma, a microwave plasma, a wave heated plasma, an arc discharge plasma, a corona discharge plasma, a dielectric barrier discharge plasma, and a piezoelectric direct discharge plasma.
  • the system 200 can be designed so that the plasma 212 is generated in one or more of various regions within the chamber 202.
  • the plasma 212 is generated so that powder introduced into chamber 202 contacts the plasma 212 in a manner that facilitates spheroidization and de-hydriding of the powder 208 to form the spheroidized metallic particles 210 with reduced ( e.g ., low or substantially no) hydrogen content.
  • the system 200 can be designed so that the plasma 212 is generated axially with respect to the flow of the powder 208 through the chamber 202.
  • the positioning of the plasma 212 within the chamber 202 also can be arranged to enhance the de-oxygenation effects of the plasma 212, so as to reduce oxygen content of powder introduced into chamber 202 along with reducing hydrogen content of and spheroidizing the particles.
  • the plasma 212 comprises inductively coupled plasma.
  • the plasma 212 comprises microwave plasma.
  • the plasma can be a thermal plasma or a non-thermal plasma.
  • the plasma 212 can comprise a temperature suitable to promote de-hydriding of the powder 208 and/or suitable to melt the powder 208 to promote spheroidization.
  • an electron temperature of the plasma 212 is at least 3,000 K (Kelvin) such as, for example, at least 4,000 K, at least 5,000 K, at least 6,000 K, at least 7,000 K, 4,000 K to 10,000 K, or 6,000 K to 10,000 K.
  • a gas feed line 214 can supply a gas to the chamber 202.
  • the gas feed line 214 can communicate with the inlet 204, which then feeds the gas into the chamber 202 along with the powder 208, or, alternatively, the gas feed line 214 can directly communicate with the chamber 202.
  • the plasma 212 can be produced from gas fed to the system 200 by the gas feed line 214.
  • the gas can comprise an inert gas.
  • the gas can comprises at least one of helium, argon, nitrogen, hydrogen, oxygen, carbon tetrachloride, and an alkane.
  • the gas is supplied to the chamber 202 with the powder 208 in the inlet 204.
  • the gas introduced into the chamber 202 comprises hydrogen.
  • the gas introduced into the chamber 202 can comprise 1% to 20% hydrogen by volume, such as, for example, 2% to 15% hydrogen by volume, 1% to 4% hydrogen by volume, or 8% to 12% hydrogen by volume.
  • the addition of hydrogen to the gas can facilitate the removal of oxygen from the powder 208 given that the oxygen can react with the hydrogen in the chamber 202.
  • the gas introduced into the chamber 202 can comprise at least one of oxygen, nitrogen, and an alkane.
  • the oxygen, nitrogen, and/or alkane can react with the powder and produce spheroidized metallic particles comprising at least one surface bound group of an oxide, a nitride, and a carbide.
  • the surface bound group can differ depending on the nature of the gas introduced into the chamber 202.
  • the inner portion below the surface of the spheroidized metallic particles can be substantially free of the surface bound group.
  • the surface bound group can be used to indicate that the spheroidized metallic particles were created by the process according to the present disclosure.
  • the surface bound group on the spheroidized metallic particles can be identified by x-ray photoelectron spectroscopy, auger electron spectroscopy, or other suitable identification technique.
  • the identification of the surface bound group can indicate that the spheroidized metallic particles were created by the process according to the present disclosure.
  • the surface bound group can form a shell around the spheroidized metallic particles and the thickness of the shell can be used to indicate the spheroidized metallic particles were created by the process according to the present disclosure.
  • a recycle line 216 can be in fluid communication with the outlet 210 and adapted to receive the spheroidized metallic particles 210.
  • the recycle line 216 can be suitable to output at least a portion of the spheroidized metallic particles 210 into the inlet 208, in which they are then conveyed into the chamber 202 to pass through the plasma 212.
  • the spheroidized metallic particles 210 can be recycled into the chamber 202 through recycle line 216 as many times as necessary to remove the desired levels of hydrogen and/or oxygen from the spheroidized metallic particles 210.
  • the spheroidized metallic particles produced according to the present disclosure can be used to produce a part.
  • the spheroidized metallic particles can be used as powder material in a powder metallurgy system and/or process such as, for example, an additive manufacturing system and/or process.
  • the part produced by the system and/or process can comprise, for example, at least one of an aerospace component, an automotive component, an industrial component, a consumer product, and a building component.
  • additive manufacturing refers to a process of joining materials to make objects from three dimensional model data, usually layer upon layer, as opposed to subtractive manufacturing methodologies, as defined in ASTM F2792-l2a entitled“Standard Terminology for Additively Manufacturing Technologies”.
  • additive manufacturing processes useful in producing products from metallic feedstock include, for instance, DMLS (direct metal laser sintering), SLM (selective laser melting), SLS (selective laser sintering), and EBM (electron beam melting), among others.
  • Any suitable feedstock may be used, including a powder, a wire, and combinations thereof.
  • the additive manufacturing feedstock is comprised of powder.
  • Irregularly shaped metal hydride particles were produced by hydriding Ti-6Al-4V alloy source material and crushing the metal hydride.
  • the irregularly shaped metal hydride particles were passed through a plasma in a commercially available powder spheroidization system and were simultaneously de-hydrided and spheroidized to produce experimental spheroidized metallic particles utilizing suitable operating parameters.
  • the commercially available system used was the TEKSPHERO 15 plasma powder spheroidization system, available form Tekna, Sherbrooke, Quebec.
  • the irregularly shaped metal hydride particles were passed through the spheroidization system once to produce experimental spheroidized metallic particles.
  • the metal hydride particles were not subjected to a de-hydriding treatment prior to passage through the powder spheroidization system.
  • the compositions of the irregularly shaped metal hydride particles and the spheroidized metallic particles produced by passage once through the plasma in the powder spheroidization system are provided in Table 1.
  • the oxygen content of the particles was measured according to ASTM E1408.
  • the hydrogen content of the particles was measured according to ASTM El 447 with a sample size adjustment.
  • the aluminum, vanadium, and titanium contents of the particles was measured according to ASTM E-2371.
  • the hydrogen and oxygen contents of the experimental spheroidized metallic particles could be further reduced by subjecting the particles to one or more additional passes through the plasma (e.g ., recycling the particles through the spheroidization system).
  • recycling the spheroidized metallic powder through the plasma powder spheroidization system in the present example may reduce the hydrogen content of the spheroidized metallic particles to less than 2.0 weight %, and may reduce the oxygen content of the spheroidized metallic particles to less than 1.0 weight %.
  • FIG. 3 provides scanning electron microscope images of the metal hydride particles 302 and the experimental spheroidized particles 304 of the present example.
  • the metal hydride particles 302 produced by hydriding the Ti-6Al-4V alloy and crushing the hydride generally had an irregular, angular shape.
  • the particles 304 were generally substantially spherical in shape.
  • the spheroidization process also reduced both the hydrogen and oxygen contents of the irregularly shaped metal hydride particles comprising Ti-6Al-4V alloy.
  • the plasma process can convert metal hydride particles into spheroidized metallic particles having a morphology and chemistry suitable for use as powder material for further applications such as, for example, additive manufacturing.
  • the products produced by these methods have commercial end- uses in industrial applications, consumer applications (e.g. consumer electronics and/or appliances) or other areas.
  • consumer applications e.g. consumer electronics and/or appliances
  • the components or resulting products can be utilized in the aerospace field, automotive field, transportation field, building and construction field, in a variety of forms: fasteners, sheet, plate, castings, forgings, extrusions, post processed additive manufacturing forms, among others, including various applications (e.g. structural applications and components like beams, frames, rails, brackets, bulkheads, spars, ribs, among others.
  • a method comprising: passing a powder comprising metal hydride particles through a plasma to thereby de-hydride the metal hydride particles and spheroidize the powder to provide spheroidized metallic particles.
  • the method of clause 1 further comprising crushing a metal hydride to provide the metal hydride particles.
  • the method of clause 2 wherein the metal hydride particles comprise a median particle size less than 200 microns after crushing.
  • the method of clause 1-3, wherein the spheroidized metallic particles are
  • the metal hydride particles comprise at least one of titanium hydride particles, titanium alloy hydride particles, aluminum hydride particles, aluminum alloy hydride particles, tantalum hydride particles, tantalum alloy hydride particles, niobium hydride particles, niobium alloy hydride particles, zirconium hydride particles, zirconium alloy hydride particles, hafnium hydride particles, hafnium alloy hydride particles, molybdenum hydride particles,
  • the plasma comprises an inductively coupled plasma.
  • the plasma is produced from a gas comprising at least one of helium, argon, nitrogen, hydrogen, oxygen, carbon tetrachloride, and an alkane.
  • the spheroidized metallic particles comprises at least one surface bound group of an oxide, a nitride, and a carbide.
  • the method of clause 1-16 further comprising passing at least a portion of the spheroidized metallic particles through a plasma, thereby reducing a hydrogen content and an oxygen content in the spheroidized metallic particles.
  • the method of clause 1-19 further comprising passing at least a portion of the spheroidized metallic particles through a plasma one or more times to improve a spherical shape of the spheroidized metallic particles.
  • the method of clause 1-20 wherein a temperature of the plasma is suitable to melt the powder.
  • the method of clause 1-21 further comprising processing at least a portion of the spheroidized metallic particles by an additive manufacturing method to produce a part.
  • the method of clause 1-22 wherein the powder consists essentially of the metal hydride particles.
  • hydriding a titanium alloy comprising, in weight percentages based on total alloy weight, 87 to 91 titanium, 3.5 to 4.5 vanadium, and 5.5 to 6.75 aluminum to provide a hydrided source material;
  • a method for producing spheroidized metallic particles comprising:
  • the metal hydride particles comprise at least one of titanium hydride particles, titanium alloy hydride particles, aluminum hydride particles, aluminum alloy hydride particles, tantalum hydride particles, tantalum alloy hydride particles, niobium hydride particles, niobium alloy hydride particles, zirconium hydride particles, zirconium alloy hydride particles, hafnium hydride particles, hafnium alloy hydride particles, molybdenum hydride particles, molybdenum alloy hydride particles, vanadium hydride particles, and vanadium alloy hydride particles.
  • hydriding a titanium alloy comprising, in weight percentages based on total alloy weight, 87 to 91 titanium, 3.5 to 4.5 vanadium, and 5.5 to 6.75 aluminum to provide a hydrided source material;
  • a method for producing an additively manufactured part comprising:

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Abstract

L'invention concerne un procédé et un système destinés à convertir des poudres d'hydrure métallique irrégulières en poudres métalliques sphériques, et un article produit à partir de celles-ci. Le procédé consiste à préparer la poudre comprenant des particules d'hydrure métallique. La poudre est passée à travers un plasma pour ainsi décomposer les particules d'hydrure métallique, et la poudre est sphéroïdisée pour fournir des particules métalliques sphéroïdisées.
PCT/US2019/040053 2018-07-06 2019-07-01 Procédé et système de traitement de poudres métalliques, et articles produits à partir de celles-ci Ceased WO2020009955A1 (fr)

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US11577314B2 (en) 2015-12-16 2023-02-14 6K Inc. Spheroidal titanium metallic powders with custom microstructures
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US11611130B2 (en) 2019-04-30 2023-03-21 6K Inc. Lithium lanthanum zirconium oxide (LLZO) powder
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
US11839919B2 (en) 2015-12-16 2023-12-12 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
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US12195338B2 (en) 2022-12-15 2025-01-14 6K Inc. Systems, methods, and device for pyrolysis of methane in a microwave plasma for hydrogen and structured carbon powder production
US12261023B2 (en) 2022-05-23 2025-03-25 6K Inc. Microwave plasma apparatus and methods for processing materials using an interior liner
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US12214420B2 (en) 2015-12-16 2025-02-04 6K Inc. Spheroidal titanium metallic powders with custom microstructures
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US11471941B2 (en) 2018-06-19 2022-10-18 6K Inc. Process for producing spheroidized powder from feedstock materials
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US11611130B2 (en) 2019-04-30 2023-03-21 6K Inc. Lithium lanthanum zirconium oxide (LLZO) powder
US11311938B2 (en) 2019-04-30 2022-04-26 6K Inc. Mechanically alloyed powder feedstock
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WO2022094528A1 (fr) * 2020-10-30 2022-05-05 6K Inc. Systèmes et procédés de synthèse de poudres métalliques sphéroïdales
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US12406829B2 (en) 2021-01-11 2025-09-02 6K Inc. Methods and systems for reclamation of Li-ion cathode materials using microwave plasma processing
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CN114309621B (zh) * 2021-12-28 2023-11-10 云航时代(重庆)科技有限公司 一种含有难熔金属元素的微细TiAl合金球形粉体的制备方法
CN114309621A (zh) * 2021-12-28 2022-04-12 云航时代(重庆)科技有限公司 一种含有难熔金属元素的微细TiAl合金球形粉体的制备方法
US12261023B2 (en) 2022-05-23 2025-03-25 6K Inc. Microwave plasma apparatus and methods for processing materials using an interior liner
US12040162B2 (en) 2022-06-09 2024-07-16 6K Inc. Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows
US12094688B2 (en) 2022-08-25 2024-09-17 6K Inc. Plasma apparatus and methods for processing feed material utilizing a powder ingress preventor (PIP)
US12195338B2 (en) 2022-12-15 2025-01-14 6K Inc. Systems, methods, and device for pyrolysis of methane in a microwave plasma for hydrogen and structured carbon powder production

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