WO2020091854A1 - Method and system for processing metal powders, and articles produced therefrom - Google Patents

Method and system for processing metal powders, and articles produced therefrom Download PDF

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Publication number
WO2020091854A1
WO2020091854A1 PCT/US2019/040563 US2019040563W WO2020091854A1 WO 2020091854 A1 WO2020091854 A1 WO 2020091854A1 US 2019040563 W US2019040563 W US 2019040563W WO 2020091854 A1 WO2020091854 A1 WO 2020091854A1
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WIPO (PCT)
Prior art keywords
particles
alloy
oxygen
spheroidized
metallic powder
Prior art date
Application number
PCT/US2019/040563
Other languages
French (fr)
Inventor
Tracy BANK
Justen SCHAEFER
Mikhail GERSHENZON
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Arconic Inc.
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Publication date
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Publication of WO2020091854A1 publication Critical patent/WO2020091854A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00Products made by additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Definitions

  • the present disclosure relates to various embodiments of methods and systems for processing metallic powder and to an article produced therefrom.
  • the present disclosure relates to an additive manufacturing method and system.
  • properties of the powder feedstocks must be strictly controlled. Properties that may need to be controlled include, for example, average particle size, chemistry/composition, and/or morphology (i.e., particle shape). In such applications, and in particular in additive manufacturing applications, there are challenges to providing suitable metallic powder feedstocks.
  • the present disclosure provides a method for processing metallic powder for use in a powder metallurgy manufacturing process feedstock and/or additive manufacturing process feedstock.
  • the method comprises passing an oxygen- containing metallic powder feedstock and reductive metal particles through a plasma to thereby de-oxygenate and spheroidize the oxygen-containing metallic powder feedstock and produce spheroidized metallic particles. At least a portion of the reductive metal particles react with the oxygen-containing metallic powder feedstock and form an oxide compound.
  • the present disclosure provides a powder processing system.
  • the powder processing system comprises an inlet, an outlet, a reactor chamber, and a plasma generator. The inlet is in fluid communication with the reactor chamber.
  • the plasma generator is in communication with the reactor chamber and is adapted to generate a plasma in the reactor chamber.
  • the outlet is in fluid communication with the reactor chamber.
  • the inlet is adapted to receive an inlet stream comprising an oxygen-containing metallic powder feedstock and reductive metal particles and convey the inlet stream to the reactor chamber.
  • the reactor chamber is adapted to receive the inlet stream.
  • the inlet stream contacts the plasma in the reactor chamber, thereby de-oxygenating and spheroidizing the oxygen-containing metallic powder feedstock and producing reaction products comprising spheroidized metallic particles and an oxide compound.
  • the outlet is adapted to receive an outlet stream from the reactor chamber comprising the spheroidized metallic particles.
  • the spheroidized metallic particles may be used in a powder metallurgy manufacturing process and/or additive manufacturing process.
  • the present disclosure provides spheroidized metallic particles.
  • the spheroidized metallic particles may be used in a powder metallurgy process and/or an additive manufacturing process.
  • FIG. l is a flow chart illustrating a non-limiting embodiment of a method to process metallic powder according to the present disclosure.
  • FIG. 2 is a schematic representation of a non-limiting embodiment of a system adapted to process metallic powder according to the present disclosure.
  • Corresponding reference characters indicate corresponding parts throughout the several views. The examples set out herein illustrate certain embodiments, in one form, and such examples are not to be construed as limiting the scope of the appended claims in any manner.
  • 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. All such ranges are inherently described in this specification.
  • the grammatical articles“a,”“an,” and“the,” as used herein, are intended to include “at least one” or“one or more,” unless otherwise indicated, even if“at least one” or“one or more” is expressly used in certain instances.
  • the foregoing grammatical articles are used herein to refer to one or more than one (i.e., to“at least one”) of the particular identified elements.
  • the use of a singular noun includes the plural, and the use of a plural noun includes the singular, unless the context of the usage requires otherwise.
  • 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, a process to produce a tailored alloy product via additive manufacturing, or another process using metallurgical powder as a feedstock to produce a part.
  • particle size is as determined in accordance with ASTM standard B822.
  • “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).
  • 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 example, direct metal laser sintering (DMLS), selective laser melting (SLM), selective laser sintering (SLS), and electron beam melting (EBM). Any suitable feedstock may be used, including powder, wire, sheet, and combinations thereof.
  • “de-oxygenate”,“de-oxygenation”, and the like refer to reducing the oxygen content in a material, wherein the reduction in oxygen content in the material may be complete or partial.
  • A“de-oxygenated” powder for example, has a reduced oxygen content, which may be zero (i.e., oxygen content equal to 0 or below detection limits) or greater than zero (i.e., at least some oxygen content present), relative to a powder from which the de- oxygenated powder is produced.
  • “spheroidize”,“spheroidization”, and the like refer to increasing the sphericity of a powder, wherein the increase in sphericity may be complete (i.e., producing perfectly spherical particles) or partial.
  • “substantially comprise” or“substantially comprises” 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.
  • an oxygen-containing metallic powder feedstock may have an oxygen content that is too high for use in a particular powder metallurgical process or additive manufacturing process.
  • the maximum allowable oxygen content of a metallic powder may depend on, for example, the particular powder metallurgical process or additive manufacturing process; the composition of the metallic powder; and/or the final
  • an oxygen-containing metallic powder feedstock may need to be de-oxygenated to reduce oxygen content and render it suitable for use in a particular powder metallurgical process and/or additive manufacturing process.
  • a oxygen- containing metallic powder feedstock that is to be used in a particular powder metallurgical process and/or additive manufacturing process may also need to be subjected to a
  • a method and system are provided that can improve metallic feedstock characteristics (e.g., reduce oxygen content/promote de-oxygenation and/or improve sphericity).
  • oxygen-containing metallic powder feedstock and reductive metal particles can be brought into contact with (e.g., directed towards via a carrier gas) a plasma to thereby de-oxygenate and spheroidize the oxygen-containing metallic powder feedstock.
  • the de-oxygenation and spheroidization of the oxygen-containing metallic powder feedstock can occur simultaneously in a single reactor chamber and can form spheroidized metallic particles having reduced oxygen content relative to an oxygen content of the oxygen-containing metallic powder feedstock.
  • at least a portion of the reductive metal particles can react with the oxygen- containing metallic powder feedstock and form an oxide compound including oxygen derived from the metallic powder.
  • subjecting the reductive metal particles to the plasma in the reactor chamber may generate a reductive metal vapor that reacts with at least oxygen in the metallic powder (e.g., to scavenge excess oxygen from the oxygen-containing metallic powder feedstock) and produces an oxide compound.
  • a reductive metal vapor that reacts with at least oxygen in the metallic powder (e.g., to scavenge excess oxygen from the oxygen-containing metallic powder feedstock) and produces an oxide compound.
  • the metallic powder can comprise at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles, zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
  • the oxygen-containing metallic powder feedstock can comprise at least one of titanium and titanium alloy particles, for example, particles of 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 oxygen-containing metallic powder feedstock can comprise particles of Ti-6Al-4V alloy.
  • the oxygen-containing metallic powder feedstock can have a median particle size of at least 50 nm, such as, for example, at least 1 pm, at least 5 pm, at least 10 pm, at least 15 pm, at least 20 pm, at least 25 pm, at least 30 pm, at least 50 pm, at least 60 pm, at least 65 pm, or at least 105 pm.
  • the oxygen- containing metallic powder feedstock can have a median particle size no greater than 325 pm, such as, for example, no greater than 300 pm, no greater than 275 pm, no greater than 250 pm, no greater than 225 pm, no greater than 200 pm, no greater than 180 pm, no greater than 175 pm, no greater than 150 pm, no greater than 125 pm, no greater than 100 pm, no greater than 90 pm, no greater than 70 pm, no greater than 65 pm, no greater than 60 pm, no greater than 50 pm, no greater than 45 pm, no greater than 30 pm, no greater than 10 pm, or no greater than 1 pm.
  • a median particle size no greater than 325 pm, such as, for example, no greater than 300 pm, no greater than 275 pm, no greater than 250 pm, no greater than 225 pm, no greater than 200 pm, no greater than 180 pm, no greater than 175 pm, no greater than 150 pm, no greater than 125 pm, no greater than 100 pm, no greater than 90 pm, no greater than 70 pm, no greater than 65 pm, no greater than 60
  • the oxygen-containing metallic powder feedstock can have a median particle size in a range of 50 nm to 325 pm, such as, for example, 1 pm to 325 pm, 5 pm to 325 pm, 10 pm to 100 pm, 105 pm to 180 pm, 20 pm to 50 pm, 60 pm to 90 pm, 50 pm to 100 pm, 10 pm to 150 pm, 15 pm to 45 pm, 20 pm to 65 pm, 25 pm to 45 pm, 50 pm to 150 pm, 65 pm to 90 pm, 10 pm to 200 pm, 5 pm to 30 pm, 30 pm to 90 pm, or 5 pm to 50 pm.
  • the oxygen-containing metallic powder feedstock comprises, substantially comprises, or consists essentially of particles having an irregular shape.
  • Oxygen-containing metallic powder feedstock that has an irregular shape can have particles with an aspect ratio of at least 1.25 such as, for example, at least 2, where the aspect ratio is the largest diameter of a particle divided by the smallest diameter of the particle.
  • a powder that is“irregularly” shaped powder may include at least one sharp edge having an acute exterior angle.
  • Some non-limiting examples of irregularly shaped particles include: globular (non-spherical) powders, plate like powders, and/or acicular (needle shaped powders) to name a few.
  • An irregularly shaped particle may be contrasted with, for example, a substantially spherical particle.
  • reductive metal particles can be used in the method and system according to the present disclosure.
  • the reductive metal particles can be capable of reacting with at least oxygen in the metallic powder under the conditions in the reactor chamber and thereby reduce oxygen content in the oxygen-containing metallic powder feedstock.
  • the reductive metal particles are configured to be an oxygen scavenger which can remove at least some oxygen from the oxygen-containing metallic powder feedstock.
  • the reductive metal particles are configured to be an oxygen scavenger when activated by a plasma.
  • the reductive metal particles can comprise at least one of an alkali metal and an alkaline earth metal.
  • the reductive metal particles can comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium.
  • the reductive metal particles comprise calcium.
  • the reductive metal particles can comprise a composite metal compound such as, for example, dicalcium oxygen (e.g., Ca20) or ethyl magnesium bromide (e.g., CFFCFFMgBr)
  • the reductive metal particles can have a median particle size of at least 50 nm, such as, for example, at least 1 pm, at least 5 pm, at least 10 pm, at least 15 pm, at least 20 pm, at least 25 pm, at least 30 pm, at least 50 pm, at least 60 pm, at least 65 pm, at least 105 pm, at least 200 pm, at least 500 pm, or at least lmm.
  • a median particle size of at least 50 nm such as, for example, at least 1 pm, at least 5 pm, at least 10 pm, at least 15 pm, at least 20 pm, at least 25 pm, at least 30 pm, at least 50 pm, at least 60 pm, at least 65 pm, at least 105 pm, at least 200 pm, at least 500 pm, or at least lmm.
  • the reductive metal particles can have a median particle size of no greater than 2 mm, such as, for example, no greater than 1 mm, no greater than 500 pm, no greater than 325 pm, no greater than 300 pm, no greater than 275 pm, no greater than 250 pm, no greater than 225 mih, no greater than 200 mih, no greater than 180 mih, no greater than 175 mih, no greater than 150 mih, no greater than 125 mih, no greater than 100 mih, no greater than 90 mih, no greater than 70 mih, no greater than 65 mih, no greater than 60 mih, no greater than 50 mih, no greater than 45 mih, no greater than 30 mih, no greater than 10 mih, or no greater than 1 mih.
  • the reductive metal particles can have a median particle size in a range of 50 nm to 2mm, such as, for example, 1 pm to 2mm, 1 pm to lmm, 100 pm to 1 pm, 1 pm to 325 pm, 5 pm to 325 pm, 10 pm to 100 pm, 105 pm to 180 pm, 20 pm to 50 pm, 60 pm to 90 pm, 50 pm to 100 pm, 10 pm to 150 pm, 15 pm to 45 pm, 20 pm to 65 pm, 25 pm to 45 pm, 50 pm to 150 pm, 65 pm to 90 pm, 10 pm to 200 pm, 5 pm to 30 pm, 30 pm to 90 pm, or 5 pm to 50 pm.
  • the particle size of the reductive metal particle may be chosen/configured in order to control the amount and/or concentration of reductive metal vapor that can be generated in the reactor chamber when the reductive metal particles are subjected to the plasma.
  • the process can thereby be configured such that the plasma process and reductive metal particles are tailored for a particular oxygen-containing metallic powder feedstock (e.g., promoting maximum oxygen removal/oxygen scavenging while not utilizing excess reductive metal particles that may require additional removal steps).
  • the reductive metal particles can be chosen/configured based on a vaporization temperature of the reductive metal particles and/or the affinity for oxygen of the reductive metal particles.
  • the reductive metal particles can be chosen to have an affinity for oxygen greater than an affinity for oxygen of the oxygen-containing metallic powder feedstock.
  • a flow chart illustrating a non-limiting embodiment of a method to process oxygen-containing metallic powder feedstock according to the present disclosure is provided.
  • a oxygen-containing metallic powder feedstock and reductive metal particles can be combined in preselected proportions (102) to provide a substantially homogenous blend and/or a comingled mixture.
  • the oxygen-containing metallic powder feedstock and the reductive metal particles can be manually premixed to create a blend, or the oxygen-containing metallic powder feedstock and the reductive metal particles can be mixed in a dynamic in-line mixer.
  • the oxygen-containing metallic powder feedstock and the reductive metallic particles can be fed to the reactor chamber separately and mixed in-situ , in which case steps 102 and 104 in FIG. 1 can occur in tandem or simultaneously.
  • steps 102 and 104 in FIG. 1 can occur in tandem or simultaneously.
  • Other techniques for mixing/blending metallic powder and reductive metal particles will be apparent to those ordinarily skilled upon considering the present disclosure.
  • the oxygen-containing metallic powder feedstock and the reductive metal particles can be combined in a weight-to-weight or volume-to-volume ratio of oxygen-containing metallic powder feedstock to reductive metal particles of at least 1 :99 such as, for example, at least 5:95, at least 10:90, at least 20:80, at least 30:70, at least 40:60, at least 50:50, at least 60:40, at least 70:30, at least 80:20, at least 90: 10, or at least 95:5.
  • the oxygen-containing metallic powder feedstock and the reductive metal particles can be combined in a weight-to-weight or volume-to-volume ratio of oxygen- containing metallic powder feedstock to reductive metal particles no greater than 99: 1 such as, for example, no greater than 95: 1, no greater than 90: 10, no greater than 80:20, no greater than 70:30, no greater than 60:40, no greater than 50:50, no greater than 40:60, no greater than 30:70, no greater than 20:80, no greater than 10:90, or no greater than 5:95.
  • the oxygen-containing metallic powder feedstock and the reductive metal particles can be combined in a weight-to-weight or volume-to-volume ratio of oxygen- containing metallic powder feedstock to reductive metal particles in a range of 1 : 99 to 99: 1 such as, for example, 5:95 to 95:5, 40:60 to 99: 1, 50:50 to 99: 1, 60:40 to 99: 1, 70:30 to 99: 1, 80:20 to 99: 1, 90: 10 to 99:1, 95: 1 to 99: 1, 40:60 to 95:5, 50:50 to 95:5, 60:40 to 95:5, 70:30 to 95:5, 80:20 to 95:5, or 90: 10 to 95:5.
  • the process can be configured to maximize oxygen removal/oxygen scavenging while not utilizing excess reductive metal particles that may require additional removal steps).
  • the oxygen-containing metallic powder feedstock and the reductive metal particles contact plasma in a reactor chamber, producing spheroidized metallic particles from the oxygen-containing metallic powder feedstock (104).
  • a carrier gas is conducted into the reactor chamber with the oxygen-containing metallic powder feedstock and the reductive metal particles.
  • the carrier gas is designed to promote movement of the blend of oxygen-containing metallic powder feedstock and reductive metal particles to oxygen-containing metallic powder feedstock and reductant through the process.
  • the carrier gas can comprise, for example, at least one of helium, argon, nitrogen, and hydrogen.
  • the plasma is produced in the reactor chamber at least partially from the carrier gas.
  • the plasma is produced in the reactor chamber at least partially from a carrier gas and a second gas.
  • the second gas may be the same or different than the carrier gas.
  • the second gas can be at least one of helium, argon, nitrogen, and hydrogen.
  • the plasma can have an elevated temperature sufficient to at least partially vaporize the reductive metal particles and/or at least partially melt the oxygen-containing metallic powder feedstock.
  • the reductive metal particles can react with at least oxygen in the oxygen-containing metallic powder feedstock and form an oxide compound (106).
  • the plasma can both at least partially vaporize the reductive metal particles to form reductive metal vapor and at least partially melt the oxygen- containing metallic powder feedstock to form molten metallic powder feedstock.
  • the reductive metal vapor can react with at least oxygen in the molten metallic powder feedstock and form at least one oxide compound, reducing oxygen content of the molten metallic powder.
  • the oxide compound can be a reaction product of the reductive metal vapor and oxygen derived from the molten metallic powder.
  • a temperature of the plasma in the reactor chamber is sufficient to heat the reductive metal particles to at least 700 degrees Celsius such as, for example, at least 800 degrees Celsius, at least 900 degrees Celsius, at least 1000 degrees Celsius, at least 1100 degrees Celsius, at least 1200 degrees Celsius, at least 1300 degrees Celsius, at least 1400 degrees Celsius, at least 1500 degrees Celsius, at least 2000 degrees Celsius, at least 2500 degrees Celsius, or at least 3000 degrees Celsius.
  • a temperature of the plasma in the reactor chamber is sufficient to heat the reductive metal particles to no greater than 4000 degrees Celsius such as, for example, no greater than 3000 degrees Celsius, no greater than 2500 degrees Celsius, no greater than 2000 degrees Celsius, no greater than 1500 degrees Celsius, no greater than 1400 degrees Celsius, no greater than 1300 degrees Celsius, no greater than 1200 degrees Celsius, no greater than 1100 degrees Celsius, no greater than 1000 degrees Celsius, no greater than 900 degrees Celsius, or no greater than 800 degrees Celsius.
  • a temperature of the plasma in the reactor chamber is sufficient to heat the reductive metal particles to at least a boiling point temperature of the composition comprising the reductive metal particles.
  • the temperature of plasma and heating of the reductive metal particles can be tailored to/based upon the combination of reductive metal particles and oxygen-containing metallic powder feedstock selected (e.g., to promote melting and/or vaporization but not burn off/consumption of the feedstock).
  • a temperature of the plasma in the reactor chamber is sufficient to heat the oxygen-containing metallic powder feedstock to at least 700 degrees Celsius such as, for example, at least 800 degrees Celsius, at least 900 degrees Celsius, at least 1000 degrees Celsius, at least 1100 degrees Celsius, at least 1200 degrees Celsius, at least 1300 degrees Celsius, at least 1400 degrees Celsius, at least 1500 degrees Celsius, at least 2000 degrees Celsius, at least 2500 degrees Celsius, or at least 3000 degrees Celsius.
  • a temperature of the plasma in the reactor chamber is sufficient to heat the oxygen-containing metallic powder feedstock to no greater than 4000 degrees Celsius such as, for example, no greater than 3000 degrees Celsius, no greater than 2500 degrees Celsius, no greater than 2000 degrees Celsius, no greater than 1500 degrees Celsius, no greater than 1400 degrees Celsius, no greater than 1300 degrees Celsius, no greater than 1200 degrees Celsius, no greater than 1100 degrees Celsius, no greater than 1000 degrees Celsius, no greater than 900 degrees Celsius, or no greater than 800 degrees Celsius.
  • a temperature of the plasma in the reactor chamber is sufficient to heat the oxygen-containing metallic powder feedstock to at least a melting point temperature of the composition of the oxygen-containing metallic powder feedstock.
  • the contact time between the reductive metal particles and the oxygen-containing metallic powder feedstock and the plasma can be selected to at least partially vaporize the reductive metal particles and melt the oxygen-containing metallic powder feedstock.
  • the contact time between the reductive metal particles and the oxygen- containing metallic powder feedstock and the plasma can be at least 10 milliseconds (ms), such as, for example, at least 50 ms, at least 100 ms, or at least 500 ms.
  • the contact time between the reductive metal particles and the oxygen- containing metallic powder feedstock and the plasma can be no greater than 1 second (s), such as, for example, no greater than 500 ms, no greater than 100 ms, or no greater than 50 ms.
  • the contact time between the reductive metal particles and the oxygen-containing metallic powder feedstock and the plasma can be in a range of 10 ms to 1 s such as, for example, 50ms to 500ms.
  • the melting of the oxygen-containing metallic powder feedstock in the reactor chamber can increase sphericity of (i.e., spheroidize) the oxygen-containing metallic powder feedstock.
  • melted metallic powder in the reactor chamber may form molten spherical droplets that are cooled in the controlled environment of the reactor chamber and form dense spherical powder (e.g., metallic feedstock powder having improved (lowered) oxygen content and/or improved morphology; for example, the resulting density of the dense spherical powder is increased and/or the resulting packing density is improved as compared to the initial, oxygen-containing metallic feedstock powder).
  • dense spherical powder e.g., metallic feedstock powder having improved (lowered) oxygen content and/or improved morphology; for example, the resulting density of the dense spherical powder is increased and/or the resulting packing density is improved as compared to the initial, oxygen-containing metallic feedstock powder).
  • the oxygen-containing metallic powder feedstock is simultaneously de- oxygenated and spheroidized in a single process when contacting the hot plasma in the reactor chamber, resulting in spheroidized metallic particles having a reduced oxygen content as compared with an oxygen content of the metallic powder prior to contacting the plasma.
  • the oxide compound can be at least one of an alkali metal oxide and an alkaline earth metal oxide.
  • the oxide compound can comprise at least one of lithium oxide, sodium oxide, potassium oxide, beryllium oxide, magnesium oxide, calcium oxide, strontium oxide, and barium oxide.
  • the reductive metal particles can comprise calcium oxide.
  • the oxide compound has a median particle size that is within a range of 0.01 % to 100 % of the median particle size of the reductive metal particles such as, for example, 10 % to 90 % or 20% to 80%.
  • the oxide compound has a median particle size that is at least 0.01 % of the median particle size of the reductive metal particles, such as, for example, at least 10% or at least 20%. In various embodiments, the oxide compound has a median particle size that is no greater than 100 % of the median particle size of the reductive metal particles, such as, for example, no greater than 90% or no greater than 80%. For example, the oxide compound can have a median particle size smaller than the median particle size of the reductive metal particles. In some embodiments, the median particle size of the oxide compound can be based on the amount and/or size of the reductive metal particles that are introduced into the reactor chamber. In some embodiments, the reductive metal particles are tailored such that the resulting oxide compound is configured relative to the oxygen- containing metallic powder feedstock to promote improved mechanical/physical separation processes (e.g., differences in median particle size).
  • the spheroidized and de-oxygenated metallic particles produced in the reactor can comprise a composition similar to the oxygen-containing metallic powder feedstock introduced into the reactor, but the spheroidized and de-oxygenated metallic particles can have a higher sphericity and lower oxygen content than the oxygen- containing metallic powder feedstock.
  • the spheroidized and de-oxygenated metallic particles can comprise at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
  • the spheroidized and de- oxygenated metallic particles 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 spheroidized and de-oxygenated metallic particles can comprise Ti-6Al-4V alloy.
  • the spheroidized and de-oxygenated metallic particles comprise a concentration of no greater than 99% of reductive metal particles and/or the oxide compound based on the total weight of the oxygenated metallic particles, such as, for example, no greater than 5 % by weight of reductive metal particles and/or the oxide compound, no greater than 1 % by weight of reductive metal particles and/or the oxide compound, or no greater than 0.1 % by weight of reductive metal particles and/or the oxide compound, all based on the total weight of the oxygenated metallic particles.
  • the spheroidized and de-oxygenated metallic particles do not contain reductive metal particles and/or the oxide compound.
  • the spheroidized and de-oxygenated metallic particles have a median particle size that at least 50 % of a median particle size of the metallic powder introduced into the reactor chamber such as, for example, at least 55% or at least 60%. In various embodiments, the spheroidized and de-oxygenated metallic particles have a median particle size that is no greater than 100 % of a median particle size of the metallic powder introduced into the reactor chamber such as, for example, no greater than 95% or no greater than 90%.
  • the spheroidized and de-oxygenated metallic particles have a median particle size that is within a range of 50 % to 100 % of a median particle size of the metallic powder introduced into the reactor chamber such as, for example, 55% to 95% or 60% to 90%.
  • the spheroidized and de-oxygenated metallic particles can have a weight percent oxygen content no greater than 95% of the oxygen content of the oxygen-containing metallic powder feedstock such as, for example, no greater than 90%, no greater than 80%, no greater than 70%, no greater than 60%, no greater than 50%, no greater than 40%, no greater than 30%, no greater than 20%, no greater than 10%, no greater than 5%, or no greater than 1% of the oxygen content of the metallic powder.
  • the spheroidized and de-oxygenated metallic particles can have a sphericity of at least 0.8, such as, for example, at least 0.85 or at least 0.92.
  • Sphericity of particles can be measured utilizing a Camsizer XT with an X-Dry module and an X-Jet cartridge according to equation 1.
  • a and P can be measured by capturing images of the particles using a high-resolution video camera in the Camsizer XT. Then the Camsizer XT automatically utilizes image analysis to identify, separate, and trace the edges of particles. Based on the traces, A and P can be determined.
  • sphericity refers to the average sphericity of the particles measured.
  • oxygen contents of the oxygen-containing metallic powder feedstock introduced into the reactor chamber and of the spheroidized and de-oxygenated metallic particles can vary depending on composition of the oxygen-containing metallic powder feedstock.
  • oxygen-containing metallic powder feedstock comprising a titanium alloy may include 0.2% to 1% by weight oxygen
  • spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.2% by weight, for example, less than 0.16% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising an aluminum alloy may include 0.2% to 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.20% by weight oxygen, such as, for example, no greater than 0.16% by weight oxygen or no greater than 0.1% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising a cobalt alloy may include 0.2% to 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.2% by weight oxygen such as, for example, no greater than 0.1% by weight oxygen or no greater than 0.06% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising a nickel alloy may include 0.05% to 0.5% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.05% by weight oxygen, such as, for example, no greater than 0.015% by weight oxygen or no greater than 0.010% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising an iron alloy may include 0.1% to 0.5% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.1% by weight oxygen, such as, for example, less than 0.03% by weight oxygen or less than 0.02% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising a copper alloy may include at least 0.2% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.2% by weight oxygen, such as, for example, no greater than 0.04% by weight oxygen or no greater than 0.02% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising a tantalum alloy may include at least 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 1% by weight oxygen, such as, for example, no greater than 0.2% by weight oxygen or no greater than 0.1% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising tungsten may include at least 0.3% by weight oxygen, and spheroidized and de- oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.3% by weight oxygen, such as, for example, no greater than 0.05% by weight oxygen or no greater than 0.02% by weight oxygen.
  • oxygen-containing metallic powder feedstock comprising, and in various embodiments consisting of, molybdenum may include at least 0.3% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.3% by weight oxygen, such as, for example, no greater than 0.05% by weight oxygen or no greater than 0.02% by weight oxygen.
  • the oxygen contents described herein are for illustration purposes only and should not be considered limiting.
  • the desired oxygen content in the spheroidized and de-oxygenated metallic particles can vary depending on, for example, the powder metallurgical process and/or additive manufacturing process in which the metallic particles will be used.
  • the spheroidized and de-oxygenated metallic particles, and optionally at least a portion of at least one of the oxide compound and any unreacted reductive metal particles can be recycled through a plasma (e.g., passed through the plasma one or more additional times) (108), thereby further reducing an oxygen content in the metallic particles.
  • the spheroidized and de-oxygenated metallic particles can be passed through a plasma a plurality of (i.e., two or more) times.
  • Several passes through a plasma can further reduce the oxygen content of the metallic particles and further promote a spherical shape (e.g., increase sphericity) of metallic particles.
  • the additional passes also can produce additional oxide compound.
  • additional reductive metal particles can be combined with the recycled metallic particles that are being recycled, either before or simultaneously with introducing the recycled metallic particles into a reactor chamber to contact a plasma.
  • At least a portion of the spheroidized and de-oxygenated metallic particles produced using the method and/or system of the present disclosure can be separated from oxide compound and any unreacted reductive metal particles (110). Separating the particles can be accomplished using mechanical separation equipment including, but not limited to: at least one of a sieve, a settling chamber, and a cyclone. Selecting the median particle size of the reductive metallic particles used in the method/system based on the median particle size of the oxygen-containing metallic powder feedstock used can increase the efficiency of the separation. For example, a median particle size of the reductive metal particles can be selected so that it differs from a median particle size of the oxygen-containing metallic powder feedstock. A difference in median particle size may facilitate separation of the metallic feedstock powder and/or spheroidized and de-oxygenated metallic particles produced therefrom from the reductive metal particles and/or oxide compound produced therefrom.
  • separating (108) can comprise contacting the spheroidized and de-oxygenated metallic particles with a solvent to thereby dissolve at least a portion of the oxide compound. Thereafter, the solvent and dissolved oxide compound can be removed from the spheroidized and de-oxygenated metallic particles which can result in a product comprising, substantially comprising, or consisting of spheroidized and de-oxygenated metallic particles.
  • the solvent can be any of the various materials known in the art for dissolving an oxide compound.
  • the solvent can comprise at least one of water and an acid.
  • spheroidized and de-oxygenated metallic particles produced by the method and/or system according to the present disclosure can be used to produce a part.
  • the spheroidized and de-oxygenated metallic particles can be used as powder in a powder metallurgy system/process and/or an additive manufacturing system/process and processed into a part 112.
  • at least a portion of spheroidized and de-oxygenated metallic particles made using the present method and/or system can be processed by an additive manufacturing method to produce a part and/or in a coating process, such as, for example, a cold spray process or a plasma spray process.
  • FIG. 2 a schematic representation of a non-limiting embodiment of a system 200 to process oxygen-containing metallic powder feedstock is shown.
  • Reaction chamber 202 is provided with an inlet 204 and an outlet 206.
  • the inlet 204 is adapted to receive an inlet stream comprising oxygen-containing metallic powder feedstock 208 and reductive metal particles 210.
  • the inlet 204 can be adapted to convey the inlet stream into the reactor chamber 202 as a combined inlet stream (including both metallic powder and reductive metal particles) or in separate inlet streams (a first inlet stream conveying oxygen- containing metallic powder feedstock, and a second inlet stream conveying reductive metal particles).
  • the inlet 204 may comprise a first section adapted to receive oxygen-containing metallic powder feedstock 208, a second section adapted to receive reductive metal particles 210, and a dynamic mixer adapted to blend quantities of the oxygen-containing metallic powder feedstock 208 and the reductive metal particles 210 in a preselected weight-to-weight or volume-to-volume ratio, and wherein the blended materials are then passed into the reactor chamber 202.
  • the inlet stream comprises an additional material such as, for example, a carrier gas and a second gas.
  • the reactor chamber 202 is adapted so that spheroidized and de- oxygenated metallic particles 212 and an oxide compound 214 are formed within the reactor chamber 202 from the oxygen-containing metallic powder feedstock 208 and the reductive metal particles 210.
  • the chamber 202 can be configured to include a plasma generator 216 adapted to produce a hot plasma 218, and the oxygen-containing metallic powder feedstock 208 and reductive metal particles 210 can be brought into contact with the plasma 218 in the chamber 202.
  • the plasma 218 can promote at least partial melting of the oxygen-containing metallic powder feedstock 208 to produce molten oxygen-containing metallic powder feedstock 208a, and can also promote at least partial vaporization of the reductive metal particles 210 to form reductive metal vapor 230.
  • the reductive metal vapor 230 can react with at least oxygen in the molten oxygen-containing metallic powder feedstock 208a, thereby reducing oxygen content in the molten oxygen-containing metallic powder feedstock 208a.
  • the reductive metal vapor 230 and oxygen derived from the molten metallic powder 208a can form the oxide compound 214.
  • the reactor chamber 202 operates under conditions that promote spheroidization of the metallic powder 208 in the reactor chamber 202.
  • the reactor chamber 202 can have a pressure of 5 pounds per square inch absolute (psia) to 25 psia to promote spheroidization of the metallic powder 208 in the reactor chamber 202, such as for example, 14 psia to 16 psia.
  • the reactor chamber 202 has a pressure greater than atmospheric pressure outside of the reactor chamber 202.
  • the spheroidization can, for example, reduce the number of faces, edges, and/or features otherwise out of round in the oxygen-containing metallic powder feedstock 208.
  • the spheroidization occurring in the reactor chamber 202 increases sphericity of the oxygen-containing metallic powder feedstock 208.
  • an outlet stream comprising spheroidized and de-oxygenated metallic particles 212 and oxide compound 214 formed in the reactor chamber 202, and unreacted reductive metal particles 210, can pass into outlet 206 and can be collected.
  • 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 occurring in the reactor chamber 202.
  • the plasma 218 produced in reactor chamber 202 can be generated by any of various plasma generating apparatus or techniques known in the art.
  • plasma 218 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 plasma 218 is generated in one or more of various regions within the chamber 202.
  • the plasma 218 is generated so that oxygen-containing metallic powder feedstock 208 introduced into chamber 202 contacts plasma 218 in a manner that facilitates de-oxygenation and
  • the system 200 can be designed so that the plasma 218 is generated axially with respect to the flow of the oxygen- containing metallic powder feedstock 208 through the reactor chamber 202.
  • the plasma 218 can also be positioned within the reactor chamber 202 to enhance the de-oxygenation effect of the plasma 218, so as to reduce oxygen content of oxygen-containing metallic powder feedstock 208 introduced into reactor chamber 202.
  • the plasma 218 comprises inductively coupled plasma.
  • the plasma 218 comprises microwave plasma.
  • the plasma can be a thermal plasma or a non- thermal plasma.
  • the plasma 218 can have a temperature suitable to promote at least partial melting of the oxygen-containing metallic powder feedstock 208 and/or at least partial vaporization of the reductive metal particles 210.
  • an electron temperature of the plasma 218 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, or at least 10,000 K.
  • the electron temperature of the plasma 218 can be in a range of 3,000 K to 12,000 K such as, for example, 4,000 K to 12,000 K, 4,000 K to 10,000 K, 6,000 K to 12,000 K, or 6,000 K to 10,000 K.
  • the plasma 218 can be at least partially produced from a carrier gas and/or a second gas fed to the system 200 through, for example, the inlet 204.
  • a vacuum port 220 can be provided in fluid communication with the reactor chamber 202.
  • the vacuum port 220 can be adapted to convey gases and particulate from the chamber 202.
  • the pressure in the vacuum port 220 can be less than a pressure in the chamber 202 to create a pressure differential which facilitates movement of gases and particulate into the vacuum port 220.
  • the vacuum port 220 can be in fluid communication with a vacuum source 222 such as, for example, a vacuum pump, to create a pressure differential between the vacuum port 220 and the reactor chamber 202.
  • the particulate entering the vacuum port 220 under influence of the pressure differential can substantially comprise the oxide compound 214 and residual reductive metal particles 210.
  • the particulate entering the vacuum port 220 under influence of the pressure differential can additionally comprise spheroidized and de-oxygenated metallic particles 212.
  • the vacuum port 220 can be positioned and oriented in relation to the reactor chamber 202 to limit conveyance of spheroidized and de-oxygenated metallic particles 212 into the vacuum port 220.
  • vacuum port 220 may be positioned on a side wall of the chamber 202 and/or may have an incline.
  • the spheroidized and de-oxygenated metallic particles 212 can have a larger median particle size than a median particle size of the oxide compound 214 and/or residual reductive metal particles 210 such that the larger spheroidized and de-oxygenated metallic particles 212 generally are not drawn into the vacuum port 220. However, trace amounts of spheroidized and de-oxygenated metallic particles 212 still may be drawn into the vacuum port 220.
  • a filter 224 can be provided in fluid communication with the vacuum port 220 and adapted to separate particulate from gases. After a period of time, the particulate may be removed from the vacuum port 220 by replacing the filter 224 and/or removing the particulate from the filter 224.
  • a size classification module 226 can be provided in fluid communication with the outlet 206.
  • the size classification module 226 can be adapted to receive the outlet stream from the outlet 206 and separate spheroidized and de-oxygenated metallic particles 212 from at least one of residual reductive metal particles 210 and oxide compound 214 in the outlet stream.
  • the size classification module 226 can comprise at least one of a sieve, a settling chamber, and a cyclone.
  • the size classification module includes a washing module adapted to receive the outlet stream and contact the outlet stream with a solvent suitable to dissolve at least a portion of the oxide compound 214 in the outlet stream. The washing module can remove the solvent and dissolved oxide compound from the spheroidized and de-oxygenated metallic particles 212 and produce a product comprising, substantially comprising, or consisting of spheroidized and de-oxygenated metallic particles 212.
  • a recycle line 228 can be in fluid communication with the outlet 206 and adapted to receive at least a portion of the spheroidized and de-oxygenated metallic particles 212 from the outlet 206.
  • the recycle line 228 can be suitable to output at least a portion of the spheroidized and de-oxygenated metallic particles 212 into the inlet 204, through which the particles are conveyed into the reactor chamber 202 to pass through the plasma 218.
  • the spheroidized and de-oxygenated metallic particles 212 can be recycled into the reactor chamber 202 through recycle line 228 as many times as necessary to remove the desired level of oxygen from and/or further spheroidize the spheroidized and de-oxygenated metallic particles 212.
  • the spheroidized and de-oxygenated metallic particles 212 produced utilizing system 200 can be used to produce a part.
  • at least a portion of the spheroidized and de- oxygenated metallic particles 212 can be used as powder in a powder metallurgy system/process such as, for example, an additive manufacturing system/process, and processed into a part.
  • at least a portion of the spheroidized and de-oxygenated metallic particles 212 produced in system 200 can be processed by an additive manufacturing method to produce a part comprising the spheroidized and de-oxygenated metallic particles 212.
  • an additive manufacturing process includes depositing successive layers of powder and then selectively melting and/or sintering the powder to create, layer-by-layer, a part.
  • a powder bed is used to create a part such as, for example, a tailored alloy part and/or a unique structure unachievable through traditional manufacturing techniques (e.g., without excessive post-processing machining).
  • Non-limiting examples of additive manufacturing processes useful in producing parts from feedstocks include, for example, BJAM, DMLS, SLM, SLS, and EBM, among others.
  • an additive manufacturing process uses an EOSINT M 280 Direct Metal Laser Sintering (DMLS) additive manufacturing system, or comparable system, available from EOS GmbH (Robert-Stirling-Ring 1, 82152 Krailling/Munich, Germany).
  • Additive manufacturing techniques e.g., when utilizing metallic feedstocks
  • feedstocks may be used, including powder, a wire, a sheet, and combinations thereof.
  • the feedstock may be, for example, metallic feedstocks (e.g., with additives to promote various properties such as, for example, grain refiners and/or ceramic materials), polymeric feedstocks (e.g., plastic feedstocks), and ceramic feedstocks.
  • the wire can comprise a ribbon and/or a tube.
  • the metallic feedstocks can be at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy.
  • reagent-based feedstock materials which form polymeric parts can be used as feedstock.
  • aluminum alloy means a metal alloy having aluminum as the predominant alloying element. Similar definitions apply to the other corresponding alloys referenced herein (e.g., titanium alloy means a titanium alloy having titanium as the predominant alloying element).
  • an additive manufacturing process comprises (a) dispersing a feedstock (e.g., powder in a powder bed), (b) selectively heating a portion of the powder (e.g., via an energy source) to a temperature above the liquidus temperature of the powder,
  • a feedstock e.g., powder in a powder bed
  • a portion of the powder e.g., via an energy source
  • Steps (a)-(d) may be repeated as necessary until the additively manufactured part is completed.
  • an additive manufacturing process comprises (a) dispersing a feedstock (e.g., metallic powder) in a deposition region, (b) selectively binder jetting the feedstock, and (c) repeating steps (a)-(b), thereby producing a final additively manufactured part (e.g., including optionally heating to burn off binder and form a green form, followed by sintering to form the additively manufactured part).
  • a feedstock e.g., metallic powder
  • steps (a)-(b) thereby producing a final additively manufactured part (e.g., including optionally heating to burn off binder and form a green form, followed by sintering to form the additively manufactured part).
  • Electron beam techniques are utilized to produce at least a portion of the additively manufactured part. Electron beam techniques may facilitate production of larger parts than readily produced via laser additive manufacturing techniques.
  • An illustrative example provides feeding a wire to the wire feeder portion of an electron beam gun.
  • the wire may comprise a metallic feedstock.
  • the electron beam heats the wire above the liquidus point of the metallic feedstock and deposits the molten pool in a deposition region. Thereafter, rapid solidification of the molten pool to form the deposited material occurs.
  • the additively manufactured part may be subject to any appropriate dissolving (e.g., includes homogenization), working and/or precipitation hardening steps. If employed, the dissolving and/or the working steps may be conducted on an intermediate form of the additively manufactured part and/or may be conducted on a final form of the additively manufactured part. If employed, the precipitation hardening step is generally conducted relative to the final form of the additively manufactured part.
  • dissolving and/or the working steps may be conducted on an intermediate form of the additively manufactured part and/or may be conducted on a final form of the additively manufactured part.
  • the precipitation hardening step is generally conducted relative to the final form of the additively manufactured part.
  • an additively manufactured part may be deformed (e.g., by one or more of rolling, extruding, forging, stretching, compressing).
  • the final deformed product may realize, for instance, improved properties due to the tailored regions and thermo- mechanical processing of the final deformed part.
  • the final part is a wrought part, the word“wrought” referring to the working (hot working and/or cold working) of the additively manufactured part, wherein the working occurs relative to an intermediate and/or final form of the additively manufactured part.
  • the final part is a non-wrought product, i.e., is not worked during or after the additive
  • the resulting additively manufactured parts made in accordance with the systems and methods described herein may be used in a variety of product applications such as, commercial end-uses in industrial applications, in consumer applications (e.g., consumer electronics and/or appliances), or in other areas.
  • the additively manufactured parts can be utilized in at least one of the aerospace field (e.g., aerospace component), automotive field (e.g., automotive component), transportation field (e.g., transportation component), or building and construction field (e.g., building component or construction component).
  • the additively manufactured parts can be configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component.
  • an additively manufactured part can be utilized in an elevated temperature application, such as in an aerospace or automotive vehicle.
  • an additively manufactured part can be utilized as an engine component in an aerospace vehicle (e.g., in the form of a blade, such as a compressor blade incorporated into the engine).
  • an additively manufactured part can be used as a heat exchanger for the engine of the aerospace vehicle.
  • the aerospace vehicle including the engine component / heat exchanger may subsequently be operated.
  • an additively manufactured part can be an automotive engine component.
  • the automotive vehicle including an automotive component (e.g., engine component) may subsequently be operated.
  • the additively manufactured part may be used as a turbo charger component (e.g., a compressor wheel of a turbo charger, where elevated temperatures may be realized due to recycling engine exhaust back through the turbo charger), and the automotive vehicle including the turbo charger component may be operated.
  • a turbo charger component e.g., a compressor wheel of a turbo charger, where elevated temperatures may be realized due to recycling engine exhaust back through the turbo charger
  • an additively manufactured part may be used as a blade in a land based (stationary) turbine for electrical power generation, and the land-based turbine included the additively manufactured part may be operated to facilitate electrical power generation.
  • an additively manufactured part can be utilized in defense applications, such as in body armor, and armed vehicles (e.g., armor plating).
  • the additively manufactured part can be utilized in consumer electronic applications, such as in consumer electronics, such as, laptop computer cases, battery cases, cell phones, cameras, mobile music players, handheld devices, computers, televisions, microwaves, cookware, washers/dryers, refrigerators, and sporting goods, among others.
  • consumer electronics such as, laptop computer cases, battery cases, cell phones, cameras, mobile music players, handheld devices, computers, televisions, microwaves, cookware, washers/dryers, refrigerators, and sporting goods, among others.
  • an additively manufactured part can be utilized in a structural application, such as, for example, an aerospace structural application and an automotive structural application.
  • the additively manufactured part may be formed into various aerospace structural components, including floor beams, seat rails, fuselage framing, bulkheads, spars, ribs, longerons, and brackets, among others.
  • the additively manufactured part can be utilized in an automotive structural application.
  • the additively manufactured part can be formed into various automotive structural components including nodes of space frames, shock towers, and subframes, among others.
  • the additively manufactured part can be a body -in-white automotive product.
  • the additively manufactured part can be utilized in an industrial engineering application.
  • the additively manufactured part or products may be formed into various industrial engineering products, such as tread-plate, tool boxes, bolting decks, bridge decks, and ramps, among others.
  • the reductive metal particles comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium.
  • the method of any one of clauses 1 to 5 wherein the reductive metal particles comprise a median particle size in a range of 50 nm to 2mm.
  • the method of any one of clauses 1 to 6 wherein the reductive metal particles comprise a median particle size different than a median particle size of the oxygen- containing metallic powder feedstock.
  • the solvent comprises at least one of water and an acid.
  • the oxygen-containing metallic powder feedstock has a median particle size in a range of 50 nm to 325 pm.
  • the oxygen-containing metallic powder feedstock comprises an irregular shape.
  • the oxygen-containing metallic powder feedstock comprises at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
  • the method of any one of clauses 1 to 16 further comprising passing a carrier gas through the plasma, the carrier gas comprising at least one of helium, argon, nitrogen, and hydrogen.
  • the plasma at least partially vaporizes the reductive metal particles and at least partially melts the oxygen-containing metallic powder feedstock
  • the vaporized reductive metal particles and the melted metallic powder feedstock react to form products comprising the spheroidized and de-oxygenated metallic particles and the oxide compound.
  • the oxygen-containing metallic powder feedstock comprises a titanium alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises an aluminum alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises a cobalt alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises a nickel alloy and a weight percentage oxygen content in a range of 0.05 percent by weight oxygen to 0.5 percent by weight oxygen and the
  • the oxygen-containing metallic powder feedstock comprises an iron alloy and a weight percentage oxygen content in a range of 0.1 percent by weight oxygen to 0.5 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.1 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises a copper alloy and a weight percentage oxygen content of at least 0.2 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises a tantalum alloy and a weight percentage oxygen content of at least 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 1 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises a tungsten alloy and a weight percentage oxygen content of at least 0.3 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.3 percent by weight oxygen.
  • the oxygen-containing metallic powder feedstock comprises a molybdenum alloy and a weight percentage oxygen content of at least 0.3 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.3 percent by weight oxygen.
  • the spheroidized and de-oxygenated metallic particles of clause 34 wherein the particles are selected from the group comprising titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
  • the part comprises at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy.
  • the part of any one of clauses 37 to 38, wherein the part comprises Ti-6Al-4V alloy.
  • the part of any one of clauses 37 to 39, wherein the part is configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component.
  • a powder processing system comprising:
  • a plasma generator in communication with the reactor chamber and adapted to generate a plasma in the reactor chamber
  • the inlet is adapted to receive an inlet stream comprising an oxygen- containing metallic powder feedstock and reductive metal particles and convey the inlet stream to the reactor chamber;
  • the reactor chamber is adapted to receive the inlet stream and contact the inlet stream with the plasma, thereby de-oxygenating and spheroidizing the oxygen-containing metallic powder feedstock and producing reaction products comprising spheroidized and de-oxygenated metallic particles and an oxide compound;
  • outlet is adapted to receive an outlet stream from the reactor chamber comprising the spheroidized and de-oxygenated metallic particles.
  • a vacuum port in fluid communication with the reactor chamber, the vacuum port adapted to convey gases and particulate from the reactor, the particulate substantially comprising the oxide compound and residual reductive metal particles.
  • the system of clause 42 further comprising a filter in fluid communication with the vacuum port and adapted to separate the particulate from the gases.
  • the inlet comprises a first section adapted to receive the oxygen-containing metallic powder feedstock, a second section adapted to receive the reductive metal particles, and a dynamic mixer adapted to blend quantities of the oxygen-containing metallic powder feedstock and the reductive metal particles in a preselected weight-to-weight or volume-to-volume ratio.
  • a weight percentage oxygen content of the spheroidized and de-oxygenated metallic particles is no greater than 95 percent a weight percentage oxygen content of the oxygen-containing metallic powder feedstock.
  • the reductive metal particles comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium.
  • a size classification module in fluid communication with the outlet, the size classification module adapted to receive the outlet stream from the outlet and separate the spheroidized and de-oxygenated metallic particles from at least one of residual reductive metal particles and the oxide compound in the outlet stream.
  • the size classification module comprises at least one of a sieve, a settling chamber, and a cyclone.
  • a washing module in communication with the outlet, the washing module adapted to receive the outlet stream and contact the outlet stream with a solvent suitable to dissolve at least a portion of the oxide compound.
  • the solvent comprises at least one of water and an acid.
  • the metallic powder comprises at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
  • recycle line in communication with the outlet and the inlet, the recycle line adapted to receive at least a portion of the spheroidized and de-oxygenated metallic particles from the outlet and transport the at least a portion of the spheroidized and de- oxygenated metallic particles to the inlet.

Abstract

A method and a system for processing metallic powders, and an article produced therefrom are provided. An oxygen-containing metallic powder feedstock and reductive metal particles are contacted with a plasma to thereby de-oxygenate and spheroidize the oxygen-containing metallic powder feedstock and produce spheroidized and de-oxygenated metallic particles. At least a portion of the reductive metal particles react with at least oxygen in the oxygen-containing metallic powder feedstock and form an oxide compound.

Description

TITLE
METHOD AND SYSTEM FOR PROCESSING METAL POWDERS,
AND ARTICLES PRODUCED THEREFROM
CROSS-REFERENCE
[0001] This application claims priority to U.S. Provisional Patent Application No.
62/753,102, which was filed on October 31, 2018. The contents of which is incorporated by reference into this specification.
FIELD OF USE
[0002] The present disclosure relates to various embodiments of methods and systems for processing metallic powder and to an article produced therefrom. In certain embodiments, the present disclosure relates to an additive manufacturing method and system.
BACKGROUND
[0003] In various powder metallurgy manufacturing applications and/or additive
manufacturing applications, properties of the powder feedstocks must be strictly controlled. Properties that may need to be controlled include, for example, average particle size, chemistry/composition, and/or morphology (i.e., particle shape). In such applications, and in particular in additive manufacturing applications, there are challenges to providing suitable metallic powder feedstocks.
SUMMARY
[0004] According to one aspect, the present disclosure provides a method for processing metallic powder for use in a powder metallurgy manufacturing process feedstock and/or additive manufacturing process feedstock. The method comprises passing an oxygen- containing metallic powder feedstock and reductive metal particles through a plasma to thereby de-oxygenate and spheroidize the oxygen-containing metallic powder feedstock and produce spheroidized metallic particles. At least a portion of the reductive metal particles react with the oxygen-containing metallic powder feedstock and form an oxide compound. [0005] According to yet another aspect, the present disclosure provides a powder processing system. The powder processing system comprises an inlet, an outlet, a reactor chamber, and a plasma generator. The inlet is in fluid communication with the reactor chamber. The plasma generator is in communication with the reactor chamber and is adapted to generate a plasma in the reactor chamber. The outlet is in fluid communication with the reactor chamber. The inlet is adapted to receive an inlet stream comprising an oxygen-containing metallic powder feedstock and reductive metal particles and convey the inlet stream to the reactor chamber. The reactor chamber is adapted to receive the inlet stream. The inlet stream contacts the plasma in the reactor chamber, thereby de-oxygenating and spheroidizing the oxygen-containing metallic powder feedstock and producing reaction products comprising spheroidized metallic particles and an oxide compound. The outlet is adapted to receive an outlet stream from the reactor chamber comprising the spheroidized metallic particles. The spheroidized metallic particles may be used in a powder metallurgy manufacturing process and/or additive manufacturing process.
[0006] According to a further aspect, the present disclosure provides spheroidized metallic particles. The spheroidized metallic particles may be used in a powder metallurgy process and/or an additive manufacturing process.
[0007] It is understood that the inventions disclosed and described in this specification are not limited to the aspects summarized in this Summary. The reader will appreciate the foregoing details, as well as others, upon considering the following detailed description of various non-limiting and non-exhaustive aspects according to this specification.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The features and advantages of the examples, and the manner of attaining them, will become more apparent, and the examples will be better understood by reference to the following description taken in conjunction with the accompanying drawings, wherein:
[0009] FIG. l is a flow chart illustrating a non-limiting embodiment of a method to process metallic powder according to the present disclosure; and
[0010] FIG. 2 is a schematic representation of a non-limiting embodiment of a system adapted to process metallic powder according to the present disclosure. [0011] Corresponding reference characters indicate corresponding parts throughout the several views. The examples set out herein illustrate certain embodiments, in one form, and such examples are not to be construed as limiting the scope of the appended claims in any manner.
DETAILED DESCRIPTION OF NON-LIMITING EMBODIMENTS
[0012] Various embodiments are described and illustrated herein to provide an overall understanding of the structure, function, and use of the disclosed methods, systems, and articles of manufacture. The various embodiments described and illustrated herein are non limiting and non-exhaustive. Thus, the invention is not limited by the description of the various non-limiting and non-exhaustive embodiments disclosed herein. Rather, the invention is defined solely by the claims. The features and characteristics illustrated and/or described in connection with various embodiments may be combined with the features and characteristics of other embodiments. Such modifications and variations are intended to be included within the scope of this specification. As such, the claims may be amended to recite any features or characteristics expressly or inherently described in, or otherwise expressly or inherently supported by, this specification. Further, Applicant reserves the right to amend the claims to affirmatively disclaim features or characteristics that may be present in the prior art. The various embodiments disclosed and described in this specification can comprise, consist of, or consist essentially of the features and characteristics as variously described herein.
[0013] Any patent, publication, or other disclosure material identified herein is incorporated herein by reference in its entirety unless otherwise indicated, but only to the extent that the incorporated material does not conflict with existing definitions, statements, or other disclosure material expressly set forth in this specification. As such, and to the extent necessary, the express disclosure as set forth in this specification supersedes any conflicting material incorporated by reference herein. Any material, or portion thereof, that is said to be incorporated by reference into this specification, but which conflicts with existing definitions, statements, or other disclosure material set forth herein, is only incorporated to the extent that no conflict arises between that incorporated material and the existing disclosure material. Applicant reserves the right to amend this specification to expressly recite any subject matter, or portion thereof, incorporated by reference herein. [0014] Any references herein to“various embodiments,”“some embodiments,”“one embodiment,”“an embodiment,” or like phrases, mean that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, appearances of the phrases“in various embodiments,”“in some embodiments,”“in one embodiment,”“in an embodiment,” or like phrases, in the
specification do not necessarily refer to the same embodiment. Furthermore, the particular described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. Thus, the particular features, structures, or characteristics illustrated or described in connection with one embodiment may be combined, in whole or in part, with the features, structures, or characteristics of one or more other embodiments without limitation. Such modifications and variations are intended to be included within the scope of the present embodiments.
[0015] In this specification, unless otherwise indicated, all numerical parameters are to be understood as being prefaced and modified in all instances by the term“about,” in which the numerical parameters possess the inherent variability characteristic of the underlying measurement techniques used to determine the numerical value of the parameter. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter described herein should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
[0016] Also, any numerical range recited herein includes all sub-ranges subsumed within the recited range. For example, 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. All such ranges are inherently described in this specification.
[0017] The grammatical articles“a,”“an,” and“the,” as used herein, are intended to include “at least one” or“one or more,” unless otherwise indicated, even if“at least one” or“one or more” is expressly used in certain instances. Thus, the foregoing grammatical articles are used herein to refer to one or more than one (i.e., to“at least one”) of the particular identified elements. Further, the use of a singular noun includes the plural, and the use of a plural noun includes the singular, unless the context of the usage requires otherwise.
[0018] As used herein,“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, a process to produce a tailored alloy product via additive manufacturing, or another process using metallurgical powder as a feedstock to produce a part.
[0019] As used herein,“particle size” is as determined in accordance with ASTM standard B822.
[0020] As used herein,“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).
[0021] As used herein,“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.” Non-limiting examples of additive manufacturing processes useful in producing products from metallic feedstock include, for example, direct metal laser sintering (DMLS), selective laser melting (SLM), selective laser sintering (SLS), and electron beam melting (EBM). Any suitable feedstock may be used, including powder, wire, sheet, and combinations thereof.
[0022] As used herein,“de-oxygenate”,“de-oxygenation”, and the like refer to reducing the oxygen content in a material, wherein the reduction in oxygen content in the material may be complete or partial. A“de-oxygenated” powder, for example, has a reduced oxygen content, which may be zero (i.e., oxygen content equal to 0 or below detection limits) or greater than zero (i.e., at least some oxygen content present), relative to a powder from which the de- oxygenated powder is produced.
[0023] As used herein,“spheroidize”,“spheroidization”, and the like refer to increasing the sphericity of a powder, wherein the increase in sphericity may be complete (i.e., producing perfectly spherical particles) or partial. [0024] As used herein,“substantially comprise” or“substantially comprises” 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.
[0025] In some embodiments, an oxygen-containing metallic powder feedstock may have an oxygen content that is too high for use in a particular powder metallurgical process or additive manufacturing process. The maximum allowable oxygen content of a metallic powder may depend on, for example, the particular powder metallurgical process or additive manufacturing process; the composition of the metallic powder; and/or the final
specifications for the part composed of/formed from the powder (e.g., end use application); among others. In some embodiments, an oxygen-containing metallic powder feedstock may need to be de-oxygenated to reduce oxygen content and render it suitable for use in a particular powder metallurgical process and/or additive manufacturing process. A oxygen- containing metallic powder feedstock that is to be used in a particular powder metallurgical process and/or additive manufacturing process may also need to be subjected to a
spheroidization process to increase sphericity of the powder. In the present disclosure, a method and system are provided that can improve metallic feedstock characteristics (e.g., reduce oxygen content/promote de-oxygenation and/or improve sphericity).
[0026] According to the present disclosure, oxygen-containing metallic powder feedstock and reductive metal particles can be brought into contact with (e.g., directed towards via a carrier gas) a plasma to thereby de-oxygenate and spheroidize the oxygen-containing metallic powder feedstock. In some embodiments, the de-oxygenation and spheroidization of the oxygen-containing metallic powder feedstock can occur simultaneously in a single reactor chamber and can form spheroidized metallic particles having reduced oxygen content relative to an oxygen content of the oxygen-containing metallic powder feedstock. During this process, at least a portion of the reductive metal particles can react with the oxygen- containing metallic powder feedstock and form an oxide compound including oxygen derived from the metallic powder. For example, and without limitation, subjecting the reductive metal particles to the plasma in the reactor chamber may generate a reductive metal vapor that reacts with at least oxygen in the metallic powder (e.g., to scavenge excess oxygen from the oxygen-containing metallic powder feedstock) and produces an oxide compound. [0027] Various oxygen-containing metallic powder feedstocks can be processed using the method and system of the present disclosure. For example, and without limitation, the metallic powder can comprise at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles, zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles. In various embodiments, the oxygen-containing metallic powder feedstock can comprise at least one of titanium and titanium alloy particles, for example, particles of 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. In various embodiments, the oxygen-containing metallic powder feedstock can comprise particles of Ti-6Al-4V alloy.
[0028] In various embodiments, the oxygen-containing metallic powder feedstock can have a median particle size of at least 50 nm, such as, for example, at least 1 pm, at least 5 pm, at least 10 pm, at least 15 pm, at least 20 pm, at least 25 pm, at least 30 pm, at least 50 pm, at least 60 pm, at least 65 pm, or at least 105 pm. In various embodiments, the oxygen- containing metallic powder feedstock can have a median particle size no greater than 325 pm, such as, for example, no greater than 300 pm, no greater than 275 pm, no greater than 250 pm, no greater than 225 pm, no greater than 200 pm, no greater than 180 pm, no greater than 175 pm, no greater than 150 pm, no greater than 125 pm, no greater than 100 pm, no greater than 90 pm, no greater than 70 pm, no greater than 65 pm, no greater than 60 pm, no greater than 50 pm, no greater than 45 pm, no greater than 30 pm, no greater than 10 pm, or no greater than 1 pm. In various embodiments, the oxygen-containing metallic powder feedstock can have a median particle size in a range of 50 nm to 325 pm, such as, for example, 1 pm to 325 pm, 5 pm to 325 pm, 10 pm to 100 pm, 105 pm to 180 pm, 20 pm to 50 pm, 60 pm to 90 pm, 50 pm to 100 pm, 10 pm to 150 pm, 15 pm to 45 pm, 20 pm to 65 pm, 25 pm to 45 pm, 50 pm to 150 pm, 65 pm to 90 pm, 10 pm to 200 pm, 5 pm to 30 pm, 30 pm to 90 pm, or 5 pm to 50 pm. [0029] In various embodiments, the oxygen-containing metallic powder feedstock comprises, substantially comprises, or consists essentially of particles having an irregular shape.
Oxygen-containing metallic powder feedstock that has an irregular shape can have particles with an aspect ratio of at least 1.25 such as, for example, at least 2, where the aspect ratio is the largest diameter of a particle divided by the smallest diameter of the particle. For example, a powder that is“irregularly” shaped powder may include at least one sharp edge having an acute exterior angle. Some non-limiting examples of irregularly shaped particles include: globular (non-spherical) powders, plate like powders, and/or acicular (needle shaped powders) to name a few. An irregularly shaped particle may be contrasted with, for example, a substantially spherical particle.
[0030] Various reductive metal particles can be used in the method and system according to the present disclosure. The reductive metal particles can be capable of reacting with at least oxygen in the metallic powder under the conditions in the reactor chamber and thereby reduce oxygen content in the oxygen-containing metallic powder feedstock. For example, the reductive metal particles are configured to be an oxygen scavenger which can remove at least some oxygen from the oxygen-containing metallic powder feedstock. In various
embodiments, the reductive metal particles are configured to be an oxygen scavenger when activated by a plasma.
[0031] In various embodiment, the reductive metal particles can comprise at least one of an alkali metal and an alkaline earth metal. For example, the reductive metal particles can comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium. In various embodiments, the reductive metal particles comprise calcium. In various embodiments, the reductive metal particles can comprise a composite metal compound such as, for example, dicalcium oxygen (e.g., Ca20) or ethyl magnesium bromide (e.g., CFFCFFMgBr)
[0032] In various embodiments, the reductive metal particles can have a median particle size of at least 50 nm, such as, for example, at least 1 pm, at least 5 pm, at least 10 pm, at least 15 pm, at least 20 pm, at least 25 pm, at least 30 pm, at least 50 pm, at least 60 pm, at least 65 pm, at least 105 pm, at least 200 pm, at least 500 pm, or at least lmm. In various
embodiments, the reductive metal particles can have a median particle size of no greater than 2 mm, such as, for example, no greater than 1 mm, no greater than 500 pm, no greater than 325 pm, no greater than 300 pm, no greater than 275 pm, no greater than 250 pm, no greater than 225 mih, no greater than 200 mih, no greater than 180 mih, no greater than 175 mih, no greater than 150 mih, no greater than 125 mih, no greater than 100 mih, no greater than 90 mih, no greater than 70 mih, no greater than 65 mih, no greater than 60 mih, no greater than 50 mih, no greater than 45 mih, no greater than 30 mih, no greater than 10 mih, or no greater than 1 mih. In various embodiments, the reductive metal particles can have a median particle size in a range of 50 nm to 2mm, such as, for example, 1 pm to 2mm, 1 pm to lmm, 100 pm to 1 pm, 1 pm to 325 pm, 5 pm to 325 pm, 10 pm to 100 pm, 105 pm to 180 pm, 20 pm to 50 pm, 60 pm to 90 pm, 50 pm to 100 pm, 10 pm to 150 pm, 15 pm to 45 pm, 20 pm to 65 pm, 25 pm to 45 pm, 50 pm to 150 pm, 65 pm to 90 pm, 10 pm to 200 pm, 5 pm to 30 pm, 30 pm to 90 pm, or 5 pm to 50 pm.
[0033] In some embodiments, the particle size of the reductive metal particle may be chosen/configured in order to control the amount and/or concentration of reductive metal vapor that can be generated in the reactor chamber when the reductive metal particles are subjected to the plasma. As such, the process can thereby be configured such that the plasma process and reductive metal particles are tailored for a particular oxygen-containing metallic powder feedstock (e.g., promoting maximum oxygen removal/oxygen scavenging while not utilizing excess reductive metal particles that may require additional removal steps). In various embodiments, the reductive metal particles can be chosen/configured based on a vaporization temperature of the reductive metal particles and/or the affinity for oxygen of the reductive metal particles. For example, the reductive metal particles can be chosen to have an affinity for oxygen greater than an affinity for oxygen of the oxygen-containing metallic powder feedstock.
[0034] Referring to FIG. 1, a flow chart illustrating a non-limiting embodiment of a method to process oxygen-containing metallic powder feedstock according to the present disclosure is provided. A oxygen-containing metallic powder feedstock and reductive metal particles can be combined in preselected proportions (102) to provide a substantially homogenous blend and/or a comingled mixture. For example, prior to introduction into the reactor, the oxygen-containing metallic powder feedstock and the reductive metal particles can be manually premixed to create a blend, or the oxygen-containing metallic powder feedstock and the reductive metal particles can be mixed in a dynamic in-line mixer. Alternatively, the oxygen-containing metallic powder feedstock and the reductive metallic particles can be fed to the reactor chamber separately and mixed in-situ , in which case steps 102 and 104 in FIG. 1 can occur in tandem or simultaneously. Other techniques for mixing/blending metallic powder and reductive metal particles will be apparent to those ordinarily skilled upon considering the present disclosure.
[0035] In various embodiments, the oxygen-containing metallic powder feedstock and the reductive metal particles can be combined in a weight-to-weight or volume-to-volume ratio of oxygen-containing metallic powder feedstock to reductive metal particles of at least 1 :99 such as, for example, at least 5:95, at least 10:90, at least 20:80, at least 30:70, at least 40:60, at least 50:50, at least 60:40, at least 70:30, at least 80:20, at least 90: 10, or at least 95:5. In various embodiments, the oxygen-containing metallic powder feedstock and the reductive metal particles can be combined in a weight-to-weight or volume-to-volume ratio of oxygen- containing metallic powder feedstock to reductive metal particles no greater than 99: 1 such as, for example, no greater than 95: 1, no greater than 90: 10, no greater than 80:20, no greater than 70:30, no greater than 60:40, no greater than 50:50, no greater than 40:60, no greater than 30:70, no greater than 20:80, no greater than 10:90, or no greater than 5:95. In various embodiments, the oxygen-containing metallic powder feedstock and the reductive metal particles can be combined in a weight-to-weight or volume-to-volume ratio of oxygen- containing metallic powder feedstock to reductive metal particles in a range of 1 : 99 to 99: 1 such as, for example, 5:95 to 95:5, 40:60 to 99: 1, 50:50 to 99: 1, 60:40 to 99: 1, 70:30 to 99: 1, 80:20 to 99: 1, 90: 10 to 99:1, 95: 1 to 99: 1, 40:60 to 95:5, 50:50 to 95:5, 60:40 to 95:5, 70:30 to 95:5, 80:20 to 95:5, or 90: 10 to 95:5. The process can be configured to maximize oxygen removal/oxygen scavenging while not utilizing excess reductive metal particles that may require additional removal steps).
[0036] The oxygen-containing metallic powder feedstock and the reductive metal particles contact plasma in a reactor chamber, producing spheroidized metallic particles from the oxygen-containing metallic powder feedstock (104). In various embodiments, a carrier gas is conducted into the reactor chamber with the oxygen-containing metallic powder feedstock and the reductive metal particles. In some embodiments, the carrier gas is designed to promote movement of the blend of oxygen-containing metallic powder feedstock and reductive metal particles to oxygen-containing metallic powder feedstock and reductant through the process. The carrier gas can comprise, for example, at least one of helium, argon, nitrogen, and hydrogen. In various embodiments, the plasma is produced in the reactor chamber at least partially from the carrier gas. In various embodiments, the plasma is produced in the reactor chamber at least partially from a carrier gas and a second gas. The second gas may be the same or different than the carrier gas. The second gas can be at least one of helium, argon, nitrogen, and hydrogen. The plasma can have an elevated temperature sufficient to at least partially vaporize the reductive metal particles and/or at least partially melt the oxygen-containing metallic powder feedstock.
[0037] In some embodiments, at least a portion of the reductive metal particles can react with at least oxygen in the oxygen-containing metallic powder feedstock and form an oxide compound (106). In various embodiments, the plasma can both at least partially vaporize the reductive metal particles to form reductive metal vapor and at least partially melt the oxygen- containing metallic powder feedstock to form molten metallic powder feedstock. The reductive metal vapor can react with at least oxygen in the molten metallic powder feedstock and form at least one oxide compound, reducing oxygen content of the molten metallic powder. As such, the oxide compound can be a reaction product of the reductive metal vapor and oxygen derived from the molten metallic powder.
[0038] In various embodiments, a temperature of the plasma in the reactor chamber is sufficient to heat the reductive metal particles to at least 700 degrees Celsius such as, for example, at least 800 degrees Celsius, at least 900 degrees Celsius, at least 1000 degrees Celsius, at least 1100 degrees Celsius, at least 1200 degrees Celsius, at least 1300 degrees Celsius, at least 1400 degrees Celsius, at least 1500 degrees Celsius, at least 2000 degrees Celsius, at least 2500 degrees Celsius, or at least 3000 degrees Celsius. In various embodiments, a temperature of the plasma in the reactor chamber is sufficient to heat the reductive metal particles to no greater than 4000 degrees Celsius such as, for example, no greater than 3000 degrees Celsius, no greater than 2500 degrees Celsius, no greater than 2000 degrees Celsius, no greater than 1500 degrees Celsius, no greater than 1400 degrees Celsius, no greater than 1300 degrees Celsius, no greater than 1200 degrees Celsius, no greater than 1100 degrees Celsius, no greater than 1000 degrees Celsius, no greater than 900 degrees Celsius, or no greater than 800 degrees Celsius. In various embodiments, a temperature of the plasma in the reactor chamber is sufficient to heat the reductive metal particles to at least a boiling point temperature of the composition comprising the reductive metal particles. The temperature of plasma and heating of the reductive metal particles can be tailored to/based upon the combination of reductive metal particles and oxygen-containing metallic powder feedstock selected (e.g., to promote melting and/or vaporization but not burn off/consumption of the feedstock).
[0039] In various embodiments, a temperature of the plasma in the reactor chamber is sufficient to heat the oxygen-containing metallic powder feedstock to at least 700 degrees Celsius such as, for example, at least 800 degrees Celsius, at least 900 degrees Celsius, at least 1000 degrees Celsius, at least 1100 degrees Celsius, at least 1200 degrees Celsius, at least 1300 degrees Celsius, at least 1400 degrees Celsius, at least 1500 degrees Celsius, at least 2000 degrees Celsius, at least 2500 degrees Celsius, or at least 3000 degrees Celsius. In various embodiments, a temperature of the plasma in the reactor chamber is sufficient to heat the oxygen-containing metallic powder feedstock to no greater than 4000 degrees Celsius such as, for example, no greater than 3000 degrees Celsius, no greater than 2500 degrees Celsius, no greater than 2000 degrees Celsius, no greater than 1500 degrees Celsius, no greater than 1400 degrees Celsius, no greater than 1300 degrees Celsius, no greater than 1200 degrees Celsius, no greater than 1100 degrees Celsius, no greater than 1000 degrees Celsius, no greater than 900 degrees Celsius, or no greater than 800 degrees Celsius. In various embodiments, a temperature of the plasma in the reactor chamber is sufficient to heat the oxygen-containing metallic powder feedstock to at least a melting point temperature of the composition of the oxygen-containing metallic powder feedstock.
[0040] The contact time between the reductive metal particles and the oxygen-containing metallic powder feedstock and the plasma can be selected to at least partially vaporize the reductive metal particles and melt the oxygen-containing metallic powder feedstock. In various embodiments, the contact time between the reductive metal particles and the oxygen- containing metallic powder feedstock and the plasma can be at least 10 milliseconds (ms), such as, for example, at least 50 ms, at least 100 ms, or at least 500 ms. In various embodiments, the contact time between the reductive metal particles and the oxygen- containing metallic powder feedstock and the plasma can be no greater than 1 second (s), such as, for example, no greater than 500 ms, no greater than 100 ms, or no greater than 50 ms. In various embodiments, the contact time between the reductive metal particles and the oxygen-containing metallic powder feedstock and the plasma can be in a range of 10 ms to 1 s such as, for example, 50ms to 500ms.
[0041] In various embodiments of the method and system of the present disclosure, the melting of the oxygen-containing metallic powder feedstock in the reactor chamber can increase sphericity of (i.e., spheroidize) the oxygen-containing metallic powder feedstock.
For example, melted metallic powder in the reactor chamber may form molten spherical droplets that are cooled in the controlled environment of the reactor chamber and form dense spherical powder (e.g., metallic feedstock powder having improved (lowered) oxygen content and/or improved morphology; for example, the resulting density of the dense spherical powder is increased and/or the resulting packing density is improved as compared to the initial, oxygen-containing metallic feedstock powder). In various embodiments of the present method and system, the oxygen-containing metallic powder feedstock is simultaneously de- oxygenated and spheroidized in a single process when contacting the hot plasma in the reactor chamber, resulting in spheroidized metallic particles having a reduced oxygen content as compared with an oxygen content of the metallic powder prior to contacting the plasma.
[0042] In various embodiments, the oxide compound can be at least one of an alkali metal oxide and an alkaline earth metal oxide. For example, the oxide compound can comprise at least one of lithium oxide, sodium oxide, potassium oxide, beryllium oxide, magnesium oxide, calcium oxide, strontium oxide, and barium oxide. In various embodiments, the reductive metal particles can comprise calcium oxide. In various embodiments, the oxide compound has a median particle size that is within a range of 0.01 % to 100 % of the median particle size of the reductive metal particles such as, for example, 10 % to 90 % or 20% to 80%. In various embodiments, the oxide compound has a median particle size that is at least 0.01 % of the median particle size of the reductive metal particles, such as, for example, at least 10% or at least 20%. In various embodiments, the oxide compound has a median particle size that is no greater than 100 % of the median particle size of the reductive metal particles, such as, for example, no greater than 90% or no greater than 80%. For example, the oxide compound can have a median particle size smaller than the median particle size of the reductive metal particles. In some embodiments, the median particle size of the oxide compound can be based on the amount and/or size of the reductive metal particles that are introduced into the reactor chamber. In some embodiments, the reductive metal particles are tailored such that the resulting oxide compound is configured relative to the oxygen- containing metallic powder feedstock to promote improved mechanical/physical separation processes (e.g., differences in median particle size).
[0043] In various embodiments, the spheroidized and de-oxygenated metallic particles produced in the reactor can comprise a composition similar to the oxygen-containing metallic powder feedstock introduced into the reactor, but the spheroidized and de-oxygenated metallic particles can have a higher sphericity and lower oxygen content than the oxygen- containing metallic powder feedstock. For example, the spheroidized and de-oxygenated metallic particles can comprise at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles. In various embodiments, the spheroidized and de- oxygenated metallic particles 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. In various embodiments, the spheroidized and de-oxygenated metallic particles can comprise Ti-6Al-4V alloy. In various embodiments, the spheroidized and de-oxygenated metallic particles comprise a concentration of no greater than 99% of reductive metal particles and/or the oxide compound based on the total weight of the oxygenated metallic particles, such as, for example, no greater than 5 % by weight of reductive metal particles and/or the oxide compound, no greater than 1 % by weight of reductive metal particles and/or the oxide compound, or no greater than 0.1 % by weight of reductive metal particles and/or the oxide compound, all based on the total weight of the oxygenated metallic particles. In various other embodiments, the spheroidized and de-oxygenated metallic particles do not contain reductive metal particles and/or the oxide compound. In various embodiments, the spheroidized and de-oxygenated metallic particles have a median particle size that at least 50 % of a median particle size of the metallic powder introduced into the reactor chamber such as, for example, at least 55% or at least 60%. In various embodiments, the spheroidized and de-oxygenated metallic particles have a median particle size that is no greater than 100 % of a median particle size of the metallic powder introduced into the reactor chamber such as, for example, no greater than 95% or no greater than 90%. In various embodiments, the spheroidized and de-oxygenated metallic particles have a median particle size that is within a range of 50 % to 100 % of a median particle size of the metallic powder introduced into the reactor chamber such as, for example, 55% to 95% or 60% to 90%. [0044] Through de-oxygenation resulting from reaction of the oxygen-containing metallic powder feedstock and the reductive metal particles in the reactor chamber, the spheroidized and de-oxygenated metallic particles can have a weight percent oxygen content no greater than 95% of the oxygen content of the oxygen-containing metallic powder feedstock such as, for example, no greater than 90%, no greater than 80%, no greater than 70%, no greater than 60%, no greater than 50%, no greater than 40%, no greater than 30%, no greater than 20%, no greater than 10%, no greater than 5%, or no greater than 1% of the oxygen content of the metallic powder. In various embodiments, the spheroidized and de-oxygenated metallic particles can have a sphericity of at least 0.8, such as, for example, at least 0.85 or at least 0.92. Sphericity of particles can be measured utilizing a Camsizer XT with an X-Dry module and an X-Jet cartridge according to equation 1.
[0045] Equation 1
4pA
Sphericity =— p r- wherein A equals measured area of a particle projection and P equals measured
perimeter/circumference of a particle projection. A and P can be measured by capturing images of the particles using a high-resolution video camera in the Camsizer XT. Then the Camsizer XT automatically utilizes image analysis to identify, separate, and trace the edges of particles. Based on the traces, A and P can be determined. As used herein“sphericity” refers to the average sphericity of the particles measured.
[0046] The oxygen contents of the oxygen-containing metallic powder feedstock introduced into the reactor chamber and of the spheroidized and de-oxygenated metallic particles can vary depending on composition of the oxygen-containing metallic powder feedstock. For example, certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising a titanium alloy may include 0.2% to 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.2% by weight, for example, less than 0.16% by weight oxygen.
[0047] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising an aluminum alloy may include 0.2% to 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.20% by weight oxygen, such as, for example, no greater than 0.16% by weight oxygen or no greater than 0.1% by weight oxygen.
[0048] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising a cobalt alloy may include 0.2% to 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.2% by weight oxygen such as, for example, no greater than 0.1% by weight oxygen or no greater than 0.06% by weight oxygen.
[0049] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising a nickel alloy may include 0.05% to 0.5% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.05% by weight oxygen, such as, for example, no greater than 0.015% by weight oxygen or no greater than 0.010% by weight oxygen.
[0050] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising an iron alloy may include 0.1% to 0.5% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.1% by weight oxygen, such as, for example, less than 0.03% by weight oxygen or less than 0.02% by weight oxygen.
[0051] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising a copper alloy may include at least 0.2% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.2% by weight oxygen, such as, for example, no greater than 0.04% by weight oxygen or no greater than 0.02% by weight oxygen.
[0052] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising a tantalum alloy may include at least 1% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 1% by weight oxygen, such as, for example, no greater than 0.2% by weight oxygen or no greater than 0.1% by weight oxygen.
[0053] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising tungsten may include at least 0.3% by weight oxygen, and spheroidized and de- oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.3% by weight oxygen, such as, for example, no greater than 0.05% by weight oxygen or no greater than 0.02% by weight oxygen.
[0054] Certain non-limiting embodiments of oxygen-containing metallic powder feedstock comprising, and in various embodiments consisting of, molybdenum may include at least 0.3% by weight oxygen, and spheroidized and de-oxygenated metallic particles created from that oxygen-containing metallic powder feedstock by the method and system of the present disclosure may comprise less than 0.3% by weight oxygen, such as, for example, no greater than 0.05% by weight oxygen or no greater than 0.02% by weight oxygen.
[0055] The oxygen contents described herein are for illustration purposes only and should not be considered limiting. The desired oxygen content in the spheroidized and de-oxygenated metallic particles can vary depending on, for example, the powder metallurgical process and/or additive manufacturing process in which the metallic particles will be used.
[0056] By combining de-oxygenation and spheroidization together in the reactor, the microstructure of the spheroidized and de-oxygenated metallic particles can be improved.
[0057] With further reference to FIG. 1, in various embodiments, at least a portion of the spheroidized and de-oxygenated metallic particles, and optionally at least a portion of at least one of the oxide compound and any unreacted reductive metal particles can be recycled through a plasma (e.g., passed through the plasma one or more additional times) (108), thereby further reducing an oxygen content in the metallic particles. For example, the spheroidized and de-oxygenated metallic particles can be passed through a plasma a plurality of (i.e., two or more) times. Several passes through a plasma can further reduce the oxygen content of the metallic particles and further promote a spherical shape (e.g., increase sphericity) of metallic particles. The additional passes also can produce additional oxide compound. In various examples, additional reductive metal particles can be combined with the recycled metallic particles that are being recycled, either before or simultaneously with introducing the recycled metallic particles into a reactor chamber to contact a plasma.
[0058] At least a portion of the spheroidized and de-oxygenated metallic particles produced using the method and/or system of the present disclosure can be separated from oxide compound and any unreacted reductive metal particles (110). Separating the particles can be accomplished using mechanical separation equipment including, but not limited to: at least one of a sieve, a settling chamber, and a cyclone. Selecting the median particle size of the reductive metallic particles used in the method/system based on the median particle size of the oxygen-containing metallic powder feedstock used can increase the efficiency of the separation. For example, a median particle size of the reductive metal particles can be selected so that it differs from a median particle size of the oxygen-containing metallic powder feedstock. A difference in median particle size may facilitate separation of the metallic feedstock powder and/or spheroidized and de-oxygenated metallic particles produced therefrom from the reductive metal particles and/or oxide compound produced therefrom.
[0059] In various examples, separating (108) can comprise contacting the spheroidized and de-oxygenated metallic particles with a solvent to thereby dissolve at least a portion of the oxide compound. Thereafter, the solvent and dissolved oxide compound can be removed from the spheroidized and de-oxygenated metallic particles which can result in a product comprising, substantially comprising, or consisting of spheroidized and de-oxygenated metallic particles. The solvent can be any of the various materials known in the art for dissolving an oxide compound. For example, the solvent can comprise at least one of water and an acid. In various embodiments, it may be desirable to select a relatively small median particle size for the reductive metal particles in order to form an oxide compound, and/or to have residual reductive metallic particles, with a small median particle that may facilitate quicker dissolution in a solvent.
[0060] With further reference to FIG. 1, spheroidized and de-oxygenated metallic particles produced by the method and/or system according to the present disclosure can be used to produce a part. For example, the spheroidized and de-oxygenated metallic particles can be used as powder in a powder metallurgy system/process and/or an additive manufacturing system/process and processed into a part 112. In certain applications, at least a portion of spheroidized and de-oxygenated metallic particles made using the present method and/or system can be processed by an additive manufacturing method to produce a part and/or in a coating process, such as, for example, a cold spray process or a plasma spray process.
[0061] Referring to FIG. 2, a schematic representation of a non-limiting embodiment of a system 200 to process oxygen-containing metallic powder feedstock is shown. Reaction chamber 202 is provided with an inlet 204 and an outlet 206. The inlet 204 is adapted to receive an inlet stream comprising oxygen-containing metallic powder feedstock 208 and reductive metal particles 210. The inlet 204 can be adapted to convey the inlet stream into the reactor chamber 202 as a combined inlet stream (including both metallic powder and reductive metal particles) or in separate inlet streams (a first inlet stream conveying oxygen- containing metallic powder feedstock, and a second inlet stream conveying reductive metal particles). In one non-limiting embodiment, the inlet 204 may comprise a first section adapted to receive oxygen-containing metallic powder feedstock 208, a second section adapted to receive reductive metal particles 210, and a dynamic mixer adapted to blend quantities of the oxygen-containing metallic powder feedstock 208 and the reductive metal particles 210 in a preselected weight-to-weight or volume-to-volume ratio, and wherein the blended materials are then passed into the reactor chamber 202. In various embodiments of the system 200, the inlet stream comprises an additional material such as, for example, a carrier gas and a second gas.
[0062] In some embodiment, the reactor chamber 202 is adapted so that spheroidized and de- oxygenated metallic particles 212 and an oxide compound 214 are formed within the reactor chamber 202 from the oxygen-containing metallic powder feedstock 208 and the reductive metal particles 210. For example, the chamber 202 can be configured to include a plasma generator 216 adapted to produce a hot plasma 218, and the oxygen-containing metallic powder feedstock 208 and reductive metal particles 210 can be brought into contact with the plasma 218 in the chamber 202. The plasma 218 can promote at least partial melting of the oxygen-containing metallic powder feedstock 208 to produce molten oxygen-containing metallic powder feedstock 208a, and can also promote at least partial vaporization of the reductive metal particles 210 to form reductive metal vapor 230. The reductive metal vapor 230 can react with at least oxygen in the molten oxygen-containing metallic powder feedstock 208a, thereby reducing oxygen content in the molten oxygen-containing metallic powder feedstock 208a. The reductive metal vapor 230 and oxygen derived from the molten metallic powder 208a can form the oxide compound 214. [0063] In certain embodiments, the reactor chamber 202 operates under conditions that promote spheroidization of the metallic powder 208 in the reactor chamber 202. For example, the reactor chamber 202 can have a pressure of 5 pounds per square inch absolute (psia) to 25 psia to promote spheroidization of the metallic powder 208 in the reactor chamber 202, such as for example, 14 psia to 16 psia. In various embodiments, the reactor chamber 202 has a pressure greater than atmospheric pressure outside of the reactor chamber 202. The spheroidization can, for example, reduce the number of faces, edges, and/or features otherwise out of round in the oxygen-containing metallic powder feedstock 208. In various embodiments, the spheroidization occurring in the reactor chamber 202 increases sphericity of the oxygen-containing metallic powder feedstock 208.
[0064] In some embodiments, an outlet stream comprising spheroidized and de-oxygenated metallic particles 212 and oxide compound 214 formed in the reactor chamber 202, and unreacted reductive metal particles 210, can pass into outlet 206 and can be collected. In certain embodiments of system 200, at least a portion of spheroidized and de-oxygenated metallic particles 212 produced in reactor chamber 202, and optionally at least a portion of unreacted reductive metal particles 210, is recycled by passing the material back into the reactor chamber 202 and contacting the plasma 218. Recycling in this way can further reduce oxygen content and/or further spheroidize the metallic particles 212. In certain embodiments, 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 occurring in the reactor chamber 202.
[0065] The plasma 218 produced in reactor chamber 202 can be generated by any of various plasma generating apparatus or techniques known in the art. For example, plasma 218 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 plasma 218 is generated in one or more of various regions within the chamber 202. In certain embodiments, the plasma 218 is generated so that oxygen-containing metallic powder feedstock 208 introduced into chamber 202 contacts plasma 218 in a manner that facilitates de-oxygenation and
spheroidization of the oxygen-containing metallic powder feedstock 208 to form the spheroidized and de-oxygenated metallic particles 212. For example, the system 200 can be designed so that the plasma 218 is generated axially with respect to the flow of the oxygen- containing metallic powder feedstock 208 through the reactor chamber 202. The plasma 218 can also be positioned within the reactor chamber 202 to enhance the de-oxygenation effect of the plasma 218, so as to reduce oxygen content of oxygen-containing metallic powder feedstock 208 introduced into reactor chamber 202. In various embodiments, the plasma 218 comprises inductively coupled plasma. In other embodiments, the plasma 218 comprises microwave plasma. In various embodiments, the plasma can be a thermal plasma or a non- thermal plasma.
[0066] The plasma 218 can have a temperature suitable to promote at least partial melting of the oxygen-containing metallic powder feedstock 208 and/or at least partial vaporization of the reductive metal particles 210. For example, in various embodiments, an electron temperature of the plasma 218 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, or at least 10,000 K. The electron temperature of the plasma 218 can be in a range of 3,000 K to 12,000 K such as, for example, 4,000 K to 12,000 K, 4,000 K to 10,000 K, 6,000 K to 12,000 K, or 6,000 K to 10,000 K.
The plasma 218 can be at least partially produced from a carrier gas and/or a second gas fed to the system 200 through, for example, the inlet 204.
[0067] A vacuum port 220 can be provided in fluid communication with the reactor chamber 202. The vacuum port 220 can be adapted to convey gases and particulate from the chamber 202. The pressure in the vacuum port 220 can be less than a pressure in the chamber 202 to create a pressure differential which facilitates movement of gases and particulate into the vacuum port 220. The vacuum port 220 can be in fluid communication with a vacuum source 222 such as, for example, a vacuum pump, to create a pressure differential between the vacuum port 220 and the reactor chamber 202. The particulate entering the vacuum port 220 under influence of the pressure differential can substantially comprise the oxide compound 214 and residual reductive metal particles 210. In various embodiments, the particulate entering the vacuum port 220 under influence of the pressure differential can additionally comprise spheroidized and de-oxygenated metallic particles 212.
[0068] The vacuum port 220 can be positioned and oriented in relation to the reactor chamber 202 to limit conveyance of spheroidized and de-oxygenated metallic particles 212 into the vacuum port 220. For example, vacuum port 220 may be positioned on a side wall of the chamber 202 and/or may have an incline. The spheroidized and de-oxygenated metallic particles 212 can have a larger median particle size than a median particle size of the oxide compound 214 and/or residual reductive metal particles 210 such that the larger spheroidized and de-oxygenated metallic particles 212 generally are not drawn into the vacuum port 220. However, trace amounts of spheroidized and de-oxygenated metallic particles 212 still may be drawn into the vacuum port 220.
[0069] In various examples, a filter 224 can be provided in fluid communication with the vacuum port 220 and adapted to separate particulate from gases. After a period of time, the particulate may be removed from the vacuum port 220 by replacing the filter 224 and/or removing the particulate from the filter 224.
[0070] In various embodiments, a size classification module 226 can be provided in fluid communication with the outlet 206. The size classification module 226 can be adapted to receive the outlet stream from the outlet 206 and separate spheroidized and de-oxygenated metallic particles 212 from at least one of residual reductive metal particles 210 and oxide compound 214 in the outlet stream. The size classification module 226 can comprise at least one of a sieve, a settling chamber, and a cyclone. In various embodiments, the size classification module includes a washing module adapted to receive the outlet stream and contact the outlet stream with a solvent suitable to dissolve at least a portion of the oxide compound 214 in the outlet stream. The washing module can remove the solvent and dissolved oxide compound from the spheroidized and de-oxygenated metallic particles 212 and produce a product comprising, substantially comprising, or consisting of spheroidized and de-oxygenated metallic particles 212.
[0071] In various embodiments, a recycle line 228 can be in fluid communication with the outlet 206 and adapted to receive at least a portion of the spheroidized and de-oxygenated metallic particles 212 from the outlet 206. The recycle line 228 can be suitable to output at least a portion of the spheroidized and de-oxygenated metallic particles 212 into the inlet 204, through which the particles are conveyed into the reactor chamber 202 to pass through the plasma 218. The spheroidized and de-oxygenated metallic particles 212 can be recycled into the reactor chamber 202 through recycle line 228 as many times as necessary to remove the desired level of oxygen from and/or further spheroidize the spheroidized and de-oxygenated metallic particles 212.
[0072] The spheroidized and de-oxygenated metallic particles 212 produced utilizing system 200 can be used to produce a part. For example, at least a portion of the spheroidized and de- oxygenated metallic particles 212 can be used as powder in a powder metallurgy system/process such as, for example, an additive manufacturing system/process, and processed into a part. For example, at least a portion of the spheroidized and de-oxygenated metallic particles 212 produced in system 200 can be processed by an additive manufacturing method to produce a part comprising the spheroidized and de-oxygenated metallic particles 212.
[0073] Additive Manufacturing
[0074] The parts described herein may be manufactured via any appropriate additive manufacturing technique described in ASTM G2792- 12a. In one embodiment, an additive manufacturing process includes depositing successive layers of powder and then selectively melting and/or sintering the powder to create, layer-by-layer, a part. In one embodiment, a powder bed is used to create a part such as, for example, a tailored alloy part and/or a unique structure unachievable through traditional manufacturing techniques (e.g., without excessive post-processing machining).
[0075] Non-limiting examples of additive manufacturing processes useful in producing parts from feedstocks include, for example, BJAM, DMLS, SLM, SLS, and EBM, among others. In one embodiment, an additive manufacturing process uses an EOSINT M 280 Direct Metal Laser Sintering (DMLS) additive manufacturing system, or comparable system, available from EOS GmbH (Robert-Stirling-Ring 1, 82152 Krailling/Munich, Germany). Additive manufacturing techniques (e.g., when utilizing metallic feedstocks) may facilitate the selective heating of powder above the liquidus temperature of the powder, thereby forming a molten pool followed by rapid solidification of the molten pool.
[0076] Any suitable feedstocks may be used, including powder, a wire, a sheet, and combinations thereof. In various embodiments, the feedstock may be, for example, metallic feedstocks (e.g., with additives to promote various properties such as, for example, grain refiners and/or ceramic materials), polymeric feedstocks (e.g., plastic feedstocks), and ceramic feedstocks. In certain embodiments, the wire can comprise a ribbon and/or a tube. The metallic feedstocks can be at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy. In certain embodiments, reagent-based feedstock materials which form polymeric parts can be used as feedstock.
[0077] As used herein,“aluminum alloy” means a metal alloy having aluminum as the predominant alloying element. Similar definitions apply to the other corresponding alloys referenced herein (e.g., titanium alloy means a titanium alloy having titanium as the predominant alloying element).
[0078] In one approach, an additive manufacturing process comprises (a) dispersing a feedstock (e.g., powder in a powder bed), (b) selectively heating a portion of the powder (e.g., via an energy source) to a temperature above the liquidus temperature of the powder,
(c) forming a molten pool and (d) cooling the molten pool at a cooling rate of at least l000°C per second, such as, for example, at least l0,000°C per second, at least l00,000°C per second, or at least l,000,000°C per second. Steps (a)-(d) may be repeated as necessary until the additively manufactured part is completed.
[0079] In another approach, an additive manufacturing process comprises (a) dispersing a feedstock (e.g., metallic powder) in a deposition region, (b) selectively binder jetting the feedstock, and (c) repeating steps (a)-(b), thereby producing a final additively manufactured part (e.g., including optionally heating to burn off binder and form a green form, followed by sintering to form the additively manufactured part).
[0080] In another approach, electron beam or plasma arc techniques are utilized to produce at least a portion of the additively manufactured part. Electron beam techniques may facilitate production of larger parts than readily produced via laser additive manufacturing techniques. An illustrative example provides feeding a wire to the wire feeder portion of an electron beam gun. The wire may comprise a metallic feedstock. The electron beam heats the wire above the liquidus point of the metallic feedstock and deposits the molten pool in a deposition region. Thereafter, rapid solidification of the molten pool to form the deposited material occurs.
[0081] Production and Processing
[0082] In some embodiments, the additively manufactured part may be subject to any appropriate dissolving (e.g., includes homogenization), working and/or precipitation hardening steps. If employed, the dissolving and/or the working steps may be conducted on an intermediate form of the additively manufactured part and/or may be conducted on a final form of the additively manufactured part. If employed, the precipitation hardening step is generally conducted relative to the final form of the additively manufactured part.
[0083] After or during production, an additively manufactured part may be deformed (e.g., by one or more of rolling, extruding, forging, stretching, compressing). The final deformed product may realize, for instance, improved properties due to the tailored regions and thermo- mechanical processing of the final deformed part. Thus, in some embodiments, the final part is a wrought part, the word“wrought” referring to the working (hot working and/or cold working) of the additively manufactured part, wherein the working occurs relative to an intermediate and/or final form of the additively manufactured part. In other approaches, the final part is a non-wrought product, i.e., is not worked during or after the additive
manufacturing process. In these non-wrought product embodiments, any appropriate number of dissolving and precipitating steps may still be utilized.
[0084] Product Applications
[0085] The resulting additively manufactured parts made in accordance with the systems and methods described herein may be used in a variety of product applications such as, commercial end-uses in industrial applications, in consumer applications (e.g., consumer electronics and/or appliances), or in other areas. For example, the additively manufactured parts can be utilized in at least one of the aerospace field (e.g., aerospace component), automotive field (e.g., automotive component), transportation field (e.g., transportation component), or building and construction field (e.g., building component or construction component). In certain embodiments, the additively manufactured parts can be configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component.
[0086] In one embodiment, an additively manufactured part can be utilized in an elevated temperature application, such as in an aerospace or automotive vehicle. In one embodiment, an additively manufactured part can be utilized as an engine component in an aerospace vehicle (e.g., in the form of a blade, such as a compressor blade incorporated into the engine). In another embodiment, an additively manufactured part can be used as a heat exchanger for the engine of the aerospace vehicle. The aerospace vehicle including the engine component / heat exchanger may subsequently be operated. In one embodiment, an additively manufactured part can be an automotive engine component. The automotive vehicle including an automotive component (e.g., engine component) may subsequently be operated. For instance, the additively manufactured part may be used as a turbo charger component (e.g., a compressor wheel of a turbo charger, where elevated temperatures may be realized due to recycling engine exhaust back through the turbo charger), and the automotive vehicle including the turbo charger component may be operated. In another embodiment, an additively manufactured part may be used as a blade in a land based (stationary) turbine for electrical power generation, and the land-based turbine included the additively manufactured part may be operated to facilitate electrical power generation. In some embodiments, an additively manufactured part can be utilized in defense applications, such as in body armor, and armed vehicles (e.g., armor plating). In other embodiments, the additively manufactured part can be utilized in consumer electronic applications, such as in consumer electronics, such as, laptop computer cases, battery cases, cell phones, cameras, mobile music players, handheld devices, computers, televisions, microwaves, cookware, washers/dryers, refrigerators, and sporting goods, among others.
[0087] In another aspect, an additively manufactured part can be utilized in a structural application, such as, for example, an aerospace structural application and an automotive structural application. For instance, the additively manufactured part may be formed into various aerospace structural components, including floor beams, seat rails, fuselage framing, bulkheads, spars, ribs, longerons, and brackets, among others. In another embodiment, the additively manufactured part can be utilized in an automotive structural application. For instance, the additively manufactured part can be formed into various automotive structural components including nodes of space frames, shock towers, and subframes, among others. In one embodiment, the additively manufactured part can be a body -in-white automotive product.
[0088] In another aspect, the additively manufactured part can be utilized in an industrial engineering application. For instance, the additively manufactured part or products may be formed into various industrial engineering products, such as tread-plate, tool boxes, bolting decks, bridge decks, and ramps, among others.
[0089] Various aspects of the invention according to the present disclosure include, but are not limited to, the aspects listed in the following numbered clauses. A method comprising:
passing an oxygen-containing metallic powder feedstock and reductive metal particles through a plasma to thereby de-oxygenate and spheroidize the oxygen- containing metallic powder feedstock and produce spheroidized and de-oxygenated metallic particles;
wherein at least a portion of the reductive metal particles react with the oxygen-containing metallic powder feedstock and form an oxide compound. The method of clause 1, wherein a weight percentage oxygen content of the spheroidized and de-oxygenated metallic particles is no greater than 95 percent a weight percentage oxygen content of the oxygen-containing metallic powder feedstock. The method of any one of clauses 1 to 2, wherein the spheroidized and de-oxygenated metallic particles comprise a sphericity of at least 0.8. The method of any one of clauses 1 to 3, wherein the reductive metal particles comprise at least one of an alkali metal and an alkaline earth metal. The method of any one of clauses 1 to 4, wherein the reductive metal particles comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium. The method of any one of clauses 1 to 5, wherein the reductive metal particles comprise a median particle size in a range of 50 nm to 2mm. The method of any one of clauses 1 to 6, wherein the reductive metal particles comprise a median particle size different than a median particle size of the oxygen- containing metallic powder feedstock. The method of any one of clauses 1 to 7, further comprising:
separating at least a portion of the spheroidized and de-oxygenated metallic particles from the oxide compound and any unreacted reductive metal particles. The method of clause 8, wherein the separating comprises utilizing at least one of a sieve, a settling chamber, and a cyclone. The method of any one of clauses 1 to 9, further comprising:
contacting the spheroidized and de-oxygenated metallic particles with a solvent to thereby dissolve at least a portion of the oxide compound. The method of clause 10, wherein the solvent comprises at least one of water and an acid. The method of any one of clauses 1 to 11, wherein the oxygen-containing metallic powder feedstock has a median particle size in a range of 50 nm to 325 pm. The method of any one of clauses 1 to 12, wherein the oxygen-containing metallic powder feedstock comprises an irregular shape. The method of any one of clauses 1 to 13, wherein the oxygen-containing metallic powder feedstock comprises at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles. The method of any one of clauses 1 to 14, wherein the oxygen-containing metallic powder feedstock comprises a Ti-6Al-4V alloy and the reductive metal particles comprise calcium. The method of any one of clauses 1 to 15, wherein the oxygen-containing metallic powder feedstock and the reductive metal particles are passed through the plasma in a weight-to-weight or volume -to-volume ratio of oxygen-containing metallic powder feedstock to reductive metal particles in a range of 1 :99 to 99: 1. The method of any one of clauses 1 to 16, further comprising passing a carrier gas through the plasma, the carrier gas comprising at least one of helium, argon, nitrogen, and hydrogen. The method of clause 17, wherein the plasma is at least partially produced from the carrier gas. The method of any one of clauses 1 to 18, wherein a temperature of the plasma is sufficient to at least partially vaporize the reductive metal particles. The method of any one of clauses 1 to 19, wherein a temperature of the plasma is sufficient to at least partially melt the oxygen-containing metallic powder feedstock. The method of any one of clauses 1 to 20, wherein:
the plasma at least partially vaporizes the reductive metal particles and at least partially melts the oxygen-containing metallic powder feedstock; and
the vaporized reductive metal particles and the melted metallic powder feedstock react to form products comprising the spheroidized and de-oxygenated metallic particles and the oxide compound. The method of any one of clauses 1 to 21, wherein the reductive metal particles are heated to at least 700 degrees Celsius by the plasma. The method of any one of clauses 1 to 22, further comprising recycling at least a portion of the spheroidized and de-oxygenated metallic particles and additional reductive metal particles through the plasma, thereby reducing an oxygen content in the spheroidized and de-oxygenated metallic particles and producing additional oxide compound. The method of any one of clauses 1 to 23, further comprising processing at least a portion of the spheroidized and de-oxygenated metallic particles by an additive manufacturing method to produce a part comprising the spheroidized and de- oxygenated metallic particles. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a titanium alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises an aluminum alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a cobalt alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a nickel alloy and a weight percentage oxygen content in a range of 0.05 percent by weight oxygen to 0.5 percent by weight oxygen and the
spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.05 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises an iron alloy and a weight percentage oxygen content in a range of 0.1 percent by weight oxygen to 0.5 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.1 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a copper alloy and a weight percentage oxygen content of at least 0.2 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a tantalum alloy and a weight percentage oxygen content of at least 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 1 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a tungsten alloy and a weight percentage oxygen content of at least 0.3 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.3 percent by weight oxygen. The method of any one of clauses 1 to 24, the oxygen-containing metallic powder feedstock comprises a molybdenum alloy and a weight percentage oxygen content of at least 0.3 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.3 percent by weight oxygen. Spheroidized and de-oxygenated metallic particles produced by the method according to any one of clauses 1 to 33. The spheroidized and de-oxygenated metallic particles of clause 34, wherein the particles are selected from the group comprising titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles. The spheroidized and de-oxygenated metallic particles of any one of clauses 34 to 35, wherein the particles are Ti-6Al-4V particles. A part produced by an additive manufacturing system or method utilizing the spheroidized and de-oxygenated metallic particles made by the method of any one of clauses 1 to 33. The part of clause 37, wherein the part comprises at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy. The part of any one of clauses 37 to 38, wherein the part comprises Ti-6Al-4V alloy. The part of any one of clauses 37 to 39, wherein the part is configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component. A powder processing system comprising:
an inlet in fluid communication with a reactor chamber;
a plasma generator in communication with the reactor chamber and adapted to generate a plasma in the reactor chamber; and
an outlet in fluid communication with the reactor chamber;
wherein the inlet is adapted to receive an inlet stream comprising an oxygen- containing metallic powder feedstock and reductive metal particles and convey the inlet stream to the reactor chamber;
wherein the reactor chamber is adapted to receive the inlet stream and contact the inlet stream with the plasma, thereby de-oxygenating and spheroidizing the oxygen-containing metallic powder feedstock and producing reaction products comprising spheroidized and de-oxygenated metallic particles and an oxide compound; and
wherein the outlet is adapted to receive an outlet stream from the reactor chamber comprising the spheroidized and de-oxygenated metallic particles. The system of clause 41, further comprising:
a vacuum port in fluid communication with the reactor chamber, the vacuum port adapted to convey gases and particulate from the reactor, the particulate substantially comprising the oxide compound and residual reductive metal particles. The system of clause 42, further comprising a filter in fluid communication with the vacuum port and adapted to separate the particulate from the gases. The system of any one of clauses 41 to 43, wherein the inlet comprises a first section adapted to receive the oxygen-containing metallic powder feedstock, a second section adapted to receive the reductive metal particles, and a dynamic mixer adapted to blend quantities of the oxygen-containing metallic powder feedstock and the reductive metal particles in a preselected weight-to-weight or volume-to-volume ratio. The system of any one of clauses 41 to 44, wherein a weight percentage oxygen content of the spheroidized and de-oxygenated metallic particles is no greater than 95 percent a weight percentage oxygen content of the oxygen-containing metallic powder feedstock. The system of any one of clauses 41 to 45, wherein the spheroidized and de- oxygenated metallic particles comprise a sphericity of at least 0.8. The system of any one of clauses 41 to 46, wherein the reductive metal particles comprise at least one of an alkali metal and an alkaline earth metal. The system of any one of clauses 41 to 47, wherein the reductive metal particles comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium. The system of any one of clauses 41 to 48, wherein the reductive metal particles comprise a median particle size in a range of 50 nm to 2mm. The system of any one of clauses 41 to 49, wherein the reductive metal particles have a median particle size different than a median particle size of the oxygen-containing metallic powder feedstock. The system of any one of clauses 41 to 50, further comprising:
a size classification module in fluid communication with the outlet, the size classification module adapted to receive the outlet stream from the outlet and separate the spheroidized and de-oxygenated metallic particles from at least one of residual reductive metal particles and the oxide compound in the outlet stream. The system of clause 51, wherein the size classification module comprises at least one of a sieve, a settling chamber, and a cyclone. The system of any one of clauses 41 to 52, further comprising:
a washing module in communication with the outlet, the washing module adapted to receive the outlet stream and contact the outlet stream with a solvent suitable to dissolve at least a portion of the oxide compound. The system of claim 53, wherein the solvent comprises at least one of water and an acid. The system of any one of clauses 41 to 54, wherein the oxygen-containing metallic powder feedstock has a median particle size in the range of 50 nm to 325 pm. The system of any one of clauses 41 to 55, wherein the metallic powder has an irregular shape. The system of any one of clauses 41 to 56, wherein the metallic powder comprises at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles. The system of any one of clauses 41 to 57, wherein the metallic powder comprises Ti- 6A1-4V alloy and the reductive metal particles comprise calcium. The system of any one of clauses 41 to 58, wherein the inlet stream further comprises a carrier gas comprising at least one of helium, argon, nitrogen, and hydrogen. The system of any one of clauses 41 to 59, wherein the plasma has a temperature sufficient to at least one of at least partially vaporize the reductive metal particles, and at least partially melt the oxygen-containing metallic powder feedstock. The system of any one of clauses 41 to 60, wherein the plasma has an electron temperature of at least 700 degrees Celsius. 62. The system of any one of clauses 41 to 61, further comprising:
a recycle line in communication with the outlet and the inlet, the recycle line adapted to receive at least a portion of the spheroidized and de-oxygenated metallic particles from the outlet and transport the at least a portion of the spheroidized and de- oxygenated metallic particles to the inlet.
63. The system of any one of clauses 41 to 62, further comprising an additive
manufacturing system suitable to utilize at least a portion of the spheroidized and de- oxygenated metallic particles to produce a part.
64. Spheroidized and de-oxygenated metallic particles produced by the system according to any one of clauses 41 to 63.
65. A part produced by an additive manufacturing system or method utilizing the
spheroidized and de-oxygenated metallic particles made by the system of any one of clauses 41 to 63.
66. The part of clause 65, wherein the part comprises at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy.
67. The part of any one of clauses 65 to 66, wherein the part comprises Ti-6Al-4V alloy.
68. The part of any one of clauses 65 to 67, wherein the part is configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component.
[0090] One skilled in the art will recognize that the herein described methods, systems, components, devices, operations/actions, and objects, and the discussion accompanying them, are used as examples for the sake of conceptual clarity and that various configuration modifications are contemplated. Consequently, as used herein, the specific
examples/embodiments set forth and the accompanying discussion are intended to be representative of their more general classes. In general, use of any specific exemplar is intended to be representative of its class, and the non-inclusion of specific components, devices, operations/actions, and objects should not be taken limiting. While the present disclosure provides descriptions of various specific aspects for the purpose of illustrating various aspects of the present disclosure and/or its potential applications, it is understood that variations and modifications will occur to those skilled in the art. Accordingly, the invention or inventions described herein should be understood to be at least as broad as they are claimed and not as more narrowly defined by particular illustrative aspects provided herein.

Claims

CLAIMS What is claimed is:
1. A method comprising:
passing an oxygen-containing oxygen-containing metallic powder feedstock and reductive metal particles through a plasma to thereby de-oxygenate and spheroidize the oxygen-containing metallic powder feedstock and produce
spheroidized and de-oxygenated metallic particles;
wherein at least a portion of the reductive metal particles react with at least oxygen in the oxygen-containing metallic powder feedstock and form an oxide compound.
2. The method of claim 1, wherein a weight percentage oxygen content of the
spheroidized and de-oxygenated metallic particles is no greater than 95 percent a weight percentage oxygen content of the oxygen-containing metallic powder feedstock.
3. The method of any one of claims 1-2, wherein the spheroidized and de-oxygenated metallic particles comprise a sphericity of at least 0.8.
4. The method of any one of claims 1-3, wherein the reductive metal particles comprise at least one of an alkali metal and an alkaline earth metal.
5. The method of any one of claims 1-4, wherein the reductive metal particles comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium.
6. The method of any one of claims 1-5, wherein the reductive metal particles comprise a median particle size in a range of 50 nm to 2mm.
7. The method of any one of claims 1-6, wherein the reductive metal particles comprise a median particle size different than a median particle size of the oxygen-containing metallic powder feedstock.
8. The method of any one of claims 1-7, further comprising:
separating at least a portion of the spheroidized and de-oxygenated metallic particles from the oxide compound and any unreacted reductive metal particles.
9. The method of claim 8, wherein the separating comprises utilizing at least one of a sieve, a settling chamber, and a cyclone.
10. The method of any one of claims 1-9, further comprising:
contacting the spheroidized and de-oxygenated metallic particles with a solvent to thereby dissolve at least a portion of the oxide compound.
11. The method of claim 10, wherein the solvent comprises at least one of water and an acid.
12. The method of any one of claims 1-11, wherein the oxygen-containing metallic
powder feedstock has a median particle size in a range of 50 nm to 325 pm.
13. The method of any one of claims 1-12, wherein the oxygen-containing metallic
powder feedstock comprises an irregular shape.
14. The method of any one of claims 1-13, wherein the oxygen-containing metallic
powder feedstock comprises at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
15. The method of any one of claims 1-14, wherein the oxygen-containing metallic
powder feedstock comprises Ti-6Al-4V alloy and the reductive metal particles comprise calcium.
16. The method of any one of claims 1-15, wherein the oxygen-containing metallic
powder feedstock and the reductive metal particles are passed through the plasma in a ratio of oxygen-containing metallic powder feedstock to reductive metal particles in a range of 1 :99 to 99: 1.
17. The method of any one of claims 1-16, further comprising passing a carrier gas through the plasma, the carrier gas comprising at least one of helium, argon, nitrogen, and hydrogen.
18. The method of claim 17, wherein the plasma is produced at least partially from the carrier gas.
19. The method of any one of claims 1-18, wherein a temperature of the plasma is
sufficient to at least partially vaporize the reductive metal particles.
20. The method of any one of claims 1-19, wherein a temperature of the plasma is
sufficient to at least partially melt the oxygen-containing metallic powder feedstock.
21. The method of any one of claims 1-20, wherein:
the plasma at least partially vaporizes the reductive metal particles and at least partially melts the oxygen-containing metallic powder feedstock; and
the vaporized reductive metal particles and the melted metallic powder feedstock react to form products comprising the spheroidized and de-oxygenated metallic particles and the oxide compound.
22. The method of any one of claims 1-21, wherein the reductive metal particles are
heated to at least 700 degrees Celsius by the plasma.
23. The method of any one of claims 1-22, further comprising recycling at least a portion of the spheroidized and de-oxygenated metallic particles and additional reductive metal particles through the plasma, thereby reducing an oxygen content in the spheroidized and de-oxygenated metallic particles and producing additional oxide compound.
24. The method of any one of claims 1-23, further comprising processing at least a
portion of the spheroidized and de-oxygenated metallic particles by an additive manufacturing method to produce a part comprising the spheroidized and de- oxygenated metallic particles.
25. The method of any one of claims 1-24, the oxygen-containing metallic powder
feedstock comprises a titanium alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
26. The method of any one of claims 1-25, the oxygen-containing metallic powder
feedstock comprises an aluminum alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
27. The method of any one of claims 1-26, the oxygen-containing metallic powder
feedstock comprises a cobalt alloy and a weight percentage oxygen content in a range of 0.2 percent by weight oxygen to 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
28. The method of any one of claims 1-27, the oxygen-containing metallic powder
feedstock comprises a nickel alloy and a weight percentage oxygen content in a range of 0.05 percent by weight oxygen to 0.5 percent by weight oxygen and the
spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.05 percent by weight oxygen.
29. The method of any one of claims 1-28, the oxygen-containing metallic powder
feedstock comprises an iron alloy and a weight percentage oxygen content in a range of 0.1 percent by weight oxygen to 0.5 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.1 percent by weight oxygen.
30. The method of any one of claims 1-29, the oxygen-containing metallic powder
feedstock comprises a copper alloy and a weight percentage oxygen content of at least 0.2 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.2 percent by weight oxygen.
31. The method of any one of claims 1-30, the oxygen-containing metallic powder
feedstock comprises a tantalum alloy and a weight percentage oxygen content of at least 1 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 1 percent by weight oxygen.
32. The method of any one of claims 1-31, the oxygen-containing metallic powder
feedstock comprises a tungsten alloy and a weight percentage oxygen content of at least 0.3 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.3 percent by weight oxygen.
33. The method of any one of claims 1-32, the oxygen-containing metallic powder
feedstock comprises a molybdenum alloy and a weight percentage oxygen content of at least 0.3 percent by weight oxygen and the spheroidized and de-oxygenated metallic particles comprise a weight percentage oxygen content of less than 0.3 percent by weight oxygen.
34. Spheroidized and de-oxygenated metallic particles produced by the method according to any one of claims 1-33.
35. The spheroidized and de-oxygenated metallic particles of claim 34, wherein the
particles are selected form the group comprising titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
36. The spheroidized and de-oxygenated metallic particles of any one of claims 34-35, wherein the particles are Ti-6Al-4V particles.
37. A part produced by an additive manufacturing system or method utilizing the
spheroidized and de-oxygenated metallic particles made by the method of any one of claims 1-33.
38. The part of claim 37, wherein the part comprises at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy.
39. The part of any one of claims 37-38, wherein the part comprises Ti-6Al-4V alloy.
40. The part of any one of claims 37-39, wherein the part is configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component.
41. A powder processing system comprising:
an inlet in fluid communication with a reactor chamber;
a plasma generator in communication with the reactor chamber and adapted to generate a plasma in the reactor chamber; and
an outlet in fluid communication with the reactor chamber;
wherein the inlet is adapted to receive an inlet stream comprising an oxygen- containing oxygen-containing metallic powder feedstock and reductive metal particles and convey the inlet stream to the reactor chamber;
wherein the reactor chamber is adapted to receive the inlet stream and contact the inlet stream with the plasma, thereby de-oxygenating and spheroidizing the oxygen-containing metallic powder feedstock and producing reaction products comprising spheroidized and de-oxygenated metallic particles and an oxide compound; and
wherein the outlet is adapted to receive an outlet stream from the reactor chamber comprising the spheroidized and de-oxygenated metallic particles.
42. The system of claim 41, further comprising:
a vacuum port in fluid communication with the reactor chamber, the vacuum port adapted to convey gases and particulate from the reactor, the particulate substantially comprising the oxide compound and residual reductive metal particles.
43. The system of claim 42, further comprising a filter in fluid communication with the vacuum port and adapted to separate the particulate from the gases.
44. The system of any one of claims 41-43, wherein the inlet comprises a first section adapted to receive the oxygen-containing metallic powder feedstock, a second section adapted to receive the reductive metal particles, and a dynamic mixer adapted to blend quantities of the oxygen-containing metallic powder feedstock and the reductive metal particles in a preselected ratio.
45. The system of any one of claims 41-44, wherein a weight percentage oxygen content in the spheroidized and de-oxygenated metallic particles is no greater than 95 percent a weight percentage oxygen content of the oxygen-containing metallic powder feedstock.
46. The system of any one of claims 41-45, wherein the spheroidized and de-oxygenated metallic particles comprise a sphericity of at least 0.8.
47. The system of any one of claims 41-46, wherein the reductive metal particles
comprise at least one of an alkali metal and an alkaline earth metal.
48. The system of any one of claims 41-47, wherein the reductive metal particles
comprise at least one of lithium, sodium, potassium, beryllium, magnesium, calcium, strontium, and barium.
49. The system of any one of claims 41-48, wherein the reductive metal particles
comprise a median particle size in a range of 50 nm to 2mm.
50. The system of any one of claims 41-49, wherein the reductive metal particles have a median particle size different than a median particle size of the oxygen-containing metallic powder feedstock.
51. The system of any one of claims 41-50, further comprising:
a size classification module in fluid communication with the outlet, the size classification module adapted to receive the outlet stream from the outlet and separate the spheroidized and de-oxygenated metallic particles from at least one of residual reductive metal particles and the oxide compound in the outlet stream.
52. The system of claim 51, wherein the size classification module comprises at least one of a sieve, a settling chamber, and a cyclone.
53. The system of any one of claims 41-52, further comprising:
a washing module in communication with the outlet, the washing module adapted to receive the outlet stream and contact the outlet stream with a solvent suitable to dissolve at least a portion of the oxide compound.
54. The system of claim 53, wherein the solvent comprises at least one of water and an acid.
55. The system of any one of claims 41-54, wherein the oxygen-containing metallic
powder feedstock has a median particle size in the range of 50 nm to 325 pm.
56. The system of any one of claims 41-55, wherein the oxygen-containing metallic
powder feedstock has an irregular shape.
57. The system of any one of claims 41-56, wherein the oxygen-containing metallic
powder feedstock comprises at least one of titanium particles, titanium alloy particles, aluminum particles, aluminum alloy particles, nickel particles, nickel alloy particles, iron particles, iron alloy particles, cobalt particles, cobalt alloy particles, copper particles, copper alloy particles, molybdenum particles, molybdenum alloy particles, magnesium particles, magnesium alloy particles, tantalum particles, tantalum alloy particles, tungsten particles, tungsten alloy particles , zinc particles, zinc alloy particles, silver particles, silver alloy particles, chromium particles, chromium alloy particles, tin particles, tin alloy particles, gold particles, gold alloy particles, platinum particles, platinum alloy particles, zirconium particles, and zirconium alloy particles.
58. The system of any one of claims 41-57, wherein the oxygen-containing metallic
powder feedstock comprises Ti-6Al-4V alloy and the reductive metal particles comprise calcium.
59. The system of any one of claims 41-58, wherein the inlet stream further comprises a carrier gas comprising at least one of helium, argon, nitrogen, and hydrogen.
60. The system of any one of claims 41-59, wherein the plasma has a temperature
sufficient to at least one of at least partially vaporize the reductive metal particles and at least partially melt the oxygen-containing metallic powder feedstock.
61. The system of any one of claims 41-60, wherein the plasma has an electron temperature of at least 700 degrees Celsius.
62. The system of any one of claims 41-61, further comprising:
a recycle line in communication with the outlet and the inlet, the recycle line adapted to receive at least a portion of the spheroidized and de-oxygenated metallic particles from the outlet and transport the at least a portion of the spheroidized and de- oxygenated metallic particles to the inlet.
63. The system of any one of claims 41-62, further comprising an additive manufacturing system suitable to utilize at least a portion of the spheroidized and de-oxygenated metallic particles to produce a part.
64. Spheroidized and de-oxygenated metallic particles produced by the system according to any one of claims 41-63.
65. A part produced by an additive manufacturing system or method utilizing the
spheroidized and de-oxygenated metallic particles made by the system of any one of claims 41-63.
66. The part of claim 65, wherein the part comprises at least one of titanium, titanium alloy, aluminum, aluminum alloy, nickel, nickel alloy, iron, iron alloy, cobalt, cobalt alloy, copper, copper alloy, molybdenum, molybdenum alloy, magnesium, magnesium alloy, tantalum, tantalum alloy, tungsten, tungsten alloy, zinc, zinc alloy, silver, silver alloy, chromium, chromium alloy, tin, tin alloy, gold, gold alloy, platinum, platinum alloy, zirconium, and zirconium alloy.
67. The part of any one of claims 65-66, wherein the part comprises Ti-6Al-4V alloy.
68. The part of any one of claims 65-67, wherein the part is configured as at least one of an aerospace component, an automotive component, a transportation component, and a building and construction component.
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