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WO2023115119A1 - Procédé de production d'une poudre métallique compactable à froid - Google Patents

Procédé de production d'une poudre métallique compactable à froid Download PDF

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Publication number
WO2023115119A1
WO2023115119A1 PCT/AU2022/051541 AU2022051541W WO2023115119A1 WO 2023115119 A1 WO2023115119 A1 WO 2023115119A1 AU 2022051541 W AU2022051541 W AU 2022051541W WO 2023115119 A1 WO2023115119 A1 WO 2023115119A1
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WIPO (PCT)
Prior art keywords
particles
powder
metal particles
metallic
metallic powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/AU2022/051541
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English (en)
Inventor
Robert Wilson
Shiqin Yan
Kun Yang
Ling Chen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Commonwealth Scientific and Industrial Research Organization CSIRO
Original Assignee
Commonwealth Scientific and Industrial Research Organization CSIRO
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Filing date
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Priority claimed from AU2021904141A external-priority patent/AU2021904141A0/en
Application filed by Commonwealth Scientific and Industrial Research Organization CSIRO filed Critical Commonwealth Scientific and Industrial Research Organization CSIRO
Priority to AU2022420976A priority Critical patent/AU2022420976A1/en
Priority to EP22908881.0A priority patent/EP4444492A4/fr
Priority to JP2024537360A priority patent/JP2025501551A/ja
Priority to CN202280091388.3A priority patent/CN118647475A/zh
Priority to CA3241509A priority patent/CA3241509A1/fr
Priority to KR1020247024379A priority patent/KR20240128028A/ko
Priority to US18/722,512 priority patent/US20250144706A1/en
Publication of WO2023115119A1 publication Critical patent/WO2023115119A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/068—Flake-like particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/09—Mixtures of metallic powders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only
    • C23C24/04—Impact or kinetic deposition of particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/10—Inert gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B22F2301/205—Titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only

Definitions

  • the invention relates to a method of producing a cold compactible metallic powder by combining a first metallic powder comprising large metal particles and a second metallic powder comprising small metal particles to provide a precursor powder, and impact blending the combined powder to adhere the small metal particles to the large particles, thereby producing a cold compactible metallic powder comprising non- spherical particles.
  • the non-spherical particles comprise one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core.
  • the invention also relates to a method of producing a porous metallic article by subjecting the cold compactible metallic powder to a cold compaction process at a pressure sufficient to consolidate the cold compactible metallic powder.
  • Cold compaction of metallic powders provides significant benefits over traditional hot working techniques in various metallurgical manufacturing processes.
  • Such cold compaction methods have in common that the metallic powder is consolidated under pressure, with or without a binder, at temperatures below the sintering temperature, to produce a porous metal object (a compact) with sufficient structural integrity to withstand further processing via sintering or other techniques to produce a final metal product.
  • the inventors have now discovered that the cold compaction properties of a metallic powder may be improved by combining that powder with a second metallic powder composed of smaller sized particles, and subjecting the combined powder to an impact blending process.
  • the small particles (of the second metallic powder) adhere to the surface of the larger particles (of the first metallic powder), producing non-spherical particles having one large metal particle as a core and a plurality of the small metal particles as protrusions from the core.
  • Non-spherical particles having this “core-corona” type morphology can be consolidated in a cold compaction process to form compacts with desirable mechanical properties (e.g. high strength) or can be successfully consolidated to form a compact at significantly reduced pressures compared to the unmodified starting material.
  • desirable mechanical properties e.g. high strength
  • certain metal powder feedstocks not otherwise suitable for cold compaction can be upgraded to become desirable feedstocks for binderless cold compaction processes by the methods of the present disclosure.
  • the protrusions of the non-spherical particles facilitate particle interlocking during the compaction and increase the contact area at the interface between adjacent particles in the compact. Thus, compacts with excellent mechanical properties are obtained.
  • the methods disclosed herein are particularly useful for upgrading powders of high yield strength metallic compositions and/or relatively spheroidal particle morphologies, which are otherwise difficult to cold compact.
  • the invention provides a method of producing a cold compactible metallic powder, the method comprising: providing (i) a first metallic powder comprising large metal particles and (ii) a second metallic powder comprising small metal particles, wherein the d50 particle size of the second metallic powder is less than the d50 particle size of the first metallic powder; combining at least the first metallic powder and the second metallic powder to provide a precursor powder comprising the large metal particles and the small metal particles; and subjecting the precursor powder to an impact blending process to adhere the small metal particles to the large particles, thereby producing a cold compactible metallic powder comprising non-spherical particles, wherein the non-spherical particles comprise one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core.
  • At least a portion of the small metal particles adhered to the large metal particles are metallurgically bonded to the large metal particles.
  • the precursor powder has a multimodal particle size distribution comprising at least a first modal peak corresponding to the first metallic powder and a second modal peak corresponding to the second metallic powder.
  • the d50 particle size of the second metallic powder is no more than 40%, or no more than 30%, or no more than 25%, such as in the range of 10% to 25%, of the d50 particle size of the first metallic powder.
  • the d50 particle size of the second metallic powder is less than the d10 particle size of the first metallic powder. In some embodiments, the d90 particle size of the second metallic powder is less than the d10 particle size of the first metallic powder.
  • the hardness of the large metal particles is greater than or about equal to the hardness of the small metal particles.
  • the large metal particles and the small metal particles have substantially the same metallic composition. In other embodiments, the large metal particles and the small metal particles have a different metallic composition. [20] In some embodiments, the large metal particles in the first metallic powder are substantially spherical. The sphericity of the large metal particles may be greater than 0.7, or greater than 0.75.
  • subjecting the precursor powder to the impact blending process comprises impact blending the precursor powder in an impact blending chamber of an apparatus comprising (i) a stator which defines a cylindrical outer wall of the impact blending chamber, and (ii) a rotor operable to rotate in the impact blending chamber, the rotor comprising a plurality of impact blades having an impact face and an outer edge at the periphery of the rotor.
  • the apparatus may further comprise a recirculation conduit between an entry port located in the cylindrical outer wall of the impact blending chamber and an exit port directed to a central portion of the impact blending chamber, wherein the precursor powder continuously recirculates through the recirculation conduit during the impact blending.
  • each impact blade may be spaced apart from the cylindrical outer wall by a gap distance in the range of 1 mm to 5 mm, such as in the range of 2 mm to 4 mm.
  • the rotor may be rotated such that the outer edge of each impact blade has a peripheral velocity of above 35 m/s, or above 40 m/s, during the impact blending.
  • the precursor powder is impact blended for a time between 1 second and 10 minutes, or between 30 seconds and 5 minutes.
  • the precursor powder is impact blended in a dry inert gas atmosphere.
  • the large metal particles comprise a metallic composition having a yield stress of at least 400 MPa, or at least 600 MPa, such as at least 1000 MPa.
  • the large metal particles comprise a metallic composition having an elongation at break of at least 1 %, such as at least 3%, for example in the range of 5% to 30%.
  • the large metal particles, and optionally also the small metal particles comprise a metallic composition selected from the group consisting of titanium, tantalum, niobium, vanadium, molybdenum, hafnium, zirconium, tungsten, chromium, rhenium, nickel, cobalt, alloys thereof, metal matrix composites thereof, alloys of iron, alloys of zinc, alloys of magnesium, and alloys comprising both aluminium and copper.
  • a metallic composition selected from the group consisting of titanium, tantalum, niobium, vanadium, molybdenum, hafnium, zirconium, tungsten, chromium, rhenium, nickel, cobalt, alloys thereof, metal matrix composites thereof, alloys of iron, alloys of zinc, alloys of magnesium, and alloys comprising both aluminium and copper.
  • the large metal particles, and optionally also the small metal particles comprise a metallic composition selected from the group consisting of titanium, tantalum, niobium, and alloys thereof.
  • the large metal particles, and optionally also the small metal particles comprise titanium or titanium alloy. In some embodiments, the large metal particles comprise titanium alloy. In some embodiments, the large metal particles comprise titanium alloy and the small metal particles comprise a metallic composition selected from the group consisting of commercially pure titanium, titanium alloy, a master alloy for titanium, and mixtures thereof.
  • providing the first metallic powder comprises comminuting and/or spheroidizing precursor metal particles in an impact blending process to produce the large metal particles.
  • the first metallic powder has a d50 particle size of between 1 pm and 500 pm, or between 80 pm and 500 pm, such as between 100 pm and 250 pm, for example between 1 10 pm and 180 pm.
  • the second metallic powder has a d50 particle size of between 0.1 pm and 100 pm, or between 5 pm and 100 pm, such as between 5 pm and 60 pm, for example between 10 pm and 40 pm.
  • the first metallic powder comprises at least 70 wt.% of the precursor powder, or at least 80 wt.% of the precursor powder, such as between about 80 wt.% and about 90 wt.% of the precursor powder.
  • the cold compactible metallic powder comprises at least 20 wt.%, or at least 50 wt.%, of the non-spherical particles comprising one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core.
  • the invention provides a cold compactible metallic powder produced by a method according to any embodiment of the first aspect.
  • the invention provides a cold compactible metallic powder comprising non-spherical particles, the non-spherical particles comprising a large titanium or titanium alloy particle as a core and a plurality of small metal particles as protrusions from the core, wherein at least a portion of the small metal particles are metallurgically bonded to the large titanium or titanium alloy particle.
  • the non-spherical particles comprise a large titanium alloy particle as a core and the small metal particles comprise a metallic composition selected from the group consisting of commercially pure titanium, titanium alloy, a master alloy for titanium, and mixtures thereof.
  • the invention provides a method of producing a porous metallic article, the method comprising: providing (i) a cold compactible metallic powder comprising non-spherical particles, wherein the non- spherical particles comprise a large metal particle as a core and a plurality of small metal particles as protrusions from the core, preferably wherein at least a portion of the small metal particles are metallurgically bonded to the large metal particle, or (ii) a cold compactible metallic powder produced by a method according to any embodiment of the first aspect, or (iii) a cold compactible metallic powder according to any embodiment of the third aspect; and subjecting the cold compactible metallic powder to a cold compaction process at a pressure sufficient to consolidate the cold compactible metallic powder, thereby producing a porous metallic article.
  • the invention provides a method of producing a porous metallic article, the method comprising: providing (i) a first metallic powder comprising large metal particles and (ii) a second metallic powder comprising small metal particles, wherein the d50 particle size of the second metallic powder is less than the d50 particle size of the first metallic powder; combining at least the first metallic powder and the second metallic powder to provide a precursor powder comprising the large metal particles and the small metal particles; subjecting the precursor powder to an impact blending process to adhere the small metal particles to the large particles, thereby producing a cold compactible metallic powder comprising non-spherical particles, wherein the non-spherical particles comprise one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core; and subjecting the cold compactible metallic powder to a cold compaction process at a pressure sufficient to consolidate the cold compactible metallic powder, thereby producing a porous metallic article.
  • the porous metallic article has a density of at least 70 % of theoretical density.
  • the pressure is below 450 MPa, such as below 400 MPa, for example below 350 MPa.
  • the cold compactible metallic powder is subjected to the cold compaction process in the absence of a binder.
  • the cold compaction process is selected from cold isostatic pressing, cold die pressing and direct powder rolling. In some embodiments, the cold compaction process is a cold isostatic pressing process.
  • first”, “second”, “third” etc in relation to various features of the disclosed devices are arbitrarily assigned and are merely intended to differentiate between two or more such features that the device may incorporate in various embodiments. The terms do not of themselves indicate any particular orientation or sequence. Moreover, it is to be understood that the presence of a “first” feature does not imply that a “second” feature is present, the presence of a “second” feature does not imply that a “first” feature is present, etc.
  • Figure 1 is a schematic depiction of a rotational impact blending apparatus for use in methods according to some embodiments of the invention.
  • Figure 2 is an isometric drawing of the impact blending chamber of rotational impact blending apparatus (Nara Hybridization System, NHS-0), as used in the Examples.
  • Figure 3 depicts the impact blending chamber and rotor of a rotational impact blending apparatus for use in methods according to some embodiments of the invention.
  • Figure 4 schematically depicts an impact blending process for converting a precursor powder comprising large and small particles into non-spherical particles comprising one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core.
  • Figure 5 schematically depicts proposed interlocking modes that may occur between adjacent non-spherical particles, as produced according to embodiments of the invention, when compressed to form a porous metal article.
  • Figure 6 contrasts an intact compact (d) produced by cold isostatic pressing from a metal powder deemed cold compactible with the broken compacts (a-c) resulting from cold isostatic pressing of metal powders which are not adequately cold compactible.
  • Figure 7 is a SEM image of non-spherical particles comprising a large prealloyed Ti-6AI-4V particle as the core and a plurality of small pre-alloyed Ti-6AI-4V particles as protrusions from the core, as produced by impact blending (8000 rpm for two minutes) a mixed powder comprising an 80:20 ratio of the large to small particles in Example 1 .
  • Figure 8 is a SEM image of non-spherical particles comprising a large prealloyed Ti-6AI-4V particle as the core and a plurality of small pre-alloyed Ti-6AI-4V particles as protrusions from the core, as produced by impact blending (10,000 rpm for 1 second) a mixed powder comprising a 90:10 ratio of the large to small particles in Example 1 .
  • Figure 9 is a SEM image of non-spherical particles comprising a large prealloyed Ti-6AI-4V particle as the core and a plurality of small CP Ti particles as protrusions from the core, as produced by impact blending (8000 rpm for 1 minute) a mixed powder comprising an 80:20 ratio of the large to small particles in Example 4.
  • Figure 10 is a SEM image of non-spherical particles comprising a large prealloyed Ti-6AI-4V particle as the core and a plurality of small CP Ti particles as protrusions from the core, as produced by impact blending (6000 rpm for 4 minutes) a mixed powder comprising an 80:20 ratio of the large to small particles in Example 4.
  • Figure 11 is a SEM image of spheroidized particles comprising a large prealloyed Ti-6AI-4V particle as the core and a shell of CP Ti, as produced by impact blending (8,000 rpm for 4 minute) a mixed powder comprising an 80:20 ratio of Ti-6AI- 4V particles and small CP Ti particles in Example 4.
  • Figure 12 is a SEM image of spheroidized particles comprising a large prealloyed Ti-6AI-4V particle as the core and a shell of CP Ti, as produced by impact blending (10,000 rpm for 2 minute) a mixed powder comprising an 80:20 ratio of Ti-6 Al- 4V particles and small CP Ti particles in Example 4.
  • Figure 13 is a SEM image of non-spherical particles comprising a large prealloyed Ti-6AI-4V particle as the core and a plurality of small BE Ti64 particles as protrusions from the core, as produced by impact blending (8,000 rpm for 1 minute) a mixed powder comprising an 80:20 ratio of the large to small particles in Example 5.
  • Figure 14 is a SEM image of a classified 150-250 pm fraction of the comminuted Ti-6AI-4V alloy swarf produced in Example 6.
  • Figure 15 is a SEM image of spheroidized metallic particles produced by spheroidizing the classified 150-250 pm fraction of comminuted Ti-6AI-4V alloy swarf in Example 6.
  • Figure 16 is a SEM image of non-spheroidal metallic particles comprising a large metal particle as the core and a plurality of small metal particles as protrusions from the core, as produced in Example 7 by impact blending a combination of spheroidized Ti-6AI-4V alloy particles (produced by spheroidizing in Example 6) and small Ti-6AI-4V alloy particles at 8,000 rpm for 30 seconds.
  • Figure 17 is a SEM image of a cross-section through one non-spherical particle comprising a large pre-alloyed Ti-6AI-4V particle as the core and a plurality of small pre-alloyed Ti-6AI-4V particles as protrusions from the core, as analysed in Example 9.
  • Figure 18 is a SEM image of a cross-section through a compact comprising consolidated non-spherical particles with a core-corona morphology, as analysed in Example 10.
  • Figure 19 is another SEM image of a cross-section through a compact comprising consolidated non-spherical particles with a core-corona morphology, as analysed in Example 10.
  • the present invention relates to a method of producing a cold compactible metallic powder.
  • the method comprises providing first and second metallic powders, comprising large metal particles and small metal particles respectively.
  • the d50 particle size of the second metallic powder is thus less than, and preferably no more than about 40% of, the d50 particle size of the first metallic powder.
  • the method comprises a step of combining at least the first metallic powder and the second metallic powder to provide a precursor powder comprising the large metal particles and the small metal particles.
  • the precursor powder is then subjected to an impact blending process to adhere the small metal particles to the large particles, thereby producing a cold compactible metallic powder comprising non-spherical particles.
  • the non- spherical particles comprise one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core.
  • First metallic powder may be used to modify the morphology of a first metallic powder comprising large metal particles with a second metallic powder comprising small metal particles.
  • the metal particles in the first and second metallic powders are typically present in a range of particle sizes.
  • the particle size distribution (PSD) of such metallic powders may be characterised by d10, d50 and d90 particle sizes, defined such that 10 volume % of the powder is present in particles having a size less than the d10 particle size, 50 volume % of the powder is present in particles having a size less than the d50 particle size and 90 volume % of the powder is present in particles having a size less than the d90 particle size.
  • the d10, d50 and d90 particle sizes may be measured by routine methods in materials science such as laser diffraction techniques. Suitable instruments for measuring PSD include the Mastersizer range of laser diffraction particle sizers, available from Malvern Panalytical. Particle sizes, including d10, d50 and d90 sizes, may be measured in accordance with ASTM B822 (Standard Test Method for Particle Size Distribution of Metal Powders and Related Compounds by Light Scattering).
  • Metallic powders with a wide range of d50 particle sizes may be modified, provided that the particles of the second metallic powder are correspondingly smaller.
  • the first metallic powder may thus have a d50 particle size of between 1 pm and 500 pm.
  • the d50 particle size is between 80 pm and 500 pm, or between 100 pm and 250 pm, such as between 110 pm and 180 pm.
  • the first metallic powder may be classified, for example by sieving, to provide a relatively narrow particle size distribution.
  • the particles of the first metallic powder may comprise any type of metallic composition, including commercially pure metals, metal alloys and metal matrix composites.
  • the methods of the disclosure are particularly useful for upgrading powders of high yield strength metallic compositions.
  • the particles of the first metallic powder comprise a metallic composition having a yield stress of at least 400 MPa, or at least 600 MPa, such as at least 1000 MPa.
  • such metallic compositions will also have a relatively low ductility.
  • a minimum level of ductility may be required to avoid shattering of the large particles under impact blending conditions.
  • the particles of the first metallic powder comprise a metallic composition having an elongation at break of at least 1 %, such as at least 3%, for example in the range of 5 to 30%.
  • yield stress and elongation at break are bulk material properties of a metallic composition, and can be measured by ASTM E8/E8M-13.
  • Non-limiting examples of high yield strength and low ductility metallic compositions include titanium, tantalum, niobium, vanadium, molybdenum, hafnium, zirconium, tungsten, chromium, rhenium, nickel and cobalt, alloys and metal matrix composites of these metals, low ductility alloys of iron, zinc and magnesium, and low ductility alloys comprising both aluminium and copper.
  • very soft and ductile metallic compositions such as commercially pure copper or aluminium, may be less suitable because they deform too easily and/or stick to the impact blender surfaces.
  • metallic compositions including substantial amounts of metals such as copper, lead, zinc, tin and iron are also expected to be soft, and thus susceptible to undesirable deformation and/or to functionalisation by the small particles via surface embedment (rather than metallic bonding).
  • Metallic compositions comprising such metal elements will generally be suitable only if the yield stress is high, such as at least 400 MPa.
  • certain ferritic and martensitic steels have appropriate yield strength, whereas pure iron and austenitic steels are expected to be too soft.
  • the particles of the first metallic powder include copper, lead, zinc, tin and iron only as minor ( ⁇ 20 wt.%, preferably ⁇ 10 wt.%) alloying elements in alloys of other metals or are substantially free of these metals.
  • the particles of the first metallic powder may also comprise a metallic composition having fracture properties suitable to avoid or minimise shattering of the particles during impact blending instead of the desired co-yielding and intermixing believed to occur during formation of the desirable core-corona morphology.
  • the particles of the first metallic powder comprise a metallic composition having a fracture toughness (Kic) in the range of 10 to 150 MPa.m 1/2 , such as in the range of 40 to 150 MPa.m 1/2 .
  • Kic is a bulk material property of a metallic composition, and can be measured by ASTM E1820.
  • the methods of the disclosure are also particularly useful for upgrading powders of oxygen- and/or carbon-sensitive metallic compositions. Compaction of such powders is preferably done without binders to avoid contamination of the metal composition, and methods for improving binderless cold compactibility are thus needed.
  • the metal particles of the first metallic powder comprise an oxygen- and/or carbon-sensitive metallic composition selected from the group consisting of titanium, tantalum, niobium, vanadium, molybdenum, hafnium, zirconium, tungsten, alloys and metal matrix composites of these metals.
  • the metal particles of the first metallic powder comprise a metallic composition selected from the group consisting of titanium, tantalum, niobium, and alloys thereof. In some embodiments, the metal particles comprise alloys of titanium, tantalum, or niobium. In some embodiments, the metal particles of the first metallic powder comprise a titanium alloy.
  • suitable titanium alloys include Ti-6AI-4V (i.e. titanium alloyed with 6 wt.% Al, 4 wt.% V) and Ti-10V-2Fe-3AI (i.e. titanium alloyed with 10 wt.% V, 2 wt.% Fe, 3 wt.% Al).
  • an “alloy of metal X” refers to an alloy in which metal X is the most abundant metal element by atomic %.
  • an alloy of titanium (alternatively a titanium alloy) refers to a metallic alloy in which titanium is the element present in the highest atomic %.
  • metal X is present in an amount of at least 50 atomic % in an alloy of metal X.
  • An alloy is typically a fully reacted and homogenous mixture such that the solid solutions and any intermetallic phases that form are unique to the alloy, befitting the thermodynamic and kinetic circumstances related to their reaction, and different from the elemental metal mixtures.
  • metal alloys thus may include intermetallic compounds.
  • a “metal matrix composite of metal X” refers to a composition comprising a matrix of commercially pure metal X or an alloy of metal X, with a non- metallic particulate phase dispersed in the matrix.
  • Exemplary non-metal particulate phases include ceramics added as a strengthening phase.
  • the methods of the disclosure are particularly useful for upgrading powders with relatively spherical morphologies for cold compaction applications, since such materials (without modification) can be hard to consolidate due to the small interparticle interfaces.
  • the large metal particles in the first metallic powder are substantially spherical.
  • substantially spherical particles are spherical or near-spherical in shape, in contrast to the morphologies of non- spherical powders composed of irregular or flake particles.
  • the morphology of particles may be quantified with a sphericity number, defined with respect to the cross-section of the particles as the ratio of the radius of the inscribed circle to the radius of the circumscribed circle (where the inscribed circle is the largest circle inside the particle cross-section, the circumscribed circle is the smallest circle outside the particle crosssection, and both circles are centred on the particles’ centre of mass.)
  • the sphericity of the large metal particles is greater than 0.7, or greater than 0.75.
  • Certain metallic powders produced by gas atomization have substantially spherical particle morphologies.
  • Commercial gas atomization processes generally produce a range of particle sizes, of which only a fraction may be commercially valuable (e.g. as powders for additive manufacturing).
  • the out-of- specification particle sizes, including both oversized and undersized fractions, may thus be a low cost by-product, particularly considering that re-processing these fractions through gas atomization would require remelting the metallic composition.
  • the metal particles of the first metallic powder are produced by gas atomization.
  • the inventors have demonstrated that an oversized fraction (105-250 pm) of pre-alloyed Ti-6AI-4V particles produced by gas atomization can be upgraded by the present methods for cold compaction applications, despite the highly spherical morphology of the unmodified material.
  • providing the first metallic powder comprises comminuting and/or spheroidizing precursor metal particles to form the large particles of the first metallic powder, typically prior to combination with the second metallic powder.
  • This particle modification step may include milling the precursor metal particles to reduce the particle size in suitable milling equipment.
  • Spheroidization of the precursor particles may be conducted in any suitable equipment, for example impact blending apparatus which may be the same or different to the apparatus subsequently used to impact blend the combined first and second metallic powders.
  • Impact blending for example in a Hybridizer apparatus, may be used to spheroidize irregular-shaped particles to more spheroidal form, and such modified particles may be suitable as core particles for further modification according to the principles of the present disclosure.
  • the methods of the disclosure modify the morphology of the first metallic powder using a second metallic powder comprising small metal particles, and which thus has a d50 particle size less than that of the first metallic powder.
  • the d50 particle size of the second metallic powder is no more than 40%, or no more than 30%, or no more than 25% of the d50 particle size of the first metallic powder.
  • the d50 particle size of the second metallic powder is at least 4% of the d50 particle size of the first metallic powder.
  • the d50 particle size of the second metallic powder in the range of 10% to 25% of the d50 particle size of the first metallic powder.
  • the second metallic powder may have a d50 particle size of between 0.1 pm and 100 pm, or between 5 pm and 100 pm, such as between 5 pm and 60 pm, for example between 10 pm and 40 pm.
  • the second metallic powder may be classified, for example by sieving, to provide a relatively narrow particle size distribution.
  • the particle size distributions are typically sufficiently differentiated that a combination of the first and second metallic powders will have a multimodal particle size distribution comprising at least a first modal peak corresponding to the first metallic powder and a second modal peak corresponding to the second metallic powder.
  • the d50 particle size of the second metallic powder is less than the d10 particle size of the first metallic powder.
  • the d90 particle size of the second metallic powder is less than the d10 particle size of the first metallic powder.
  • the particles of the second metallic powder may comprise any type of metallic composition, including commercially pure metals, metal alloys and metal matrix composites.
  • the small metal particles of the second metallic powder and the large metal particles of the first metallic powder may have a different metallic composition or substantially the same metallic composition.
  • a metallic composition refers to the elemental composition of the powder as a whole and not the metallurgical structure.
  • a blended elemental (BE) powder comprising alloy component particles of different compositions may have the same metallic composition as a powder consisting of pre-alloyed metallic particles.
  • large pre-alloyed Ti-6AI-4V spherical particles may be modified with small particles of the same metallic composition, either as (i) pre-alloyed Ti-6AI-4V particles or (ii) BE powder for Ti-6AI-4V composed of commercially pure Ti and 60AI-40V master alloy, to produce a cold compactible metallic powder.
  • the large metal particles may advantageously be modified without changing its metallic composition.
  • the small particles of the second metallic powder may comprise a fines fraction produced in the comminuting.
  • the spheroidized large metal particles may advantageously be modified without changing the metallic composition.
  • a second metallic powder with a different metallic composition may be preferred, to provide a cold compactible powder with a composition which differs from that of the first metallic powder.
  • the first metallic powder may advantageously be composed of a high yield strength metallic composition
  • the smaller particles of the second metallic powder may be formed of either a high yield strength material, for example as disclosed herein for the first metallic powder, or a lower strength, more ductile metallic material.
  • the metallic composition of the large metal particles has a yield stress that is greater than or about equal to that of the metallic composition of the small metal particles.
  • the small metal particles comprise a metallic composition selected from the group consisting of commercially pure titanium, titanium alloy, a master alloy for titanium, and mixtures thereof.
  • the mechanical properties of the large and small particles should be matched to allow some mutual yielding and seizing between their surfaces during impact, so that a core-corona morphology with metallurgical bonding between core and protrusions can be produced. In principle, only one of the surfaces must yield to allow joining of the particles. However, if the small particles are substantially harder than the larger particles, they are less likely to co-yield and more likely to penetrate and embed (i.e. via mechanical rather than metallurgical bonding).
  • the large particles of the first metallic powder are harder, or of equivalent hardness and of greater or equivalent yield strength, than the smaller particles of the second metallic powder.
  • the small particles may still deform sufficiently to form a desirable core-corona morphology, despite having a greater intrinsic yield strength, if the resolved shear stress of the small particles is higher during impact. This is possible because the impact surface area of the small particles may be less than the surface it impacts on the larger particle. Thus, in a collision between a large and a small particle, the smaller particle will see a larger stress for at least part of the impact than the larger particle.
  • the small particles of the second metallic powder may have any suitable particle shape.
  • they may be substantially spherical particles, for example as produced by gas atomization.
  • the inventors have demonstrated that an undersized fraction (5-25 pm) of pre-alloyed Ti-6AI-4V particles produced by gas atomization can be used to form the protrusions of non-spherical particles.
  • the small particles may have non-spherical, such as irregular, blocky or angular, morphologies. It has been found that small particles with a sphericity of only 0.3 may be used to form the protrusions.
  • the methods disclosed herein include a step of combining at least the first metallic powder and the second metallic powder to provide a precursor powder comprising the large metal particles and the small metal particles.
  • the two powders may be well-mixed before the subsequent impact blending step, although this is not essential as mixing will occur during the impact blending.
  • the two metallic powders are first combined in the impact blending apparatus.
  • the precursor powder prior to impact blending typically has a multimodal particle size distribution comprising at least a first modal peak corresponding to the first metallic powder and a second modal peak corresponding to the second metallic powder.
  • the first metallic powder is typically the primary component, by mass, in the precursor powder.
  • the first metallic powder comprises at least 70 wt.% of the precursor powder, or at least 80 wt.% of the precursor powder, such as between about 80 wt.% and about 90 wt.% of the precursor powder.
  • the second metallic powder typically forms the remainder of the precursor powder, although it is not excluded that additional metallic powders could be combined with the first and second metallic powders.
  • the methods disclosed herein include a step of subjecting the precursor powder to an impact blending process to adhere the small metal particles to the large particles.
  • an impact blending process refers to any dry powder blending process which causes high velocity impacts between the particles with sufficient intensity to adhere, and preferably metallurgically bond, the small metal particles to the large particles.
  • Suitable impact blending processes include rotational impact blending, sometimes referred to as hybridization, and various other dry particle coating technologies.
  • the impact blending process is a rotational impact blending process. In such a process, a rotor is rotated at high speed in an impact blending chamber such that impact blades or other mechanical elements mounted on the rotor strike the powder particles at high velocity.
  • the rotational impact blending process may be performed in an apparatus 100 that includes an impact blending chamber 108, the cylindrical outer wall of which is defined by a stator 110, and a rotor 1 12 which rotates in the impact blending chamber.
  • Impact blending chamber 108 is enclosed by removable front panel 1 13 and rear wall 1 17.
  • the generally disc-shaped rotor includes a plurality of radially oriented impact blades 1 14 having an impact face 1 16 and an outer edge 1 18 at the periphery of the rotor and spaced apart from the cylindrical stator by a small gap 120.
  • the rotor also includes radial ribs 1 15 on the reverse side which are spaced apart from the rear wall 1 17 of the impact chamber by a narrow gap 1 19.
  • the apparatus includes a recirculation conduit 122 extending between an entry port 124 located in the cylindrical outer wall of the impact blending chamber and an exit port 126 located in front panel 113 which is directed to the centre of the impact blending chamber. Powder is added to the impact blending chamber via inlet 128 and discharged through powder outlet port 133, also located in front panel 113, via discharge valve 137 to powder outlet 135. Cooling water is circulated through the stator via coolant ports 130, 132.
  • the metallic precursor powder is fed from a sealed vessel into the impact blending chamber via a high pressure stream of inert gas (e.g. argon).
  • the rotor is rotated such that the impact blades sweep through the impact blending chamber.
  • the metal particles of the precursor powder are thus repeatedly struck at high velocity by the impact face of the impact blades.
  • the spinning rotor also creates a vortex that accelerates the particles by centripetal forces to the peripheral gap, and causes a strong recirculating gas flow through the recirculation conduit by a fan effect, so that the powder continuously circulates through the recirculation conduit during the impact blending.
  • the accelerated particles thus collide with each other, strike the stator and impact blades and are subjected to shearing in the gap between the impact blade outer edges and the stator. Particles that migrate to the back of the rotor are forced back to the periphery by the rotating ribs 1 15.
  • Such apparatus called the Nara Hybridization System (NHS-0), is commercially available from Nara Machinery Co., Ltd.
  • Other suitable impact blending apparatus may include the Mechanofusion system and Cyclomix from Hosokawa Micron Ltd..
  • a few apparatus and process parameters of the rotational impact blending process may be particularly significant to the resultant powder morphology. These include the blade design, and in particular the gap (gap 120) between the rotating blades and the stator.
  • the inventors have found that a gap distance of 3.5 mm was suitable for modifying pre-alloyed Ti-6AI-4V particles with a d50 particle size of about 120-160 pm, and it is expected that a similar gap distance will be suited for impact blending particles with a size in the range of 1 pm to 500 pm.
  • the outer edge of each impact blade is spaced apart from the cylindrical outer wall by a gap distance in the range of 1 mm to 5 mm, such as in the range of 2 mm to 4 mm.
  • FIG. 10 Another significant parameter is the rotation speed of the rotor.
  • the rotational velocity of the impact blades near the rotor periphery must be sufficient to generate the high intensity collisions between the powder particles needed for robust particle adhesion.
  • the inventors have found that peripheral rotor velocities in the range of about 37.1 m/s to 61.8 m/s (corresponding to 6,000 rpm to 10,000 rpm) were suitable for modifying prealloyed Ti-6AI-4V large particles with a d50 particle size in the range of 120-160 pm, but it will be appreciated that lower or higher speeds may be preferred for different powder compositions and particle sizes.
  • the rotor is rotated such that the outer edge of each impact blade has a peripheral velocity of above 35 m/s, such as above 40 m/s, during the impact blending.
  • a further significant parameter is the impact blending time, which should be sufficient to adhere the small metal particles to the large core particles but not so long that the modified particles become spheroidized.
  • the second metallic powder comprises a relatively ductile metallic composition
  • the precursor powder is impact blended for a time between 1 second and 10 minutes, such as between 30 seconds and 5 minutes.
  • the time required to create a desirable particle morphology may be inversely correlated with the intensity of the impact blending conditions.
  • the inventors have found by experiment that impact blending times of as little as a few seconds may be sufficient to create a desirable morphology when modifying pre-alloyed Ti-6AI-4V particles with a d50 of about 120-160 pm at very high impact conditions (peripheral rotor velocity of about 62 m/s). Under more moderate blending conditions (peripheral rotor velocity of about 37 - 49 m/s), impact blending times of 30 seconds to 4 minutes were typically suitable.
  • the precursor powder may be impact blended in a dry inert gas atmosphere. This advantageously limits oxidation of the metal powders during the impact blending. Without limitation by theory, it is proposed that freshly exposed metal surfaces of the particles, as formed during impact blending under inert atmosphere, are not immediately sealed by an oxidic layer and thus remain capable of adhering and intermixing with the metallic surfaces of other particles.
  • FIG. 4 schematically depicts an impact blending process 400 which converts a precursor powder 410 comprising large particles 412 (derived from the first metallic powder) and small particles 414 (derived from the second metallic powder) into non-spherical particles 416 having a core-corona morphology.
  • Particles 416 comprise one of the large metal particles 412 as core 418 and a plurality of the small metal particles 414 as protrusions 420 from the core.
  • Some of the protrusions (420a) comprise a single small particle 414 while other protrusions (420b) comprise a cluster of small particles 414.
  • the inventors propose, on the basis of scanning electron microscopy (SEM) analysis of cross-sectioned core-corona particles, that the small metal particles are metallurgically bonded to the large particles along at least a portion of the inter-particle interfaces.
  • SEM scanning electron microscopy
  • This mode of chemical bonding is distinguished from mere mechanical embedding of the type produced when surfacemodifying soft non-metallic core particles with hard guest particles.
  • the large and small metal particles are thus effectively integrated into a single non-spherical metallic particle as core and protrusions.
  • the resultant mechanical integrity of the non-spherical particles is considered to be important for desirable cold compaction properties, since adhesion of the protrusions to the core must withstand the severe compressive forces when the particles are consolidated into a compact under pressure.
  • the non-spherical particles typically comprise many protrusions distributed around the periphery of the core particle. Each protrusion may comprise a single small particle or a cluster of small particles.
  • the small particles may be deformed by the bond-forming impact with the core particle, or by subsequent high velocity impacts of the non-spherical particle during the impact blending process.
  • the extent of deformation may depend on the yield strength and ductility of the small particle metallic composition, as well as the impact blending conditions and time. A degree of deformation and spheroidization can be tolerated, provided that the particles retain a core-corona morphology. However, if spheroidization continues to the extent that the small particles adhered to the core are beaten out into a substantially uniform shell around the core, the cold compaction properties of the powder may be adversely affected.
  • the morphology of particles may be quantified with a convexity number, defined as the ratio of the perimeter of a particle’s convex hull to the perimeter of the object itself (both measured with respect to a cross-section of the particles).
  • the convexity of the non-spherical particles is below 0.8, such as in the range of 0.4 to 0.8.
  • the cold compactible metallic powder thus comprises at least 20 wt.%, such as at least 50 wt.%, or at least 60%, of the non-spherical particles comprising one of the large metal particles as a core and a plurality of the small metal particles as protrusions from the core.
  • the cold compactible metallic powder comprises non- spherical particles comprising a large titanium or titanium alloy particle as a core and a plurality of small metal particles as protrusions from the core.
  • the small metal particles may comprise a metallic composition selected from the group consisting of commercially pure titanium, titanium alloy, a master alloy for titanium, and mixtures thereof.
  • the small metal particles may be metallurgically bonded to the large titanium or titanium alloy particle.
  • the invention also relates to a method of producing a porous metallic article.
  • the method comprises providing a cold compactible metallic powder comprising non- spherical particles.
  • the non-spherical particles comprise a large metal particle as a core and a plurality of small metal particles as protrusions from the core.
  • the small metal particles may be metallurgically bonded to the large metal particle along at least a portion of the interface.
  • the non-spherical particles may be produced by the methods previously disclosed herein.
  • the method includes a step of subjecting the cold compactible metallic powder to a cold compaction process at a pressure sufficient to consolidate the cold compactible metallic powder, thereby producing a porous metallic article.
  • the cold compaction process may involve any cold compaction method wherein a metallic powder is consolidated under pressure, with or without a binder, at temperatures below the sintering temperature, to produce a porous metal object (a compact) with sufficient structural integrity to withstand further processing, e.g. via sintering or other metalworking techniques, to produce a final metal product.
  • Suitable cold compaction techniques may include cold isostatic pressing, cold die pressing, direct powder rolling and metal injection moulding.
  • the metallic powder In cold isostatic pressing, the metallic powder is sealed in a forming mould with low deformation resistance, such as a rubber bag, and liquid pressure is applied to the mould. The powder is thus compressed uniformly over the entire surface of the compact because the liquid pressure is transmitted through the flexible mould.
  • cold die pressing also known as metal mould pressing
  • the metallic powder In cold die pressing, also known as metal mould pressing, the metallic powder is filled into a mould (cold die) between upper and lower punches. The powder is then compressed by narrowing the distance between the upper and lower punches.
  • direct powder rolling the metallic powder is compressed between a pair of rollers to form a continuous green strip.
  • metal injection moulding the metallic powder is blended with a binder to create an injectable feedstock which is injection moulded to produce a preform.
  • the cold compactible metallic powder is subjected to the cold compaction process in the absence of an organic binder, or in the absence of a non-metallic binder, or in the absence of any binder.
  • the cold compactible metallic powders provided by the present disclosure are particularly useful for binderless cold compaction processes because the adhesion of the particles is enhanced by the corecorona particle morphology.
  • FIG. 5 schematically depicts some proposed interlocking modes that may occur between adjacent non-spherical particles 516 in the porous metal compact. At some interparticle interfaces, such as interface 510ab between particles 516a and 516b, the particles engage via protrusions 520a and 520b of both particles.
  • the engagement of the particles is assisted by protrusion 520c of one particle only.
  • the protrusions comprise a relatively soft metal (e.g. CP Ti)
  • some joining of the protrusions on adjacent particles may also assist the consolidation of the particles in the compact.
  • such joining is not seen for non-spherical particles with harder protrusions (e.g. Ti-6AI-4V) where excellent compaction properties were nevertheless obtained.
  • the cold compaction process consolidates the cold compactible metallic powder to produce a porous metallic article. There are thus voids between the compacted metal particles in the metallic structure, which will be empty following a binderless compaction process.
  • the porosity of the metallic article will depend on the morphology of the particles, the deformability of the particles under the compaction pressure (which may be low if the particle cores are formed of a high yield strength composition) and the compaction pressure.
  • the porous metallic article has a density of at least 70 % of theoretical density.
  • the porosity of suitably robust compacts may vary in other implementations, depending on the factors mentioned above.
  • the density of the porous compact may be increased by adding small particles to the cold compactible metallic powder, the small particles sized to occupy a portion of the voids between the interlocked non-spherical particles after compaction.
  • the cold compactible metallic powder may be compacted at any pressure sufficient to consolidate the cold compactible metallic powder and thus form a porous metallic article.
  • the cold compactible metallic powders of the present disclosure comprising non-spherical particles with a core-corona morphology, may advantageously be consolidated at significantly lower pressures than required for rounded (e.g. spherical) particles which lack protrusions but have a similar metallic composition.
  • the inventors have found that compaction of non-spherical particles with cores and protrusions formed from high yield strength pre-alloyed Ti-6AI-4V particles may be consolidated to form robust compacts at pressures of only 345 MPa.
  • the cold compactible metallic powder is compacted at a pressure below 450 MPa, or below 400 MPa, such as below 350 MPa, for example below 300 MPa.
  • porous metallic articles produced by the methods disclosed herein are typically not final metal products but will instead be further processed.
  • the porous metal article is sintered to produce a sintered metal structure which may be further processed by conventional metalworking techniques.
  • the porous metallic articles may be a feedstock for a metal manufacturing technique such as extrusion.
  • the porous metallic article is a cylindrical rod titanium alloy compact, for example with dimensions of 12.5mm diameter and 400mm length, suitable for extrusion to make titanium alloy wire as disclosed in US patent 9,468,960.
  • Ti-6AI-4V (Ti64) powders were received from a commercial manufacturer in two size fractions: an oversized (large) fraction (>140# mesh, 105-250 pm, hereafter Ti64-L1 ) and an undersized (small) fraction (5-25 pm, hereafter Ti64-S1 ).
  • Commercially pure titanium powder CP Ti; Grade 2 with an irregular I angular morphology was received from TIPRO International Co. Ltd.
  • AI60V40 master alloy was received from Reading Alloys, Inc.
  • a portion of the Ti64-L1 powder was sieved to produce a narrower particle size distribution powder (passing 100# mesh, ⁇ 150 pm, hereafter Ti64-L2).
  • a portion of the CP Ti powder was sieved (passing 400# mesh, ⁇ 38 pm, hereafter CPTi-S2).
  • a portion of the AI60V40 master alloy was also sieved (passing 635# mesh, ⁇ 20pm, hereafter AI60V40-S2).
  • the as-received particles were characterised by scanning electron microscopy to determine the sphericity.
  • Sphericity is a measure of the degree to which the particles in a powder approach the shape of a sphere. It is measured based on the imaged cross-sections of the particles using image analysis software, in this case, “Image J”.
  • Sphericity is defined, with respect to the imaged cross-section of the particles, as the ratio of the radius of the inscribed circle to the radius of the circumscribed circle (where the inscribed circle is the largest circle inside the particle cross-section, the circumscribed circle is the smallest circle outside the particle crosssection, and both circles are centred on the particles’ centre of mass).
  • the particles were characterised by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) for their compositions, Scanning electron Microscopy (SEM) (ZEISS MerlinTM FE-SEM) for their morphologies and Mastersizer S for particle size distributions (PSD). The results are shown in Tables 1 and 2 below.
  • ICP-OES Inductively Coupled Plasma Optical Emission Spectroscopy
  • SEM Scanning electron Microscopy
  • ZEISS MerlinTM FE-SEM ZEISS MerlinTM FE-SEM
  • Mastersizer S particle size distributions
  • a titanium alloy swarf produced as a by-product of a manufacturing process in the aerospace industry (“as-received swarf”), was characterised by inductively coupled plasma-optical emission spectroscopy (ICP-OES), confirming the composition as Ti-6AI-4V alloy containing about 0.19% oxygen, which is within Grade 5 specification for this alloy.
  • ICP-OES inductively coupled plasma-optical emission spectroscopy
  • the as-received swarf was characterised by scanning electron microscopy (SEM, ZEISS MerlinTM FE-SEM) to investigate its morphology.
  • SEM scanning electron microscopy
  • ZEISS MerlinTM FE-SEM scanning electron microscopy
  • the swarf particles were observed to be flake-shaped with some curvature to the structure typical of material generated through machining processes. There are also a large number of various defects, such as cracks, jagged edges and perforations on the swarf surfaces.
  • the flake shaped swarf particles have a thickness ranging from 30-100 pm, and a particle size (maximum dimension) of up to 5 mm in length.
  • the as-received swarf was subjected to sieve analysis according to ASTM B214 to determine the particle size distribution. It was estimated that the d10, d50 and d90 particle sizes for the swarf were 0.64 mm, 1 .25 mm and 2.2 mm respectively.
  • the apparent density and tap density of the as-received swarf were determined, according to ASTM B417 and ASTM B527, to be 0.616 g/cm 3 and 0.751 g/cm 3 respectively.
  • a Nara Hybridization System (NHS-0), available from Nara Machinery Co., Ltd. and schematically depicted in Figure 1 , was used as the particle modification apparatus.
  • the system is equipped with an impact blending chamber, defined by a cylindrical stator, with a rotor and a recirculation duct. During impact blending the particles can leave the impact blending chamber via an outlet in the stator and are refed into the chamber centre via the recirculation duct.
  • the chamber is surrounded with a jacket in which coolant is circulated to keep the inside treatment temperature under 100°C, typically under 50°C.
  • the NHS-0 was operated under a high purity argon (3ppm O2) atmosphere in order to keep oxygen levels as low as possible and thus reduce the opportunity for oxygen contamination of the titanium powder materials.
  • FIG. 1 Schematic drawings of the impact blending chamber of the NHS-0 are shown in Figures 1 , 2 and 3.
  • the outer wall of the impact blending chamber is defined by stator 1 10.
  • Rotor 1 12 with a diameter of 1 18 mm, includes six radially-oriented impact blades 1 14 having an impact face 116 and an outer edge 1 18 at the periphery of the rotor.
  • the impact blades have a length in the radial direction of 20 mm, a thickness of 5 mm and flattened edges.
  • the gap 120 between outer edge 1 18 of the blades and stator 1 10 was 3.5 mm.
  • the rotor also includes radial ribs 115 on the reverse side which are spaced apart from the rear wall 1 17 of the impact chamber by gap 1 19, which was 0.9 mm.
  • the NHS-0 is operable at rotor rotation speeds of up to 16,000rpm. Generally, speeds of 6,000rpm to 10,000rpm were found most suitable. The corresponding conversion of rotational velocity to peripheral velocity (i.e. the speed of outer edge 1 18 of the blades) is shown in Table 3. The apparatus took some time to reach the set rotation speed (23, 30 and 38 seconds to reach 6,000, 8,000 and 10,000 rpm respectively). The impact blending times referred to in the subsequent examples refer to the time once the set rotation speed was reached.
  • Each mini rod had dimensions of about 8.5mm ID and a length of 30 to 50 mm, and weighed about 6.0 grams.
  • the green compacts are quite strong and hence a relatively rigid single rubber bag can be used.
  • the green compacts may not be strong enough to overcome the tensile stress generated inside the rigid rubber bag, resulting in the breakage of the compacts.
  • the double bagging method assists to mitigate this issue because there is little gripping force between the outermost flexible bag and the green compact, therefore protecting the compact from breaking.
  • the outermost bag can be recovered for further use and the thin innermost polyethylene tubing is peeled off from the intact green compact.
  • an elongate metal support such as an L-shaped metal angle (with the elongated bag secured into the angle) or a cylindrical aluminium lattice (with the elongated bag secured inside the cylinder), to hold the bag straight during cold isostatic pressing while still allowing uniform pressure to be applied to the exterior of the bag,
  • Ti64-L1 The as-received oversized Ti64 powder (Ti64-L1 ) and the undersized Ti64 powder (Ti64-S1 ) were combined and mixed at three different weight ratios: 80:20, 85:15, and 90:10.
  • the combined powders were then subjected to rotational impact blending in the NHS-0 system at various rotor rotational speeds (6,000 to 10,000 rpm) and for different impact blending times (1 second to 4 minutes). Afterwards, the impact blended powders were recovered and analysed by SEM to investigate the resultant morphology. Selected samples were also analysed by ICP-OES.
  • Impact blended powders prepared by impact blending the precursor powders having ratios of 80:20, 85:15 and 90:10 Ti64-L1 to Ti64-S1 at 9,000 rpm for 60 seconds, were further characterised by ICP-OES to determine their compositions and by the Mastersizer S to determine their particle size distributions (PSD).
  • the PSD results are shown in Table 7. There was minimal difference between the particle size distributions of the impact blended powders with different ratios of Ti64-L1 to Ti64-S1 .
  • the impact blended powders were slightly larger than the Ti64-L1 precursor due to the adhesion of the small particles to the larger core particles.
  • the specific surface areas of the impact blended powders increased by about 16% to 20% compared to the Ti64-L1 precursor, consistent with the change in morphology.
  • the impact blended powders were recovered and analysed by SEM to investigate the resultant morphology. While lower impact conditions may have been preferable, the impact blended powder nevertheless still contained a fraction of particles with a core-corona morphology, as seen in Figure 13 (8,000 rpm for 1 minute).
  • the impact blended powders were then subjected to cold isostatic pressing at pressures of 206 and 413 MPa to determine if cold compacted rods could be formed.
  • the impact blended powders were found to be cold compactible at 206 MPa, although the resultant compacts were relatively weak and thus easy to break. Nevertheless, the cold compactability results contrast against the initial mixture of particles, i.e. before impact blending, which was not cold compactible even at 413 MPa.
  • a metallic powder comprising spheroidal large metal particles, suitable for upgrading according to the methods disclosed herein, was prepared from the titanium alloy swarf using the same impact blending apparatus used for rotational impact blending in the earlier examples.
  • the as-received swarf was subjected to five sequential rounds of milling in the NHS-0 system at 10,000 rpm for 30 seconds. In the first round of milling, 100 g of swarf was processed in 10 batches, with the limitation of 10 g per batch due to the low apparent density of the swarf. After the first round of milling, the comminuted material from the 10 batches was sieved into three size ranges: -250 micron, 250-500 micron and +500 micron.
  • the two larger fractions were separately milled and classified into the same three size fractions.
  • the newly formed -250 micron fraction was combined with the prior-formed -250 micron fraction, the two newly formed 250-500 micron fractions were combined and the two newly formed +500 micron fractions were combined for the next round of milling.
  • the -250 micron fraction of particles was then further classified by sieving into -75 pm, 75-150 pm and 150-250 pm fractions.
  • the particles in each size range were then separately subjected to milling in the NHS-0 at 10,000 rpm for 14 minutes to spheroidize the particles.
  • the amount of material processed in each batch varied from 10g to 25g, limited only by the amount of material available, thus demonstrating that the spheroidization step can be conducted at higher loading concentrations in the impact chamber than the comminution step.
  • the sphericity of the powders was characterised using image analysis of SEM images.
  • the sphericity values for the as-received swarf, the input powders to spheroidization (comminuted material classified into -75 pm, 75-150 pm and 150-250 pm fractions) and resultant spheroidized powders (still in the -75 pm, 75-150 pm and 150-250 pm fractions) are shown in Table 1 1 , where the average sphericity is the average of 10 particles.
  • the as-received swarf is highly irregular, and the sphericity remains low for all fractions after comminution. After the spheroidizing step, the sphericities are greatly improved, particularly for the two large fractions.
  • the resultant powder thus comprised non-spherical particles comprising a large metal particle (derived from the previously spheroidized particles) as the core and a plurality of the small metal particles (derived from Ti64-S1 ) as protrusions from the core.
  • a representative SEM image is shown in Figure 16. At still higher intensity conditions (9000 rpm for 30 s) most of the small Ti64-S1 particles had attached to the larger spheroidized particles, with some flattening of the resultant protrusions also evident.
  • Example 7 The powders produced in Example 7, comprising non-spherical particles comprising a large spheroidized metal particle as the core and a plurality of the small metal particles as protrusions from the core, were then subjected to cold isostatic pressing (CIPing) at pressures of 380 MPa (55ksi) to determine if the powders were cold compactible.
  • CIPing cold isostatic pressing
  • the powders were compacted to form “mini rods” with dimensions of about 8.5mm diameter and a length of 30 to 50 mm.
  • Example 9 The impact blended Ti64 powder with a core-corona morphology produced in Example 3 (85:15 ratio of Ti64-L1 to Ti64-S1 , impacted blended at 9,000 rpm for one minute) was used to study the mode of bonding between the core (derived from the large Ti64-L1 particles) and the protrusions (derived from the small Ti64-S1 particles).
  • the impact blended powder particles were cold mounted and ground to 1200 grit using SiC papers and final polished using OP-S suspension. To identify and examine the interface between the large Ti64-L1 core particles and the small Ti64-S1 particles, the polished samples were etched by Kroll’s reagent. The impact blended powder was then characterized by SEM (ZEISS MerlinTM FE-SEM) at high magnification.
  • FIG. 17 A SEM image of a cross-section through one core-corona Ti64 particle is shown in Figure 17.
  • areas B In one area (area B), many small particles were present in a cluster which was bonded to the core particle.
  • the interfaces between the core and the small particles, and also between adjacent small particles in the cluster, were identifiable in the magnified SEM image as dark grey lines. Despite some tiny voids along the interfaces, the integrity of the interfaces is generally consistent with metallurgical bonding between the particles along at least a part of the interfaces. Similar interfaces between core and protrusion particles were evident in other areas of the cross-section.
  • Example 4 Impact blended powders with a core-corona morphology produced from hard large particles and softer small particles in Example 4 (Ti64-L2 large particles + CPTi- S2 small particles) and Example 5 (Ti64-L2 large particles + CPTi-S2 small particles + AI60V40-S2 small particles), were also analysed by SEM.
  • the resultant protrusions were generally smaller than those on the non-spherical particles from Example 3, due in part to the greater ductility of the small particles.
  • high resolution SEM analysis of the interface between core and protrusions again indicated that the CP Ti particles had metallurgically bonded to the Ti64 alloy core in both experiments.
  • the Ti64 green compact (pre-alloyed Ti64 large particles + pre-alloyed Ti64 small particles) produced by cold isostatic pressing at 206 MPa in Example 3 was characterized by SEM (ZEISS MerlinTM FE-SEM) at high magnification. A cross-section of the green compact was cold mounted and ground to 1200 grit using SiC papers and final polished using OP-S suspension. To identify and examine the interface between the particles in the compact, the polished samples were etched by Kroll’s reagent before the SEM analysis.
  • Example 4 A cold compact produced in Example 4 from an impact blended powder comprising pre-alloyed Ti64 large particles + CP Ti small particles (Example 4: 8,000 rpm, 2 minutes) was also characterized by SEM analysis. Again, protrusions from one or both particles were seen to be present at many of the interfaces between adjacent particles, suggesting that the protrusions facilitate interlocking between the particles during compaction. In contrast to the impact blended particles of Example 3, however, a degree of deformation of the soft CP Ti protrusions was seen and it appears that some joining of the protrusions on adjacent particles may assist the consolidation of the particles in the compact. Moreover, loose CP Ti particles were also observed in the compact. These particles either had not adhered to the core Ti 64 particles during impact blending or detached from the non-spherical particles in response to the stresses applied during the compaction process.
  • the core-corona morphology of impact blended core-corona non-spherical particles provides improved cold compactability properties compared to the substantially spherical precursor particles.
  • Convexity is the relative amount that an object differs from a convex object.
  • the convex object is the particle as measured in cross section.
  • a measurement of convexity is obtained by forming the ratio of the perimeter of a particle’s convex hull to the perimeter of the object itself, according to the equation below.
  • the convex hull is a polygon that encloses the particle cross section with no point of the polygon bending inwards.
  • Convexity - particle perimeter [179] If the particle cross section is a convex object (e.g. round particle or ellipse with a smooth surface), the convexity will be 1 , as the perimeters of the convex hull and the object are the same. The value will be less than 1 if the object has an irregular boundary. For the impact blended particles, if their convexity values are closer to 1 , their shapes are closer to the original core particles before impact blending.
  • the unmodified Ti64 powder and spheroidized swarf powder had a convexity very close to 1 , consist with the spherical nature of the particles. After impact blending with different materials, the convexity value reduces substantially because of the protrusions from the cores.
  • the impact blended powder produced in Example 3 (prealloyed Ti64 large particles + pre-alloyed Ti64 small particles) had the lowest convexity, because the small particle protrusions are relatively undeformed due to the hard metallic composition.

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Abstract

L'invention concerne un procédé de production d'une poudre métallique compactable à froid, le procédé consistant : à fournir (i) une première poudre métallique comprenant de grosses particules métalliques et (ii) une seconde poudre métallique comprenant de petites particules métalliques, la taille de particules d50 de la seconde poudre métallique étant inférieure à la taille de particules d50 de la première poudre métallique ; à combiner au moins la première poudre métallique et la seconde poudre métallique pour fournir une poudre précurseur comprenant les grosses particules métalliques et les petites particules métalliques ; et à soumettre la poudre précurseur à un procédé de mélange par impact pour faire adhérer les petites particules métalliques aux grosses particules, ce qui permet de produire une poudre métallique compactable à froid comprenant des particules non sphériques, les particules non sphériques comprenant l'une des grosses particules métalliques en tant que noyau et une pluralité de petites particules métalliques formant des protubérances à partir du noyau.
PCT/AU2022/051541 2021-12-20 2022-12-20 Procédé de production d'une poudre métallique compactable à froid Ceased WO2023115119A1 (fr)

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AU2022420976A AU2022420976A1 (en) 2021-12-20 2022-12-20 Method of producing a cold compactible metallic powder
EP22908881.0A EP4444492A4 (fr) 2021-12-20 2022-12-20 Procédé de production d'une poudre métallique compactable à froid
JP2024537360A JP2025501551A (ja) 2021-12-20 2022-12-20 冷間成形可能な金属粉末を製造する方法
CN202280091388.3A CN118647475A (zh) 2021-12-20 2022-12-20 产生可冷压实的金属粉末的方法
CA3241509A CA3241509A1 (fr) 2021-12-20 2022-12-20 Procede de production d'une poudre metallique compactable a froid
KR1020247024379A KR20240128028A (ko) 2021-12-20 2022-12-20 냉간 압축성 금속 분말의 제조 방법
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EP0224659A2 (fr) * 1985-10-07 1987-06-10 Nara Machinery Co., Ltd. Méthode pour améliorer la qualité de la surface de particules solides et appareil à cet effet
WO1999008063A1 (fr) * 1997-08-08 1999-02-18 Remington Arms Company, Inc. Projectiles desintegrants a base de poudre de fer
US20200140979A1 (en) * 2015-12-24 2020-05-07 Rovalma, S.A. Long durability high performance steel for structural, machine and tooling applications

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JP3184355B2 (ja) * 1993-02-09 2001-07-09 住友特殊金属株式会社 焼結磁石用合金粉末及びその製造方法
DE102007044918A1 (de) * 2007-09-19 2009-04-09 Bayer Technology Services Gmbh Wasserstoffpermeable Membranen aus metallischem Verbundwerkstoff
WO2018122934A1 (fr) * 2016-12-26 2018-07-05 技術研究組合次世代３Ｄ積層造形技術総合開発機構 Poudre pour fabrication additive à base de métaux et son procédé de fabrication

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EP0224659A2 (fr) * 1985-10-07 1987-06-10 Nara Machinery Co., Ltd. Méthode pour améliorer la qualité de la surface de particules solides et appareil à cet effet
WO1999008063A1 (fr) * 1997-08-08 1999-02-18 Remington Arms Company, Inc. Projectiles desintegrants a base de poudre de fer
US20200140979A1 (en) * 2015-12-24 2020-05-07 Rovalma, S.A. Long durability high performance steel for structural, machine and tooling applications

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