WO2012148714A1 - Low cost processing to produce spherical titanium and titanium alloy powder - Google Patents

Low cost processing to produce spherical titanium and titanium alloy powder Download PDF

Info

Publication number
WO2012148714A1
WO2012148714A1 PCT/US2012/033652 US2012033652W WO2012148714A1 WO 2012148714 A1 WO2012148714 A1 WO 2012148714A1 US 2012033652 W US2012033652 W US 2012033652W WO 2012148714 A1 WO2012148714 A1 WO 2012148714A1
Authority
WO
WIPO (PCT)
Prior art keywords
titanium
stream
alloy
powder
titanium alloy
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/US2012/033652
Other languages
English (en)
French (fr)
Inventor
James C. Withers
Raouf Loutfy
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.)
Materials and Electrochemical Research Corp
Original Assignee
Materials and Electrochemical Research Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Materials and Electrochemical Research Corp filed Critical Materials and Electrochemical Research Corp
Priority to CN201280020807.0A priority Critical patent/CN103608141A/zh
Priority to JP2014508399A priority patent/JP2014515792A/ja
Priority to AU2012250152A priority patent/AU2012250152B2/en
Priority to CA2834328A priority patent/CA2834328A1/en
Priority to EP12777501.3A priority patent/EP2701869B1/en
Priority to KR1020137031306A priority patent/KR20140027335A/ko
Publication of WO2012148714A1 publication Critical patent/WO2012148714A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848—Melting process before atomisation
    • 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
    • B22F2202/00—Treatment under specific physical conditions
    • B22F2202/01—Use of vibrations
    • 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

Definitions

  • the high cost of spherical titanium powder in large part is due to the high cost of conventional processing to produce alloyed titanium ingot from sponge that is then used to melt produce spherical titanium powder by one of several approaches.
  • State-of-the-art titanium processing is in very large scale and batch segregated operations.
  • Kroll sponge processing is carried out in large retorts producing approximately ten ton batches over many days of operation of adding TiCl 4 to the molten magnesium in the retort and draining resulting molten MgCl 2 from the retort followed by a week or more vacuum evaporation to remove the residual entrapped MgCl and unreacted Mg.
  • the vacuum purified sponge is then melted in very large skull type furnaces with the heat supplied by electron beams or plasmas. Alloying elements may then be added to the large ton size melts to produce desired alloy compositions such as Ti-6A1-4V which is then cast into ingots. Often triple melting is performed to attain uniform alloying. As a result, titanium ingot prices are quite cyclic that also influence the high cost of spherical titanium powder.
  • the present invention provides processes for producing low cost spherical titanium powder.
  • titanium sponge is conveyed to a plasma heating system into which is also conveyed a pre-alloy powder of desired alloying metals, e.g., aluminum and vanadium, or separately conveyed aluminum and vanadium powder may be separately conveyed to a plasma station where they are melted by the plasma to produce a pool or stream of molten uniform alloy of, e.g., Ti-6A1-4V in a continuous manner.
  • the molten alloy composition is dispersed by impinging a stream of inert gas across the surface of the pool or through the stream under controlled conditions, to blast droplets of the molten alloy which upon cooling produce spherical titanium alloy powder, e.g., Ti-6A1-4V.
  • the cost savings are significant. While the cost of titanium sponge is cyclic, its price in the 2010 - 2011 period was in the range of $3 to $ 10/lb and typically in the $4 - $6/lb range.
  • the cost to operate a plasma to melt the titanium alloy in a controlled pool size and generate spherical powder is in the range of approximately $1 - $2/lb which provides a basis to produce spherical Ti-6A1-4V powder from a typical sponge source in the range of $10 - $15/lb, which represents a significant saving over conventionally produced spherical titanium powder which, as noted supra, is in the $ 15071b cost range.
  • electrolytically produced titanium is conveyed to a plasma heated evaporator under inert atmospheric or under vacuum heated to 800 - 1600°C which rapidly evaporates the fused salt electrolyte that is returned to the electrolytic cell, and the remaining titanium is conveyed to a plasma heating station that supplies additional heat to melt and alloy the titanium analogous to the above discussed sponge feed with uniform spherical alloy powder being produced from the plasma heating station by dispensing the melt by impinging a stream of inert gas on the melt under controlled conditions to blast droplets of the molten alloy which upon cooling produce spherical powder of titanium alloy.
  • Electrolytic titanium can be produced for an estimated cost of approximately $1.50 - $2.50/lb which provides a basis for producing uniform spherical titanium alloy powder for under $ 10/lb.
  • the heat source for raising the salt-electrolytic titanium stream from approximately 500°C to over 900°C to rapidly and flash evaporate the salt can be conventional resistance, radiation, induction, microwave or plasma. Plasma heating typically is utilized for spherizing the liquid titanium into spherical powder.
  • the processes of the instant invention may be performed on a continuous basis with small segmental heating.
  • the quantity that is instantaneously heated is in the range of 10 g to 100 Kg and preferably in the range of 100 g to 10 Kg which is similar to the quantity of titanium that is being plasma melted and alloyed. Uniformity of alloying is achieved instantaneously in the small melt pools of the instant invention.
  • Figs. 1 is a schematic diagram and Fig. la is an enlarged view illustrating a process for producing spherical titanium powder in accordance with a first embodiment of the present invention
  • Fig. 2 is a schematic diagram illustrating a process for forming spherical alloy titanium particles in accordance with a second embodiment of the present invention
  • Fig. 3 is a schematic diagram illustrating a process for forming spherical alloy titanium particles in accordance with a third embodiments of the present invention
  • Fig. 4 is a scanning electron microscope photograph of spherical titanium alloy powder made in accordance with one embodiment of present invention.
  • Fig. 5 is a scanning electron microscope photograph of spherical titanium alloy powder made in accordance with another embodiment of the present invention.
  • Fig. 6 is a scanning electron microscope photograph of spherical titanium alloy powder made in accordance with a third embodiment of the present invention.
  • titanium sponge 14 is conveyed to a plasma transferred arc (PTA) welding torch of the type 10 shown in Fig. 1 of U.S. Application No. 2006/0185473-A 1 , the contents of which are incorporated herein by reference.
  • a pre-alloyed powder of aluminum- vanadium or a mixture of the elemental alloying elements was added to the plasma torch from a powder feeder 20 at a controlled rate to produce an alloy of Ti-6A 1 -4V.
  • a molten pool 22 of alloy Ti-6A1-4V approximately one-half inch in diameter by one- eighth inch to one-quarter inch deep is formed on a target substrate 24.
  • a stream of inert gas e.g.
  • argon was continuously blown from a nozzle 26 to impinge on the surface of the molten pool at 22, to blast droplets of molten alloy from the pool, which, upon cooling, solidify into spherical alloy particles.
  • Flow of the inert gas from nozzle 26 should be controlled to impinge on the surface of the molten pool at an angle of 45 to 180 degrees, and at a velocity of 10 to 1000 liters/min, to blast the molten alloy from the pool at the same rate as the pool is being formed.
  • the molten alloy is blown from the surface of the pool as fine droplets of essentially uniform size which cool almost instantaneously to form essentially uniform size particles of alloy which are deflected at particle collection baffle 28 and collected by gravity.
  • the target substrate 24 may be vibrated, e.g. by an ultrasonic horn or piezoelectric vibrator 200 (Fig. l a), to assist in lifting and dislodging of particles from the molten pool.
  • an ultrasonic horn or piezoelectric vibrator 200 Fig. l a
  • the molten titanium alloy stream from the PTA may be hit with a stream of argon gas to break the stream of titanium alloy particles into smaller particles which are then quenched into spherical powder in liquid argon.
  • TiCl 4 and Mg vapors are introduced into the reaction zone 110 of a fluid-bed reactor 112 where they can react by homogenous nucleation to produce small particles, typically under one micron, which are collected in a series of cyclones 114 designed to collect such small particles at the velocity of the reactor gas flow.
  • the small particles are recycled into the fluid-bed reactor reaction zone 110 where they are built up through additional deposition from TiCl 4 and Mg vapor reaction. Recycle is continued until the particles grow to a desirable size range of for example, 40 microns to 300 microns.
  • the extracted particles then were streamed to a shallow heated tank 118 to form a molten pool 120 of alloy.
  • a stream of argon 122 was blown through the stream, or over the surface of the molten pool to blast particles of titanium alloy, as before, which were withdrawn from the tank 118 via conduit 124.
  • a titanium powder is produced by magnesium reduction of TiCl 4 as described in my co- 2 pending application 12/016,859, the contents of which are incorporated herein by reference, in an electrolyte cell according to FIG. 2 of my aforesaid '859 application, at block 140.
  • a slurry stream of MgCl 2 containing titanium powder was produced, and was conveyed into a salt evaporation system 142 where the residual salt was evaporated by heating. Heating may be accomplished by resistance, induction, radiation, microwave or plasma under an inert atmosphere, which, if desired, may be at reduced pressure to aid evaporation.
  • the resulting titanium powder, along with alloying metal powder was conveyed into a PTA melting system similar to that shown on FIG. 1, and illustrated generally at block 144, where substantially uniform spherical alloy powder was produced by blasting droplets of molten alloy from the molten stream of alloy from the PTA, or collect up in a pool on the substrate, as before, and cooling and collecting solidified powder, as before.
  • Example 1 The process of Example 1 was repeated except the molten PTA produced melt pool was collected on a target having an orifice through which the molten titanium alloy dropped surrounded with a stream of argon gas. The molten alloy stream was broken into particles by the stream of argon gas, and the particles were quenched into spherical powder in liquid argon in the bottom of a powder catch container. The produced
  • Electrolytic titanium powder was produced by processing according to U.S. Patent Nos. 7,914,600, 7,410,562, and 7,794,580 or alternately by feeding titanium tetrachloride (TiCl 4 ) to a salt electrolyte containing KCl-LiCl.
  • TiCl 4 titanium tetrachloride
  • the titanium powder was produced in a continuous configured electrolytic system with an output pumped stream at approximately 500°C containing approximately 15% titanium powder and 75% liquid salt.
  • the electrolytic titanium powder-salt stream was pump conveyed to a shallow tank heated by induction to approximately 1000°C.
  • the tank had a slight vacuum of approximately 10 Torr which cleanly evaporated the KCl-LiCl salt in approximately three minutes.
  • the residual electrolytic titanium powder was conveyed along with aluminum and vanadium powder in a ratio to produce Ti-6A1-4V alloy in a plasma melt of blended titanium and Al-V powder against which was blown argon that produced spherical titanium alloy powder of Ti-6A1-4V as shown in Figure 6.
  • a standard Kroll reaction was run that produced titanium sponge. After draining the by-product MgCl 2 of residual unreacted Mg, the sponge with the residual MgCl 2 and Mg was conveyed directly into the plasma system described in Example 3 without pre- evaporating the residual MgCl 2 and Mg. The plasma melted the titanium and evaporated the MgCl 2 and Mg. Argon gas was blown through the plasma electrodes onto the surface of the melt, blasting droplets of liquid titanium, which were cooled and produced spherical titanium particles, which were collected as before.
  • Example 4 The process of Example 4 was repeated, except Al-V alloy or as separate powders were conveyed with the titanium sponge containing residual MgCl 2 and Mg, resulting in a titanium alloy powder being produced.
  • Titanium powder was produced using magnesium reduction of TiCI 4 as described in my co-pending application 12/016, 859 which produced a stream of MgCl 2 at approximately 800°C containing approximately 20% titanium powder.
  • a slurry stream was conveyed into the salt evaporation system described in Example 3.
  • the titanium powder along with chromium and molybdenum powder was conveyed into the PTA melting system as described in Examples 1 and 2 and spherical alloy powder by the Example 2 processing was produced consisting of Ti-5Cr- 2Mo.
  • particles of ⁇ -8 ⁇ 1- 1 Mo- 1 V alloy may be produced.
  • any titanium alloy composition can be produced in spherical alloy powder or alternatively as an ingot with the addition of alloying elements co- conveyed with the titanium powder to the plasma melter. It also is understood particulate that reacts or remains unreacted with the molten titanium can be added to be incorporated in the spherical titanium alloy powder.
  • a reactive powder example is titanium diboride that reacts to provide titanium boride on cooling, aluminum nitride to give titanium nitride and Al 3 Ti on cooling, or boron carbide to give titanium boride plus titanium carbide on cooling.
  • particles more stable than titanium include hafnium oxide or calcium oxide.
  • inert gases other than argon advantageously may be employed.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Powder Metallurgy (AREA)
PCT/US2012/033652 2011-04-27 2012-04-13 Low cost processing to produce spherical titanium and titanium alloy powder Ceased WO2012148714A1 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
CN201280020807.0A CN103608141A (zh) 2011-04-27 2012-04-13 用于制造球形钛和钛合金粉末的低成本方法
JP2014508399A JP2014515792A (ja) 2011-04-27 2012-04-13 球状チタンおよび球状チタン合金粉末を生成する低コスト処理法
AU2012250152A AU2012250152B2 (en) 2011-04-27 2012-04-13 Low cost processing to produce spherical titanium and titanium alloy powder
CA2834328A CA2834328A1 (en) 2011-04-27 2012-04-13 Low cost processing to produce spherical titanium and titanium alloy powder
EP12777501.3A EP2701869B1 (en) 2011-04-27 2012-04-13 LOW COST PROCESSING TO PRODUCE SPHERICAL TITANIUM ALLOY POWDER Ti6Al4V
KR1020137031306A KR20140027335A (ko) 2011-04-27 2012-04-13 구형 티타늄 및 티타늄 합금 파우더를 제조하기 위한 저비용 공정

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201161517871P 2011-04-27 2011-04-27
US61/517,871 2011-04-27

Publications (1)

Publication Number Publication Date
WO2012148714A1 true WO2012148714A1 (en) 2012-11-01

Family

ID=47066869

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2012/033652 Ceased WO2012148714A1 (en) 2011-04-27 2012-04-13 Low cost processing to produce spherical titanium and titanium alloy powder

Country Status (9)

Country Link
US (1) US8911529B2 (https=)
EP (1) EP2701869B1 (https=)
JP (1) JP2014515792A (https=)
KR (1) KR20140027335A (https=)
CN (1) CN103608141A (https=)
AU (1) AU2012250152B2 (https=)
CA (1) CA2834328A1 (https=)
PL (1) PL2701869T3 (https=)
WO (1) WO2012148714A1 (https=)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11241738B2 (en) 2018-06-12 2022-02-08 Korea Institute Of Science And Technology Metal powder manufacturing apparatus for metal 3D printer
EP4725624A1 (en) 2024-10-14 2026-04-15 Amazemet Spolka Z Ograniczona Odpowiedzialnoscia Method of atomization of powdered feedstock and device for atomization of powdered feedstock

Families Citing this family (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102322229B1 (ko) 2014-05-13 2021-11-05 더 유니버시티 오브 유타 리서치 파운데이션 실질적으로 구형인 금속 분말의 제조
JP6665118B2 (ja) * 2014-06-16 2020-03-13 コモンウェルス サイエンティフィック アンド インダストリアル リサーチ オーガナイゼーション 粉末生成物の製造方法
CN104209526B (zh) * 2014-08-26 2016-09-28 苏州智研新材料科技有限公司 一种微细球形钛合金粉体的制备方法
EP3227038A4 (en) 2014-12-02 2018-08-22 University of Utah Research Foundation Molten salt de-oxygenation of metal powders
US10987735B2 (en) 2015-12-16 2021-04-27 6K Inc. Spheroidal titanium metallic powders with custom microstructures
CA3009630C (en) * 2015-12-16 2023-08-01 Amastan Technologies Llc Spheroidal dehydrogenated metals and metal alloy particles
CN105537602A (zh) * 2015-12-25 2016-05-04 中国科学院重庆绿色智能技术研究院 一种3d打印用球形超高温合金粉末的快速规模化制备方法
CN105562700A (zh) * 2015-12-31 2016-05-11 龙岩紫荆创新研究院 一种用于3d打印的球形钛粉的等离子体制备方法
CN105568055B (zh) * 2016-01-06 2017-08-15 龙岩紫荆创新研究院 一种钛基合金球形粉末的等离子体制备方法
CN105642879B (zh) * 2016-01-14 2017-08-25 鞍山东大激光科技有限公司 用于激光3d打印的球形tc4钛合金粉末及其制备方法
CN105903973A (zh) * 2016-04-27 2016-08-31 龙岩紫荆创新研究院 一种球形钒粉的等离子体制备方法
CN110199039B (zh) 2016-10-21 2022-10-04 通用电气公司 通过还原四氯化钛制造钛合金材料
AU2017390111B2 (en) 2016-10-21 2021-12-09 General Electric Company Producing titanium alloy materials through reduction of titanium tetrahalide
CN106493377B (zh) * 2016-12-29 2018-05-11 哈尔滨三地增材制造材料有限公司 环形排布对撞式气流雾化钛合金粉末制取设备及制取方法
GB201701292D0 (en) * 2017-01-26 2017-03-15 Univ Ulster Method and apparatus for producing nanoscale materials
CN112654444A (zh) 2018-06-19 2021-04-13 6K有限公司 由原材料制造球化粉末的方法
KR102247338B1 (ko) 2018-12-14 2021-05-04 재단법인 포항산업과학연구원 입상 물질 제조 방법 및 제조 장치
US11066308B2 (en) 2019-02-05 2021-07-20 United Technologies Corporation Preparation of metal diboride and boron-doped powders
CN111590084B (zh) * 2019-02-21 2022-02-22 刘丽 一种金属粉体材料的制备方法
CN109750320B (zh) * 2019-03-04 2019-12-13 海安县鹰球粉末冶金有限公司 雾化电解联合制备金属合金粉末的方法
SG11202111576QA (en) 2019-04-30 2021-11-29 6K Inc Mechanically alloyed powder feedstock
CA3134579A1 (en) 2019-04-30 2020-11-05 Gregory Wrobel Lithium lanthanum zirconium oxide (llzo) powder
CN114641462A (zh) 2019-11-18 2022-06-17 6K有限公司 用于球形粉末的独特原料及制造方法
US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
CN113510246A (zh) * 2020-03-25 2021-10-19 中国科学院过程工程研究所 一种Ti-6Al-4V合金粉的制备方法及由其制得的Ti-6Al-4V合金粉
CA3180426A1 (en) 2020-06-25 2021-12-30 Richard K. Holman Microcomposite alloy structure
AU2021349358A1 (en) 2020-09-24 2023-02-09 6K Inc. Systems, devices, and methods for starting plasma
CA3196653A1 (en) 2020-10-30 2022-05-05 Sunil Bhalchandra BADWE Systems and methods for synthesis of spheroidized metal powders
CN112091229B (zh) * 2020-11-09 2021-02-12 西安赛隆金属材料有限责任公司 一种细化金属粉末粒径的装置及方法
AU2022206483A1 (en) 2021-01-11 2023-08-31 6K Inc. Methods and systems for reclamation of li-ion cathode materials using microwave plasma processing
WO2022212291A1 (en) 2021-03-31 2022-10-06 6K Inc. Systems and methods for additive manufacturing of metal nitride ceramics
WO2023229928A1 (en) 2022-05-23 2023-11-30 6K Inc. Microwave plasma apparatus and methods for processing materials using an interior liner
US12040162B2 (en) 2022-06-09 2024-07-16 6K Inc. Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows
WO2024044498A1 (en) 2022-08-25 2024-02-29 6K Inc. Plasma apparatus and methods for processing feed material utilizing a powder ingress preventor (pip)
US12195338B2 (en) 2022-12-15 2025-01-14 6K Inc. Systems, methods, and device for pyrolysis of methane in a microwave plasma for hydrogen and structured carbon powder production

Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1685908A (en) 1925-03-03 1928-10-02 Scovill Manufacturing Co Vanity case
US4544404A (en) * 1985-03-12 1985-10-01 Crucible Materials Corporation Method for atomizing titanium
US4602947A (en) * 1984-11-01 1986-07-29 Alti Corporation Process for producing titanium metal and titanium metal alloys
US4639281A (en) * 1982-02-19 1987-01-27 Mcdonnell Douglas Corporation Advanced titanium composite
US4999051A (en) * 1989-09-27 1991-03-12 Crucible Materials Corporation System and method for atomizing a titanium-based material
US5147448A (en) * 1990-10-01 1992-09-15 Nuclear Metals, Inc. Techniques for producing fine metal powder
US5213610A (en) * 1989-09-27 1993-05-25 Crucible Materials Corporation Method for atomizing a titanium-based material
US5332197A (en) * 1992-11-02 1994-07-26 General Electric Company Electroslag refining or titanium to achieve low nitrogen
US6425504B1 (en) * 1999-06-29 2002-07-30 Iowa State University Research Foundation, Inc. One-piece, composite crucible with integral withdrawal/discharge section
US20040123700A1 (en) * 2002-12-26 2004-07-01 Ling Zhou Process for the production of elemental material and alloys
US20050166706A1 (en) * 2003-08-20 2005-08-04 Withers James C. Thermal and electrochemical process for metal production
US20060185473A1 (en) 2005-01-31 2006-08-24 Materials & Electrochemical Research Corp. Low cost process for the manufacture of near net shape titanium bodies
US20070062332A1 (en) 2005-09-22 2007-03-22 Jones Robin M F Apparatus and method for clean, rapidly solidified alloys
US7297271B2 (en) 2001-02-16 2007-11-20 Sumitomo Titanium Corporation Titanium powder sintered compact
US7682556B2 (en) * 2005-08-16 2010-03-23 Ut-Battelle Llc Degassing of molten alloys with the assistance of ultrasonic vibration
US7794580B2 (en) 2004-04-21 2010-09-14 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US7914600B2 (en) 2007-01-22 2011-03-29 Materials & Electrochemical Research Corp. Continuous production of titanium by the metallothermic reduction of TiCl4

Family Cites Families (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4576642A (en) * 1965-02-26 1986-03-18 Crucible Materials Corporation Alloy composition and process
JPS59140307A (ja) * 1983-01-31 1984-08-11 Pioneer Electronic Corp 金属超微粒子の製造装置
JPS59166605A (ja) * 1983-03-11 1984-09-20 Tokyo Tekko Kk 超微粒子製造装置
JPS60194003A (ja) * 1984-03-13 1985-10-02 Hosokawa Funtai Kogaku Kenkyusho:Kk 金属微粒子製造法，並びに，装置
JPS61159501A (ja) * 1984-12-31 1986-07-19 Keisuke Honda 超音波による金属粉末の製造方法及び装置
JPS62103308A (ja) * 1985-10-30 1987-05-13 Hitachi Ltd 超微粒子の製造装置
US4731111A (en) * 1987-03-16 1988-03-15 Gte Products Corporation Hydrometallurical process for producing finely divided spherical refractory metal based powders
JPH02203932A (ja) * 1989-01-31 1990-08-13 Idemitsu Petrochem Co Ltd 超微粒子の製造方法及び製造装置
JPH03193805A (ja) * 1989-12-22 1991-08-23 Sumitomo Metal Ind Ltd 金属微粉末の生成方法
FI87896C (fi) * 1990-06-05 1993-03-10 Outokumpu Oy Foerfarande foer framstaellning av metallpulver
JPH0593213A (ja) * 1991-06-04 1993-04-16 Sumitomo Shichitsukusu Kk チタンおよびチタン合金粉末の製造方法
CN1191141C (zh) * 2000-04-26 2005-03-02 刘学晖 高纯气体超声雾化低氧钛及钛合金粉末制备方法及其产品
US6939389B2 (en) * 2003-08-08 2005-09-06 Frank Mooney Method and apparatus for manufacturing fine powders
US20070141374A1 (en) * 2005-12-19 2007-06-21 General Electric Company Environmentally resistant disk
JP4947690B2 (ja) * 2006-05-18 2012-06-06 株式会社大阪チタニウムテクノロジーズ チタン系合金球状粉末の製造方法
AU2008208040B2 (en) 2007-01-22 2012-03-01 Ats Mer, Llc Metallothermic reduction of in-situ generated titanium chloride
US8092570B2 (en) * 2008-03-31 2012-01-10 Hitachi Metals, Ltd. Method for producing titanium metal
CN101391306B (zh) * 2008-11-20 2012-01-25 核工业西南物理研究院 一种制备球形钛微粉或超微粉的装置和方法
CN101716686B (zh) * 2010-01-05 2011-02-16 北京科技大学 一种微细球形钛粉的短流程制备方法

Patent Citations (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1685908A (en) 1925-03-03 1928-10-02 Scovill Manufacturing Co Vanity case
US4639281A (en) * 1982-02-19 1987-01-27 Mcdonnell Douglas Corporation Advanced titanium composite
US4602947A (en) * 1984-11-01 1986-07-29 Alti Corporation Process for producing titanium metal and titanium metal alloys
US4544404A (en) * 1985-03-12 1985-10-01 Crucible Materials Corporation Method for atomizing titanium
US4999051A (en) * 1989-09-27 1991-03-12 Crucible Materials Corporation System and method for atomizing a titanium-based material
US5213610A (en) * 1989-09-27 1993-05-25 Crucible Materials Corporation Method for atomizing a titanium-based material
US5147448A (en) * 1990-10-01 1992-09-15 Nuclear Metals, Inc. Techniques for producing fine metal powder
US5332197A (en) * 1992-11-02 1994-07-26 General Electric Company Electroslag refining or titanium to achieve low nitrogen
US6425504B1 (en) * 1999-06-29 2002-07-30 Iowa State University Research Foundation, Inc. One-piece, composite crucible with integral withdrawal/discharge section
US7297271B2 (en) 2001-02-16 2007-11-20 Sumitomo Titanium Corporation Titanium powder sintered compact
US20040123700A1 (en) * 2002-12-26 2004-07-01 Ling Zhou Process for the production of elemental material and alloys
US20050166706A1 (en) * 2003-08-20 2005-08-04 Withers James C. Thermal and electrochemical process for metal production
US7410562B2 (en) 2003-08-20 2008-08-12 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US7794580B2 (en) 2004-04-21 2010-09-14 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US20060185473A1 (en) 2005-01-31 2006-08-24 Materials & Electrochemical Research Corp. Low cost process for the manufacture of near net shape titanium bodies
US7682556B2 (en) * 2005-08-16 2010-03-23 Ut-Battelle Llc Degassing of molten alloys with the assistance of ultrasonic vibration
US20070062332A1 (en) 2005-09-22 2007-03-22 Jones Robin M F Apparatus and method for clean, rapidly solidified alloys
US20090272228A1 (en) * 2005-09-22 2009-11-05 Ati Properties, Inc. Apparatus and Method for Clean, Rapidly Solidified Alloys
US7914600B2 (en) 2007-01-22 2011-03-29 Materials & Electrochemical Research Corp. Continuous production of titanium by the metallothermic reduction of TiCl4

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2701869A4

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11241738B2 (en) 2018-06-12 2022-02-08 Korea Institute Of Science And Technology Metal powder manufacturing apparatus for metal 3D printer
EP4725624A1 (en) 2024-10-14 2026-04-15 Amazemet Spolka Z Ograniczona Odpowiedzialnoscia Method of atomization of powdered feedstock and device for atomization of powdered feedstock

Also Published As

Publication number Publication date
PL2701869T3 (pl) 2017-02-28
EP2701869B1 (en) 2016-09-14
JP2014515792A (ja) 2014-07-03
US20120272788A1 (en) 2012-11-01
EP2701869A1 (en) 2014-03-05
US8911529B2 (en) 2014-12-16
CA2834328A1 (en) 2012-11-01
KR20140027335A (ko) 2014-03-06
CN103608141A (zh) 2014-02-26
AU2012250152B2 (en) 2016-08-04
EP2701869A4 (en) 2015-04-15
AU2012250152A1 (en) 2013-11-07

Similar Documents

Publication Publication Date Title
US8911529B2 (en) Low cost processing to produce spherical titanium and titanium alloy powder
JP2014515792A5 (https=)
US20220288684A1 (en) Methods and apparatuses for producing metallic powder material
US8092570B2 (en) Method for producing titanium metal
Sun et al. Review of the methods for production of spherical Ti and Ti alloy powder
US20080199348A1 (en) Elemental material and alloy
EP1543172B1 (en) Purification of metal particles by heat processing
EP1670961B1 (en) Methods and apparatuses for producing metallic compositions via reduction of metal halides
CN103221559B (zh) 金属钛制造装置和金属钛的制造方法
EP0444577B1 (en) Reactive spray forming process
EP1497061B1 (en) Powder formation method
CN111940730A (zh) 一种通过激光增材原位制备金属基复合材料的方法
US20080187455A1 (en) Titanium and titanium alloys
US20030061907A1 (en) Gel of elemental material or alloy and liquid metal and salt
US7435282B2 (en) Elemental material and alloy
US7445658B2 (en) Titanium and titanium alloys
KR101023225B1 (ko) 금속분말 제조방법
KR101127209B1 (ko) 반응층 생성물 분산처리장치 및 방법
KR101082124B1 (ko) 아크열을 이용하여 금속분말을 제조하는 장치 및 이를 이용하여 금속분말을 제조하는 방법
JPH10204507A (ja) ガスアトマイズ法による金属粉末の製造方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 12777501

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2014508399

Country of ref document: JP

Kind code of ref document: A

Ref document number: 2834328

Country of ref document: CA

NENP Non-entry into the national phase

Ref country code: DE

ENP Entry into the national phase

Ref document number: 2012250152

Country of ref document: AU

Date of ref document: 20120413

Kind code of ref document: A

ENP Entry into the national phase

Ref document number: 20137031306

Country of ref document: KR

Kind code of ref document: A

REEP Request for entry into the european phase

Ref document number: 2012777501

Country of ref document: EP