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WO2019118991A1 - Processus et procédé de production de blocs, de poudre sphérique et non sphérique de titane et d'alliage de titane - Google Patents

Processus et procédé de production de blocs, de poudre sphérique et non sphérique de titane et d'alliage de titane Download PDF

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Publication number
WO2019118991A1
WO2019118991A1 PCT/ZA2018/050063 ZA2018050063W WO2019118991A1 WO 2019118991 A1 WO2019118991 A1 WO 2019118991A1 ZA 2018050063 W ZA2018050063 W ZA 2018050063W WO 2019118991 A1 WO2019118991 A1 WO 2019118991A1
Authority
WO
WIPO (PCT)
Prior art keywords
titanium
billets
mould
feedstock
ingots
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/ZA2018/050063
Other languages
English (en)
Inventor
Ronald MACHAKA
Tebogo Matheti MOTSAI
Silethelwe CHIKOSHA
Christopher Nyongesa MACHIO
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.)
Council for Scientific and Industrial Research CSIR
Original Assignee
Council for Scientific and Industrial Research CSIR
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 Council for Scientific and Industrial Research CSIR filed Critical Council for Scientific and Industrial Research CSIR
Priority to NZ764309A priority Critical patent/NZ764309B2/en
Publication of WO2019118991A1 publication Critical patent/WO2019118991A1/fr
Priority to ZA2020/03526A priority patent/ZA202003526B/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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or 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
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/1208—Containers or coating used therefor
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/1208—Containers or coating used therefor
    • B22F3/1216—Container composition
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/1208—Containers or coating used therefor
    • B22F3/1216—Container composition
    • B22F3/1241—Container composition layered
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • 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
    • 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
    • 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
    • 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

Definitions

  • the invention relates to a process for producing titanium and titanium-based alloy billets, and spherical and non-spherical powders.
  • a titanium sponge is typically converted to titanium alloy products, including near net shape and mill products and powder products, by a series of processes.
  • the titanium sponge with alloying particles is provided in particle form. If needed, various alloying elements may be introduced in admixture with the sponge particles in desired amounts for producing titanium-base alloys. These unalloyed or admixtures are what we may call a starting feedstock material.
  • the feedstock material is typically pressed to compact the particles to form compacts or briquettes that are joined by welding to produce a consumable electrode.
  • the consumable electrodes are vacuum arc melted (VAR) to produce a dense titanium-based ingot.
  • the ingots are typically re-melted once or twice (double or triple VAR) to produce a final ingot.
  • the melting is commonly performed in a protective atmosphere such as vacuum and inert gas environments.
  • the re-melting is commonly performed twice in order to achieve sufficiently high chemical homogeneity and low porosity levels.
  • Alternatives to VAR melting processes include electro-slag, double electrode, electron beam, plasma melting and zone melting methods.
  • the ingot resulting from either double or triple vacuum arc melting is then typically processed by thermomechanical processing (a series of forging and annealing steps) to form from ingot products such as billets - often known as the wrought billets.
  • the wrought formed billet can either be forged or machined to a desired near-net shape product or worked further to produce mill products such as, but are not limited to, billets, bars, rods, wire, tubes, slabs, plates, sheets, and foils.
  • wrought formed billet can be the atomized to produce spherical powders.
  • the invention provides a process for producing both frangible and dense billets.
  • the billets may be produced by sintering loose powder in a mould of suitable shape.
  • the mould can be made from any suitable material, e.g. ceramic. Further, the mould can be encapsulated in an enclosure made from any suitable material, e.g. steel.
  • the sintering may be done in an open air or vacuum or argon furnace.
  • the frangible billets may be crushed and/or pulverized to non spherical powders.
  • the non spherical powders of the desired particle size distributions can find powder metallurgical applications. Further, suitable particle size distributions of the non spherical powders can be spheroidized into highly spherical powders using any commercially available plasma spheroidization equipment.
  • the dense billets may be atomized into highly spherical powders using any commercially available atomization equipment.
  • dense billets mean billets that can withstand handling without breaking. Their theoretical density can vary between 30 and 100%.
  • the powders so produced may possess similar characteristics to commercially available powders, but cost less, because the process described in this invention uses fewer steps than the current commercial process.
  • the process is not limited to any particular powder feedstock: it can be used with powders of different morphologies, and is amenable, but not limited to, titanium, titanium and its alloys. More specifically, so long as alloys contain titanium as a principal or alloying element, typically processed by way vacuum arc melted (VAR) or in any other protective environment, materials or alloys to which an uncontrolled or non-inert environment will introduce undesirable properties, other materials such as cermets and hybrid material systems.
  • VAR vacuum arc melted
  • the invention provides a process for producing dense titanium and titanium alloy billets or ingots through a melt-free solid-state sintering process, wherein the process comprises:
  • the mould capsule may be:
  • a ceramic mould such as, but not limited to, AI203, Y203, Zr02 moulds for sintering in inert environment; and/or
  • the invention extends to a method for producing a variety of titanium and titanium- based alloy mill products such as sheets, wires, seamless tubes, welded tubes, bars and forgings from the billets/ingots above using thermomechanical processing (rolling, extrusion, forging, or otherwise).
  • the invention extends to a method for producing a variety of titanium and titanium alloy spherical powders from said dense billets/ingots, using vacuum induction melting and gas atomizing (VIGA), plasma atomizing, and electrode induction melting gas atomization (EIGA).
  • VIGA vacuum induction melting and gas atomizing
  • EIGA electrode induction melting gas atomization
  • the invention extends to a method for producing a variety of titanium and titanium alloy shaped products, parts, or components from the dense billets/ingots using a machining processing such as turning or milling.
  • a melt-free solid- state homogenization process comprising:
  • a method for producing a variety of titanium and titanium alloy non-spherical powder from said frangible billets by way of crushing processes such as pulverizing, milling, mechanical alloying, etc.
  • the method for producing a variety of titanium and titanium alloy spherical powder from the non-spherical powder recovered from said frangible billets may use spheroidization or similar techniques, such as plasma-based spheroidization.
  • Embodiment 1 Method to produce dense titanium and titanium-based alloy billets/ingots through a melt-free solid-state sintering process
  • Embodiment 2 Method for producing a variety of titanium and titanium-based alloy mill products such as, but are not limited to, billets, bars, rods, wire, tubes, slabs, plates, sheets, and foils, from the billets/ingots from Embodiment 1 using thermomechanical processing (rolling, extrusion, forging, or otherwise);
  • Embodiment 3 Method for producing a variety of titanium and titanium-based alloy spherical powder from the dense billets/ingots from Embodiment 1 , using atomization techniques such as vacuum induction melting and gas atomizing (VIGA), plasma atomization and plasma rotating electrode process (PREP), and electrode induction melting gas atomization (EIGA);
  • Embodiment 4 Method for producing a variety of near net or net shaped titanium and titanium-based alloy products from the dense billets/ingots from Embodiment 1 using machining processing (e.g. turning or milling);
  • Embodiment 5 Method to produce frangible titanium and titanium-based alloy billets through a melt-free solid-state sintering-free homogenization process
  • Embodiment 6 Method for producing a variety of titanium and titanium-based alloy non-spherical powder from the frangible billets/ingots from Embodiment 5, by way of crushing processes (such as pulverizing, milling, mechanical alloying, etc.); and
  • Embodiment 7 Method for producing a variety of titanium and titanium-based alloy spherical powder from the frangible billets/ingots from Embodiment 6 using plasma-based spheroidization.
  • FIG 1 illustrates an approach for processing a starting feedstock material (Article 10) such as a titanium sponge is typically converted to titanium alloy products (Articles 20), including near-net shaped products, mill products and powder products, by a series of processes.
  • a starting feedstock material such as a titanium sponge
  • Articles 20 titanium alloy products
  • the process operations typically follow the following steps, the starting feedstock material a titanium sponge with either admixtures of alloy particles is provided in particle form if needed (Article 10).
  • the feedstock material is typically pressed to compact the particles to form compacts or briquettes that are joined as by welding to produce a consumable electrode (Step 12).
  • the pre-pressed consumable electrodes are vacuum arc melted (VAR) to produce a dense titanium-based ingot which is typically re-melted once or twice (double or triple VAR), in a protective atmosphere, to produce a final ingot.
  • VAR vacuum arc melted
  • the resulting ingot is then typically processed by a series of forging and annealing steps (thermomechanical processing) to form ingot products such as billets - often known as the wrought billets (Step 16).
  • the wrought formed billet can be processed further to produce a variety of titanium alloy products (Steps 18 and 20); i.e.
  • wrought formed billet can be atomized to produce spherical powders.
  • FIG. 2 depicts an approach for processing a starting feedstock material (Article 22), this can be a Ti sponge, TiHDH, T1H2, CP Ti, blends of (Ti sponge, TiHDH, T1H2, CP Ti), Ti-based alloys or blends of these with other alloying elements.
  • the feedstock material is introduced first in a suitably shaped mould (Step 24). While circumventing the conventional pre-pressing (Step 18) and said double or triple vacuum arc melting (Step 20), the feedstock material is then subjected to solid-state thermal processing (Step 30) in order to produce either dense billets/ingots (Article 32) or frangible billets (Article 34).
  • the solid-state thermal processing takes the form of sintering, above the beta transus temperature but below melting in the production of dense billet/ingot articles (32).
  • the dense ingots/billets (Article 32) can further be converted into mill products, machine shaped parts (Articles 36), or atomized spherical powders (Articles 38) as known and demonstrated in Figure 1.
  • the frangible billet (Article 34) can produce non-spherical powder (Articles 40) by way of crushing, pulverizing, milling, mechanical alloying or any other appropriate way and spherical powders (Article 42) by way of plasma-based spheroidization of the said non-spherical powder (Articles 40), respectively.
  • Articles 32, 34, 36, 38, 40 and 42 are also demonstrated in Figures (3 to 7) below, respectively.
  • FIG. 2 illustrates the implementations of the present invention and the current art.
  • Figure 2 demonstrates the circumvented costly aspects, of pre- compaction and melting (VAR), used in the current art for producing titanium and titanium-based billets and spherical powder.
  • VAR pre- compaction and melting
  • a frangible billet (Article 34) is shown in (4a) and (4b) shows the preparation of a titanium-based feedstock suitable for spheroidization.
  • a titanium-based spherical powder (Article 36) produced via the EIGA atomization of the solid state sintered dense billet (Article 32).
  • a mill product (Article 36) produced by cold rolling dense billet (24) is shown.
  • a non-spherical titanium-based alloy powder (a) which is produced from the frangible billets/ingots (Article 34);Ti6AI4V powder (Article 38) is shown as well one produced via spheroidization of powder from frangible billet (Article 34) in (b).
  • the first embodiment of this invention disclosure is the process for producing titanium and titanium alloy billets.
  • Our approach to producing titanium and titanium alloy billets and spherical powder from the said billets is schematically illustrated in Figure 2.
  • the implementation of the present invention specifically circumvents the compaction, vacuum arc re-melting and ingot breakdown forging steps which have become a standard in the titanium and titanium alloy production for more than 50 years and typically energy-intensive and requires a high-capital investment.
  • the said solid billets are produced by loading powder feedstock with particle sizes of up to a few millimetres into a mould.
  • the mould set-up is then placed in a furnace for heat treatment at temperatures ranging from 700°C to 1400°C for durations ranging from 15 minutes to 10 hours in a furnace with controlled environment, which can either be vacuum or argon.
  • a furnace with controlled environment which can either be vacuum or argon.
  • An open air furnace can also be used if the mould is encapsulated in a metal enclosure.
  • Other environments can be used depending on the feedstock powders.
  • the powder feedstock was titanium-based alloy.
  • the powder feedstock was titanium-based alloy.
  • the mill products defined here as rods, plates, sheets, billets, and bars can be produced therefrom via metal working fabrication processes as forging, rolling, and extrusion - these metal working fabrication processes are well established in the field.
  • the second embodiment of the present invention disclosure is the production of titanium and titanium alloy spherical powder from the dense billets (32) in Embodiment 1 , via gas atomization processes. Gas atomization is a well-known process and will not be described here. The constraint is that the billet (32) should have a suitable diameter and length. Embodiment 1 is able to produce these billets (32) because of the versatility of the process.
  • Figure 5 is an example of the spherical powders (Article 36 in Figure 2) that can be produced. The powders shown are Ti6AI4V (wt. %). Table 1 shows that the powders had a Ti6AI4V chemical composition.
  • Ti6AI4V powders ((Article 36), Figure 5) can be used for building
  • the third embodiment of the present invention disclosure is the production of titanium and titanium alloy spherical powder from the frangible billets (Article 34 in Figure 2) via the plasma spheroidization process.
  • Frangible Billet (Article 34) is crushed to form a feedstock material (Article 22) that is an irregular powder of up to 10mm.
  • the irregular powder is then pulverized in a suitable pulveriser for between 1 minute and 1 hour to reduce size to a suitable value, of between 5microns and 1000 microns.
  • This powder is then subjected to a plasma in a plasma spheroidization facility to produce powders with a spherical shape (morphology) ((Article 38) in Figure 2).
  • the Frangible Billet ((Article 34), Figure 3)) is produced as described for the Dense Billet (Article 32).

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention concerne un processus destiné à produire des blocs ou des lingots denses de titane ou d'alliage de titane au moyen d'un processus de frittage à l'état solide sans fusion ; le processus consistant en l'introduction d'un matériau de poudre de matières premières d'éponge de Ti, de TiHDH, de TiH2, de CP Ti, de leurs mélanges et/ou de mélange de ces derniers avec d'autres éléments d'alliage ; en l'introduction du matériau en poudre de matières premières dans une capsule de moule sans prépression du matériau ; et en la soumission de la capsule de moule à un traitement thermique à l'état solide pour produire un bloc/des lingots denses ou un bloc frangible sans atteindre le point de fusion du matériau de matières premières. L'invention s'étend à un procédé de production de blocs frangibles de titane et d'alliage de titane au moyen d'un processus d'homogénéisation à l'état solide sans fusion.
PCT/ZA2018/050063 2017-12-14 2018-12-04 Processus et procédé de production de blocs, de poudre sphérique et non sphérique de titane et d'alliage de titane Ceased WO2019118991A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
NZ764309A NZ764309B2 (en) 2018-12-04 A process and method for producing titanium and titanium alloy billets, spherical and non-spherical powder
ZA2020/03526A ZA202003526B (en) 2017-12-14 2020-06-12 A process and method for producing titanium and titanium alloy billets, spherical and non-spherical powder

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB1720892.7A GB2575005B (en) 2017-12-14 2017-12-14 A process and method for producing titanium and titanium alloy billets and spherical powder
GB1720892.7 2017-12-14

Publications (1)

Publication Number Publication Date
WO2019118991A1 true WO2019118991A1 (fr) 2019-06-20

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Country Status (3)

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GB (1) GB2575005B (fr)
WO (1) WO2019118991A1 (fr)
ZA (1) ZA202003526B (fr)

Cited By (7)

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CN111054914A (zh) * 2019-12-12 2020-04-24 航天海鹰(哈尔滨)钛业有限公司 一种电子束选区熔化成形用tc4钛合金粉末及其制备方法和应用
CN111644631A (zh) * 2020-06-10 2020-09-11 重庆材料研究院有限公司 球形钒粉的制备方法
CN113059172A (zh) * 2021-03-17 2021-07-02 东北大学 一种纳米多相增强钛基复合材料增材制造专用球形粉末的制造方法
CN113145852A (zh) * 2021-03-23 2021-07-23 长沙理工大学 一种新型3D打印医用TiNbZr球形合金粉的制备及3D打印的方法
CN115386758A (zh) * 2022-08-11 2022-11-25 西北工业大学 高氧钛轧板的制备方法
CN115921854A (zh) * 2022-12-13 2023-04-07 西安欧中材料科技有限公司 一种钛合金粉末的级配方法及应用
WO2023133911A1 (fr) * 2022-01-11 2023-07-20 郑州机械研究所有限公司 Procédé de préparation de poudre d'alliage sphérique à constituants multiples

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CN111644631A (zh) * 2020-06-10 2020-09-11 重庆材料研究院有限公司 球形钒粉的制备方法
CN111644631B (zh) * 2020-06-10 2023-04-18 重庆材料研究院有限公司 球形钒粉的制备方法
CN113059172A (zh) * 2021-03-17 2021-07-02 东北大学 一种纳米多相增强钛基复合材料增材制造专用球形粉末的制造方法
CN113145852A (zh) * 2021-03-23 2021-07-23 长沙理工大学 一种新型3D打印医用TiNbZr球形合金粉的制备及3D打印的方法
CN113145852B (zh) * 2021-03-23 2023-09-15 长沙理工大学 一种新型3D打印医用TiNbZr球形合金粉的制备及3D打印的方法
WO2023133911A1 (fr) * 2022-01-11 2023-07-20 郑州机械研究所有限公司 Procédé de préparation de poudre d'alliage sphérique à constituants multiples
CN115386758A (zh) * 2022-08-11 2022-11-25 西北工业大学 高氧钛轧板的制备方法
CN115386758B (zh) * 2022-08-11 2024-01-23 西北工业大学 高氧钛轧板的制备方法
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