EP2292806B1 - Procédé de fabrication de composants en titane ou en alliage de titane à l'aide de la technologie MIM - Google Patents

Procédé de fabrication de composants en titane ou en alliage de titane à l'aide de la technologie MIM Download PDF

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Publication number
EP2292806B1
EP2292806B1 EP09167195A EP09167195A EP2292806B1 EP 2292806 B1 EP2292806 B1 EP 2292806B1 EP 09167195 A EP09167195 A EP 09167195A EP 09167195 A EP09167195 A EP 09167195A EP 2292806 B1 EP2292806 B1 EP 2292806B1
Authority
EP
European Patent Office
Prior art keywords
process according
powder
titanium
titanium alloy
boron
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.)
Not-in-force
Application number
EP09167195A
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German (de)
English (en)
Other versions
EP2292806A1 (fr
Inventor
Orley Milagres Ferri
Thomas Ebel
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.)
Helmholtz Zentrum Hereon GmbH
Original Assignee
Helmholtz Zentrum Geesthacht Zentrum fuer Material und Kustenforschung GmbH
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Application filed by Helmholtz Zentrum Geesthacht Zentrum fuer Material und Kustenforschung GmbH filed Critical Helmholtz Zentrum Geesthacht Zentrum fuer Material und Kustenforschung GmbH
Priority to EP09167195A priority Critical patent/EP2292806B1/fr
Priority to US12/849,360 priority patent/US20110033334A1/en
Publication of EP2292806A1 publication Critical patent/EP2292806A1/fr
Application granted granted Critical
Publication of EP2292806B1 publication Critical patent/EP2292806B1/fr
Not-in-force legal-status Critical Current
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Classifications

    • 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
    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
    • 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 present invention relates to a method for producing a titanium or titanium alloy component by MIM technology.
  • MIM stands for "Metal Injection Molding” and is a highly efficient manufacturing process for the production of small, complex and precise metal parts.
  • the MIM technology is one of the so-called powder metallurgical processes, in which no solid metal body, but fine powder is used as the starting material for the component to be produced. This powder is mixed with a plastic-containing binder and kneaded into the so-called "feedstock".
  • the feedstock is pressed under pressure on an injection molding machine into the injection mold (tool).
  • the resulting green part already has the final geometry, but must be freed from the binder in the following steps to obtain a pure metal part.
  • the binder is removed in a chemical and / or thermal process and "sintered" the component via sintering. According to current knowledge, it is mainly used for the production of stainless steel components.
  • Titanium and titanium alloys offer an excellent strength-to-weight ratio. These metals are absolutely non-magnetic, corrosion-resistant and seawater-proof. In addition, they are biocompatible and are very well suited for implants. This combination of properties leads to the use of titanium in aerospace, marine and medical engineering. However, titanium and titanium alloys are very difficult to process.
  • Titanium alloy powders are only occasionally commercially processed by means of MIM and are limited to applications which involve only a low component load since the fatigue strength is significantly lower than in the case of components produced from TiAl6V4 semi-finished products. It is believed that the existence of pores in the MIM components and a coarser microstructure are responsible for the lower fatigue strength of the titanium alloy powder components produced by MIM technology.
  • the object of the present invention is to provide a method for the production of components made of titanium or titanium alloy powders by means of MIM, which can be exposed to a high alternating load.
  • the object is achieved by a method in which a homogeneous mixture of boron powder having a particle size of less than 10 microns, preferably less than 5 microns, more preferably less than 2 microns and titanium powder and / or titanium alloy powder is prepared and binder with the homogeneous mixture of Boron and titanium powder and / or titanium alloy powder and optionally an aggregate are mixed in a kneader, the mixture is brought by injection molding to produce a green part in the form, the formed mass to produce a brown part is chemically and / or thermally debinded and the debindered mass is sintered at a temperature between 1000 ° C and 1600 ° C.
  • the amount of boron powder is chosen so that in the component, based on its total weight after sintering 0.05 wt.% To 1.5 wt.%, Preferably 0.1 wt.% To 1.0 wt.% Boron is present , Preferably, the sintering temperature is between 1000 ° C and 1600 ° C, more preferably between 1200 ° C and 1500 ° C, more preferably between 1300 ° C and 1450 ° C. In particular, at a temperature between 1300 ° C and 1450 ° C, a residual porosity of the component of less than 3%, based on the component volume achieved.
  • the residual porosity can be determined by measuring the density in relation to the density of the solid material or by geometric analysis of microstructures by microstructures.
  • the uptake of oxygen during the process should preferably be limited so that the sintered components have an oxygen content of less than 0.3% by weight, based on the total weight of the component, since otherwise the ductility of the components is impaired.
  • the mixing of boron powder and titanium powder and / or titanium alloy powder preferably takes place under a protective gas atmosphere.
  • the mixing of the binder with the homogeneous mixture of boron and titanium powder and / or titanium alloy powder and optionally an additive takes place under a protective gas atmosphere.
  • the protective gas used is preferably argon or helium, more preferably argon.
  • the sintering is preferably carried out in a high vacuum.
  • a getter material such as titanium may be present. The latter measures serve to minimize oxygen uptake during sintering by the brown parts.
  • the oxygen content of the sintered component is preferably determined by melt extraction analysis.
  • the titanium powder and / or titanium alloy powder typically has a particle size of less than 45 ⁇ m.
  • TiAl6V4 which was preferably produced by means of inert gas atomization, can be used as the titanium alloy powder.
  • the binder is preferably selected from thermoplastic or thermosetting polymers, thermo-gelling substances, waxes or surface-active substances or mixtures obtained therefrom. Preference is given to polyamides, polyoxymethylene, polycarbonate, styrene-acrylonitrile copolymers, polyimides, natural waxes and / or oils, thermosets, cyanates, polypropylenes, polyacetates, polyethylenes, ethylene-vinyl acetate copolymers, polyvinyl alcohols, polyvinyl chlorides, polystyrene, polymethyl methacrylates, anilines, mineral oils, agar , Glycerol, polyvinyl butyryls, polybutyl methacrylates, cellulose, oleic acids, phthalates, paraffin waxes, carnauba wax, ammonium polyacrylates, diglyceride stearates and oleates, glyceryl monostearates, irpropyl titanates, lithium ste
  • the binder comprises polyethylene, stearic acid, paraffin and carnauba wax.
  • the binder contains a polyethylene copolymer such as polyethylene-ethylene vinyl acetate copolymer (PEVA) or polyethylene-butylene-methyl acrylate copolymer (PBMA) and paraffin.
  • PEVA polyethylene-ethylene vinyl acetate copolymer
  • PBMA polyethylene-butylene-methyl acrylate copolymer
  • the green part in step (d) for producing a brown part is debindered chemically in a hydrocarbon, preferably hexane and / or heptane, and then preferably thermally at a temperature of preferably 300 ° C to 600 ° C, more preferably 400 ° C to 500 ° C.
  • the chemical debinding usually takes place at temperatures between ambient temperature and 60 ° C, preferably between 40 ° C and 50 ° C.
  • the invention will now be illustrated by the following non-limiting example.
  • the particle sizes are, unless stated otherwise, to maximum particle sizes.
  • the titanium alloy powder used was recovered by sieving.
  • This is homogeneously mixed under argon atmosphere with an amorphous boron powder having a particle size of less than 2 microns.
  • the powder mixture is further kneaded and granulated under argon atmosphere with the binder components PEVA and paraffin in a Z-blade kneader at a temperature of 120 ° C for 2 h to the feedstock.
  • the feedstock is processed on an Arburg 320S injection molding machine at a melt temperature between 100 ° C and 160 ° C to produce sample parts (here rods for tensile tests).
  • the green parts are chemically debinded in heptane at 40 ° C for 20 hours, while the wax content of the binder system is dissolved out.
  • the brown parts are placed in a high vacuum oven with ceramic-free lining and tungsten heater.
  • the residual binder is first thermally decomposed by a suitable temperature program under argon atmosphere and sucked by means of a vacuum pump, before the sintering of the metal powder takes place directly afterwards.
  • the sintering preferably takes place under vacuum at a pressure of 10 -4 mbar.
  • the sintering temperature is typically 1400 ° C, the sintering time 2 hours.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Claims (13)

  1. Procédé pour la fabrication d'un composant en titane ou en alliage de titane, dans lequel
    (a) on prépare un mélange homogène d'une poudre de bore avec une granulométrie de moins de 10 µm et d'une poudre de titane et/ou d'une poudre d'alliage de titane,
    (b) on mélange un liant avec le mélange homogène de poudre de bore et de titane et/ou de poudre d'alliage de titane ainsi qu'éventuellement un additif dans un malaxeur,
    (c) le mélange est mis en forme par moulage par injection pour la fabrication d'une pièce verte,
    (d) on soumet la masse mise en forme à un déliantage par voie chimique et/ou thermique pour la fabrication d'une pièce brune,
    (e) la masse déliantée est frittée à une température comprise entre 1000 °C et 1600 °C,
    la quantité de poudre de bore étant choisie de manière à ce que le composant contient 0,05 % en poids à 1,5 % en poids de bore par rapport au poids global du composant après frittage.
  2. Procédé selon la revendication 1, caractérisé en ce que la teneur en bore est comprise entre 0,1 % en poids et 1,0 % en poids.
  3. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la température de frittage est comprise entre 1300 °C et 1450 °C.
  4. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le mélange de poudre de bore et de poudre de titane et/ou de poudre d'alliage de titane est effectué sous atmosphère protectrice.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le mélange de liant avec le mélange homogène de poudre de bore et de poudre de titane et/ou de poudre d'alliage de titane est effectué sous atmosphère protectrice.
  6. Procédé selon la revendication 4 ou 5, caractérisé en ce que l'on utilise de l'argon ou de l'hélium en tant que gaz de protection.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le frittage est effectué sous vide poussé.
  8. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les composants frittés présentent une teneur en oxygène de moins de 0,3 % en poids, déterminée grâce à une analyse d'extraction en fusion.
  9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la poudre de titane et/ou la poudre d'alliage de titane présente une granulométrie de moins de 45 µm.
  10. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'on utilise du TiAl6V4 en tant que poudre d'alliage de titane.
  11. Procédé selon la revendication 10, caractérisé en ce que l'on utilise du TiAl6V4 atomisé au gaz.
  12. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le liant est sélectionné parmi des polymères thermoplastiques ou duroplastiques, des substances à thermogélification, des cires ou substances tensioactives ou des mélanges à base de ceux-ci.
  13. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la pièce verte est déliantée par voie chimique à l'étape (d) dans un hydrocarbure, de préférence de l'hexane et/ou de l'heptane, pour la fabrication d'une pièce brune.
EP09167195A 2009-08-04 2009-08-04 Procédé de fabrication de composants en titane ou en alliage de titane à l'aide de la technologie MIM Not-in-force EP2292806B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP09167195A EP2292806B1 (fr) 2009-08-04 2009-08-04 Procédé de fabrication de composants en titane ou en alliage de titane à l'aide de la technologie MIM
US12/849,360 US20110033334A1 (en) 2009-08-04 2010-08-03 Process for producing components composed of titanium or titanium alloy by means of mim technology

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP09167195A EP2292806B1 (fr) 2009-08-04 2009-08-04 Procédé de fabrication de composants en titane ou en alliage de titane à l'aide de la technologie MIM

Publications (2)

Publication Number Publication Date
EP2292806A1 EP2292806A1 (fr) 2011-03-09
EP2292806B1 true EP2292806B1 (fr) 2012-09-19

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Country Link
US (1) US20110033334A1 (fr)
EP (1) EP2292806B1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3524280A1 (fr) 2018-02-12 2019-08-14 Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH Procédé de production d'un implant métallique

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CN106062234A (zh) * 2013-10-25 2016-10-26 格尔登知识产权有限公司 用于粉末注射成型的含非晶态合金进料
CN105880583A (zh) * 2016-04-18 2016-08-24 四川大学 用于3d打印制作钛制品的复合丝材及其制备方法
US10851437B2 (en) 2016-05-18 2020-12-01 Carpenter Technology Corporation Custom titanium alloy for 3-D printing and method of making same
CN107876575A (zh) * 2016-09-30 2018-04-06 珠海天威飞马打印耗材有限公司 三维成型丝料、制造方法及成型方法
EP3655558A4 (fr) * 2017-07-18 2020-11-04 Carpenter Technology Corporation Alliage de titane à façon, ti-64, 23+
CN107868878A (zh) * 2017-12-28 2018-04-03 宁波俐辰新能源有限公司 一种本质耐磨钛合金及其制造方法
CN110421174A (zh) * 2019-07-30 2019-11-08 中山市金瓷科技有限公司 一种金属粉末注射成形不锈钢-铁基喂料配方及制作方法
CN113333752B (zh) * 2020-03-03 2022-10-25 湖南省民鑫新材料股份有限公司 一种钛及钛合金注射成形的喂料产品及其制备方法
CN111390185A (zh) * 2020-04-14 2020-07-10 东莞市金材五金有限公司 一种钛合金零件生产方法
CN113751708A (zh) * 2021-09-15 2021-12-07 西安航空职业技术学院 一种钛合金粉末注射成形专用料及其制备方法
CN114472879B (zh) * 2021-12-20 2023-04-25 中南大学 一种纯钛粉末注射成形用粘结剂及其制备方法和应用
CN114951662B (zh) * 2022-06-14 2023-05-05 浙江大学 制备高强度多孔钛合金材料的方法
US20240369458A1 (en) * 2023-05-03 2024-11-07 The Boeing Company Reference standards comprising known defects and methods for manufacturing such reference standards

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JP3542646B2 (ja) * 1994-01-27 2004-07-14 セイコーエプソン株式会社 歯科医療用材料及びその製造方法
WO2000006327A2 (fr) * 1998-07-29 2000-02-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Procede de production de composants par un procede de moulage par injection de poudre metallique
US6592695B1 (en) * 2000-11-16 2003-07-15 General Electric Company Binder system for ceramic arc discharge lamp
KR101237122B1 (ko) * 2003-12-11 2013-02-25 오하이오 유니버시티 티타늄 합금의 미세구조 정련 방법 및 티타늄 합금의 고온-고변형률 초가소성 성형방법

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3524280A1 (fr) 2018-02-12 2019-08-14 Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH Procédé de production d'un implant métallique

Also Published As

Publication number Publication date
EP2292806A1 (fr) 2011-03-09
US20110033334A1 (en) 2011-02-10

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