EP2292806A1 - 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
EP2292806A1
EP2292806A1 EP09167195A EP09167195A EP2292806A1 EP 2292806 A1 EP2292806 A1 EP 2292806A1 EP 09167195 A EP09167195 A EP 09167195A EP 09167195 A EP09167195 A EP 09167195A EP 2292806 A1 EP2292806 A1 EP 2292806A1
Authority
EP
European Patent Office
Prior art keywords
powder
titanium
titanium alloy
boron
binder
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.)
Granted
Application number
EP09167195A
Other languages
German (de)
English (en)
Other versions
EP2292806B1 (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 Geesthacht Zentrum fuer Material und Kustenforschung GmbH
Original Assignee
GKSS Forshungszentrum Geesthacht GmbH
Helmholtz Zentrum Geesthacht Zentrum fuer Material und Kustenforschung GmbH
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 GKSS Forshungszentrum Geesthacht GmbH, Helmholtz Zentrum Geesthacht Zentrum fuer Material und Kustenforschung GmbH filed Critical GKSS Forshungszentrum Geesthacht 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
Anticipated expiration legal-status Critical

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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
    • 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
    • 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

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 chemically and / or thermally debindered shaped mass for producing a brown part 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.%, More preferably 0.1 wt.% To 1.0 wt.% Boron present is.
  • 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)
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 true EP2292806A1 (fr) 2011-03-09
EP2292806B1 EP2292806B1 (fr) 2012-09-19

Family

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Family Applications (1)

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EP09167195A Not-in-force 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

Country Status (2)

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
CN113333752A (zh) * 2020-03-03 2021-09-03 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

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015102732A2 (fr) * 2013-10-25 2015-07-09 Golden Intellectual Property, Llc Mélange-maître contenant un alliage amorphe pour moulage par injection de poudre
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
CN110997957A (zh) * 2017-07-18 2020-04-10 卡本特科技公司 定制钛合金，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
EP3524280B1 (fr) 2018-02-12 2020-01-08 Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH Procédé de production d'un implant métallique
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
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

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EP0664998A1 (fr) * 1994-01-27 1995-08-02 Injex Corporation Matériau pour le soin des dents et procédé pour sa fabrication
EP1119429B1 (fr) * 1998-07-29 2003-07-02 Gkss-Forschungszentrum Geesthacht Gmbh Procede de production de composants par un procede de moulage par injection de poudre metallique

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JP4890262B2 (ja) * 2003-12-11 2012-03-07 オハイオ ユニヴァーシティ チタン合金微細構造の精製方法および高温、高い歪み速度でのチタン合金の超塑性の形成

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
EP0664998A1 (fr) * 1994-01-27 1995-08-02 Injex Corporation Matériau pour le soin des dents et procédé pour sa fabrication
EP1119429B1 (fr) * 1998-07-29 2003-07-02 Gkss-Forschungszentrum Geesthacht Gmbh Procede de production de composants par un procede de moulage par injection de poudre metallique

Non-Patent Citations (1)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113333752A (zh) * 2020-03-03 2021-09-03 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

Also Published As

Publication number Publication date
EP2292806B1 (fr) 2012-09-19
US20110033334A1 (en) 2011-02-10

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