EP0853995B1 - Masse à moulage d'injection en contenant des oxides métalliques pour la fabrication d'objets en métaux - Google Patents

Masse à moulage d'injection en contenant des oxides métalliques pour la fabrication d'objets en métaux Download PDF

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Publication number
EP0853995B1
EP0853995B1 EP98100066A EP98100066A EP0853995B1 EP 0853995 B1 EP0853995 B1 EP 0853995B1 EP 98100066 A EP98100066 A EP 98100066A EP 98100066 A EP98100066 A EP 98100066A EP 0853995 B1 EP0853995 B1 EP 0853995B1
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EP
European Patent Office
Prior art keywords
powder
metal
hydrogen
molding
vol
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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.)
Expired - Lifetime
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EP98100066A
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German (de)
English (en)
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EP0853995A1 (fr
Inventor
Hans-Josef Dr. Sterzel
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BASF SE
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BASF SE
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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
    • 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
    • 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
    • B22F3/001—Starting from powder comprising reducible metal compounds
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the invention relates to molding compositions containing metal oxides, in particular Injection molding compositions which are suitable for the production of metal moldings, as well as processes for the production of metal moldings.
  • the binder is then removed from the molding thus formed, and the molding should not be deformed.
  • the binder can be removed in various ways. It is possible to thermally decompose the mostly organic binder by carefully increasing the temperature over a longer period of time and thus to remove it.
  • the binder can also be constructed so that it is partially soluble in a solvent and this portion can be extracted with the solvent. The further binder portion is then thermally decomposed, which can be done more quickly than in the first variant, because after the soluble binder portion has been extracted, an open-pored body is already present and the thermal decomposition therefore does not create any internal pressure which could destroy the molding.
  • the binder is most elegantly removed using a catalytic process, the binder used being, for example, a polyacetal which is directly depolymerized below its melting temperature under the influence of gaseous acids without the formation of a liquid phase to form gaseous formaldehyde.
  • This process runs from the outside to the inside of the molding walls, which means that the entire gas exchange can also only take place in the already porous parts by volume, and likewise no disadvantageous internal pressure can be built up.
  • This process has the further advantage that the debinding process takes place below the melting point of the binder, and the molding does not disadvantageously change its dimensions. Moldings which are very true to dimension are thus obtained.
  • the deviation of the linear dimensions from the target dimension is a maximum of +/- 0.3%, often less.
  • the roughness depths of the molded parts are essentially determined by the powder size used, so that roughness depths R Z of 1 ⁇ m are not undercut.
  • For the production of parts with smaller roughness metal powder would be of smaller diameter than 2 ⁇ m necessary.
  • the ratio of surface area to volume increases with decreasing particle size, which makes the metal powders more and more chemically reactive.
  • Base metals, such as iron, cobalt, zinc or nickel, become pyrophoric and cannot be processed in air.
  • the spraying of metal melts means that particle sizes of 5 ⁇ m are hardly exceeded. Often, the metal powders cannot be further crushed by grinding because they are too ductile.
  • US-A-4 415 528 relates to a process for the production of metal moldings by Injection molding.
  • nickel powder and iron powder are used Chromium oxide powder with a particle size of 0.5 ⁇ m mixed.
  • the LIGA process is used, for example, to produce tool inserts that are used to produce parts by injection molding that have dimensions in the ⁇ m range and roughness in the nanometer range.
  • a light-sensitive polymer layer is placed on a base plate, a so-called photoresist, applied and through a mask, which contains the structures to be produced in cross section.
  • the portions of the polymer layer exposed through the mask become soluble and can therefore be washed out.
  • the metal structure thus obtained can be used as a mold can be used for an injection mold.
  • the object of the invention is to provide molding compositions or injection molding compositions for the production of metal moldings that have a property profile have their use in very fine mold inserts, for example allowed from the LIGA process.
  • the shaped bodies obtained in this way are said to be in Fineness and surface quality of those produced using the LIGA process Conform shapes.
  • the object is achieved by molding compositions according to claim 9, containing in a flowable binder 20 to 50 vol .-%, based on the total volume of the molding composition, of a powder of one or more metal oxides and, if appropriate, metal carbides and / or metal nitrides which cannot be reduced with hydrogen, where at least 65% by volume of the powder have a particle size of at most 0.5 ⁇ m and the rest of the powder have a maximum particle size of 1 ⁇ m , and at least 90% by volume of the powder consist of metal oxides which can be reduced with hydrogen.
  • the present inventors have found that you can use instead of the large-grained, poorly accessible and difficult to handle metal powder, metal oxide powder with particle sizes below 1 ⁇ m for the production of the molding materials.
  • the molding compound or injection molding compound is shaped into a molding, the molding is debindered and sintered with a reduction in the metal oxides in a reducing atmosphere containing hydrogen.
  • a powder which has at least 65% by volume of a particle size of at most 0.5 ⁇ m , the rest of the powder having a particle size of at most 1 ⁇ m . Particularly preferably, at least 80% by volume of the powder have a particle size of at most 0.5 ⁇ m . At least 90% by volume of the powder consists of hydrogen-reducible metal oxides, the remaining portion of the powder consisting of hydrogen-reducible metal oxides, metal carbides and / or metal nitrides.
  • Suitable metal oxides are those which are reducible with hydrogen and are sinterable, so that they can be produced from them by heating under a hydrogen atmosphere or in the presence of hydrogen.
  • metals whose oxides can be used can be found in groups VIB, VIII, IB, IIB, IVA of the periodic table.
  • suitable metal oxides are Fe 2 O 3 , FeO, Fe 3 O 4 , NiO, CoO, Co 3 O 4 , CuO, Cu 2 O, Ag 2 O, WO 3 , MoO 3 , SnO, SnO 2 , CdO, PbO, Pb 3 O 4 , PbO 2 , Cr 2 O 3 .
  • the lower oxides are preferably used, such as Cu 2 O instead of CuO and PbO instead of PbO 2 , since the higher oxides are oxidizing agents which, under certain conditions, can react, for example, with organic binders.
  • the oxides can be used individually or as mixtures. For example, pure iron moldings or pure copper moldings can be obtained. When using mixtures of the oxides, alloys and doped metals are accessible, for example.
  • steel parts are produced from iron oxide / nickel oxide / molybdenum oxide mixtures and bronzes from copper oxide / tin oxide mixtures which may also contain zinc, nickel or lead oxide.
  • Particularly preferred metal oxides are iron oxide, nickel oxide and / or molybdenum oxide.
  • the metal oxides used in this invention having a particle size of not more than 1 ⁇ m, preferably not more than 0.5 ⁇ m, can be prepared by different methods, preferably prepared by chemical reactions.
  • the hydroxides, oxide hydrates, carbonates or oxalates, for example, can be precipitated from solutions of metal salts, the particles possibly being obtained in very fine particles in the presence of dispersants.
  • the precipitates are separated and brought to the highest possible purity by washing.
  • the precipitated particles are dried by heating and converted to the metal oxides at elevated temperatures.
  • the metal oxides or at least 65% by volume of the powder used according to the invention preferably have a BET surface area of at least 5, preferably at least 7 m 2 / g.
  • metal oxides that can be reduced with hydrogen
  • metal carbides metal nitrides that cannot be reduced with hydrogen
  • oxides ZrO 2 , Al 2 O 3 and TiO 2
  • carbides SiC, WC or TiC.
  • An example of a nitride is TiN.
  • the one used in the molding compositions according to the invention Powder has at least 90% by volume, particularly preferably at least 95% by volume, based on the powder, on hydrogen-reducible metal oxides. If metal oxides, metal carbides and / or not reducible with hydrogen Metal nitrides are used, they are preferably in amounts of 1 to 10, particularly preferably 2 to 5% by volume, based on the powder, in front.
  • the powder used according to the invention is present in the molding compositions in quantities from 20 to 50% by volume, preferably 25 to 45% by volume, particularly preferably 30 to 40 vol .-%, based on the total volume of the molding compound.
  • the powder used in the molding compositions according to the invention is distributed in a flowable binder. If necessary, additional a dispersant can be used. According to a preferred embodiment
  • the invention consists of the molding composition from that described above Powder, a flowable binder and optionally a dispersant.
  • the molding compound has In addition to these components, other components as described below are described.
  • binders which are suitable for use in the powder injection molding process can be used as flowable binders. They are preferably flowable at the processing temperature so that they can be injection molded into molds.
  • the binders described above in the prior art can be used. It is therefore possible to use binders which are thermally decomposed and thus removed, binder mixtures, some of which can be extracted with solvents and the other part can be thermally decomposed, or binders which are used, for example, in the form of a polyacetal which is below its melting temperature below the influence of gaseous acids can be depolymerized directly to gaseous products without the formation of a liquid phase. Suitable binders are known to the person skilled in the art.
  • the flowable binder preferably contains an organic polymer.
  • a polyoxymethylene copolymer is used in the molding composition according to claim 9, as described, for example, in EP-A-0 444 475, EP-A-0 446 708 and EP-A-0 444 475. It is preferably a polyoxymethylene copolymer which contains 0.5 to 10, preferably 1 to 5 mol% of butanediol formal as comonomer. Polybutanediol formal can be used as an additional binder.
  • All dispersants used for Dispersion of metal oxide particles of the specified particle size in Binders are suitable.
  • a suitable class of substances for the dispersants are alkoxylated fatty alcohols or alkoxylated fatty acid amides.
  • suitable ingredients of the molding compositions are those during processing processing stabilizers used by polyoxymethylene.
  • the molding compositions according to the invention are for injection molding usable from metal moldings. It is used to manufacture the Molding the organic and inorganic components in suitable Mixers mixed. This is preferably done in a kneading device while melting the flowable binder. After solidification the molding compositions are preferably granulated. You can be injection molded by known methods, preferably at melt temperatures from 170 to 200 ° C. The shape used preferably has a temperature of 120 to 140 ° C.
  • the binder is then removed from the moldings thus obtained. Depending on the binder used, this can be done by slowly heating, Treat with a solvent and then heat or Treat with an acid and heat up. This is preferably done Debinder simultaneously with heating to reduce and sinter the Shaped.
  • the molding in the presence of hydrogen is preferred under hydrogen atmosphere, at a rate of 1 to 20 ° C / min, preferably 2 to 10 ° C / min to the material-specific sintering temperature heated, 1 to 20, preferably 2 to 10 hours at Leave the sintering temperature and then cool down. During the slow The binder is removed by heating.
  • the one used for reduction Hydrogen preferably has a maximum dew point of -10 ° C, particularly preferably from less than -40 ° C. The dew point will be chosen so that a reduction under the Reaction conditions is possible.
  • an extremely dry hydrogen with a dew point of less than -40 ° C is required.
  • the reduction is carried out at temperatures above 1500 ° C., particularly preferably above 1600 ° C.
  • the alloy components often sinter at 1200 to 1300 ° C, while when using Cr 2 O 3 this can still remain in the molding unreduced.
  • the chromium content is therefore preferably used as ferrochrome with a particle size of the particles of at most 1 ⁇ m .
  • the volume fraction of the ferrochrome is preferably less than 35% by volume. It is thus possible to produce stainless steels alloyed with chromium and, if appropriate, nickel and molybdenum, without fear that non-reduced Cr 2 O 3 remains in the otherwise already sintered molding.
  • the invention also relates to a method for producing molded metal bodies by injection molding a molding compound as described above is, in a form, removal of the binder from the thus obtained Molding and reducing and sintering the debindered molding into one Shaped metal body in the presence of hydrogen.
  • the removal takes place of the binder preferably thermally in one step with the reducing and sintering by heating the molding to the sintering temperature in Presence of hydrogen.
  • the moldings shrink up to 5 times, based on volume or up to half based on linear Dimensions.
  • This high shrinkage is just for making very Small structures are an advantage because the injection mold is about the Factor 2 can be made larger in every dimension and therefore very large fine details can be formed.
  • the dimensional tolerances of the sintered Moldings are preferred despite the high absolute shrinkage maximum +/- 0.3%, particularly preferably +/- 0.15%.
  • the surface roughness R Z is preferably less than 1 ⁇ m, R a less than 0.2 ⁇ m, measured according to DIN 4768 or DIN 4768/1.
  • injection molding compounds listed in the examples below were Manufactured according to a uniform procedure, thermally debindered and when the material is adequate Sintering reducing temperatures under hydrogen.
  • thermoplastic polyoxymethylene copolymer which contained 2 mol% of butanediol formal as a comonomer and had a melt index of about 45 g / 10 min at 190 ° C. and 2.16 kg coating weight was used as the flowable binder.
  • Solsperse® 17000 from ICI was used as the dispersant for dispersing the inorganic powders. The amounts are given in the table below.
  • the organic and inorganic components of the molding compound were in a paddle mixer of 1 l useful content melted at 190 ° C and for Kneaded for 90 min. The paddle mixer was then cooled and the mass solidified and granulated in the rotating kneader.
  • the so obtained Injection molding compounds were at 180 ° C melt temperature in a to 130 ° C tempered mold for a bending rod with the dimensions 1.5 x 6 x 50 mm injected.
  • the bending bars produced in this way were heated up in a tube furnace under a hydrogen atmosphere (hydrogen with a dew point around -10 ° C.) at a rate of 2 ° C./min to the specified material-specific sintering temperature and left at the sintering temperature for 2 hours. The oven was then cooled. During the slow heating process, the polyoxymethylene and the polybutanediol formal depolymerized in the temperature range from 220 to 300 ° C. without the formation of cracks in the thin-walled bending rod.
  • the flexural bars were supported on a powder bed of alumina powder with about 5 ⁇ m particle size, in order to facilitate the shrinking.
  • the surface roughness values obtained with a polished injection mold were in any case less than 1 ⁇ m for R Z and less than 0.2 ⁇ m for R a .

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Claims (10)

  1. Utilisation de masses à mouler, contenant, dans un agent liant pouvant s'écouler, 20 à 50 % en volume, par rapport au volume total de la masse à mouler, d'une poudre constituée d'un ou plusieurs oxydes de métal et, le cas échéant, de carbures de métal ne pouvant pas être réduits avec de l'hydrogène et/ou de nitrures de métal ne pouvant pas être réduits avec de l'hydrogène, au moins 65 % en volume de la poudre présentant une taille de particules d'au maximum 0,5 µm et le reste de la poudre présentant une taille de particules d'au maximum 1 µm, et au moins 90 % en volume de la poudre étant constituée d'oxydes de métal pouvant être réduits avec de l'hydrogène, comme masses d'injection par pulvérisation pour la préparation de corps moulés métalliques.
  2. Utilisation selon la revendication 1, caractérisée en ce qu'au moins 65 % en volume de la poudre de la masse à mouler présente une surface BET d'au moins 5 m2/g.
  3. Utilisation selon la revendication 1 ou 2, caractérisée en ce que l'agent liant pouvant s'écouler de la masse à mouler contient un polymère organique.
  4. Utilisation selon l'une quelconque des revendications 1 à 3, caractérisée en ce que la masse à mouler contient un agent dispersant pour la poudre.
  5. Utilisation selon l'une quelconque des revendications 1 à 4, caractérisée en ce qu'on utilise dans la masse à mouler, comme oxydes de métal pouvant être réduits avec de l'hydrogène, du Fe2O3, du FeO, du Fe3O4, du NiO, du CoO, du Co3O4, du CuO, du Cu2O, de l'Ag2O, du Bi2O3, du WO3, du MoO3, du SnO, du SnO2, du CdO, du PbO, du Pb3O4, du PbO2, du Cr2O3 ou des mélanges de ceux-ci.
  6. Utilisation selon l'une quelconque des revendications 1 à 5, caractérisée en ce que la poudre dans la masse à mouler contient 1 à 10 % en volume d'oxydes de métal ne pouvant pas être réduits avec de l'hydrogène, de carbures de métal ne pouvant pas être réduits avec de l'hydrogène, de nitrures de métal ne pouvant pas être réduits avec de l'hydrogène ou de leurs mélanges, avec une taille de particules d'au maximum 0,5 µm.
  7. Procédé pour la préparation de corps moulés métalliques par moulage par injection dans une forme d'une masse à mouler, telle qu'elle est définie dans l'une quelconque des revendications 1 à 6, élimination de l'agent liant de la pièce moulée ainsi obtenue et réduction et frittage de la pièce moulée sans agent liant en un corps moulé métallique en présence d'hydrogène.
  8. Procédé selon la revendication 7, caractérisé en ce que l'élimination de l'agent liant est réalisée thermiquement en une étape avec la réduction et le frittage par chauffage de la pièce moulée à la température de frittage en présence d'hydrogène.
  9. Masse à mouler, contenant, dans un agent liant pouvant s'écouler constitué d'un copolymère de polyoxyméthylène et, le cas échéant, en outre de butanediolformal, 20 à 50 % en volume, par rapport au volume total de la masse à mouler, d'une poudre constituée d'un ou de plusieurs oxydes de métal et, le cas échéant, de carbures de métal ne pouvant pas être réduits avec de l'hydrogène et/ou de nitrures de métal ne pouvant pas être réduits avec de l'hydrogène, au moins 65 % en volume de la poudre présentant une taille de particules d'au maximum 0,5 µm et le reste de la poudre présentant une taille de particules d'au maximum 1 µm, et au moins 90 % en volume de la poudre étant constituée d'oxydes de métal pouvant être réduits avec de l'hydrogène.
  10. Masse à mouler selon la revendication 9, caractérisée en ce que le copolymère de polyoxyméthylène contient 0,5 à 10 % en mole de butanediolformal comme comonomère.
EP98100066A 1997-01-07 1998-01-05 Masse à moulage d'injection en contenant des oxides métalliques pour la fabrication d'objets en métaux Expired - Lifetime EP0853995B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19700277A DE19700277A1 (de) 1997-01-07 1997-01-07 Metalloxide enthaltende Spritzgießmassen zur Herstellung von Metallformkörpern
DE19700277 1997-01-07

Publications (2)

Publication Number Publication Date
EP0853995A1 EP0853995A1 (fr) 1998-07-22
EP0853995B1 true EP0853995B1 (fr) 2001-11-21

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EP98100066A Expired - Lifetime EP0853995B1 (fr) 1997-01-07 1998-01-05 Masse à moulage d'injection en contenant des oxides métalliques pour la fabrication d'objets en métaux

Country Status (8)

Country Link
US (1) US6080808A (fr)
EP (1) EP0853995B1 (fr)
JP (1) JPH10298606A (fr)
KR (1) KR100516081B1 (fr)
AT (1) ATE209076T1 (fr)
DE (2) DE19700277A1 (fr)
ES (1) ES2168690T3 (fr)
TW (1) TW495532B (fr)

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DE10014403A1 (de) * 2000-03-24 2001-09-27 Wolfgang Kochanek Verfahren zur Fertigung von Metallteilen
US6641776B1 (en) 2000-11-15 2003-11-04 Scimed Life Systems, Inc. Method for preparing radiopaque surgical implement
WO2004089563A1 (fr) * 2003-04-03 2004-10-21 Taisei Kogyo Co., Ltd. Procede de production de moulage de poudre frittee et moulage de poudre frittee, procede de production de moulage de poudre par injection, et moulage de poudre par injection, et matrice pour moulage de poudre par injection
KR100966754B1 (ko) * 2008-01-31 2010-06-29 한양대학교 산학협력단 환원-소결 일체형 공정을 통한 나노 금속 소결체 제조 방법
KR20140121473A (ko) 2012-02-02 2014-10-15 바스프 에스이 열가소성 ｐｏｍ 조성물
TW201500443A (zh) 2013-04-18 2015-01-01 Basf Se 聚甲醛共聚物及熱塑性ｐｏｍ組成物
US10961384B2 (en) 2014-05-21 2021-03-30 Basf Se Process for improving the flexural toughness of moldings
JP6848521B2 (ja) * 2017-02-24 2021-03-24 セイコーエプソン株式会社 金属粉末射出成形用コンパウンド、焼結体の製造方法および焼結体
EP4036167A1 (fr) * 2019-12-24 2022-08-03 Kolon Plastics, Inc. Composition de liant pour moulage par injection de poudre métallique

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US4421660A (en) * 1980-12-15 1983-12-20 The Dow Chemical Company Colloidal size hydrophobic polymers particulate having discrete particles of an inorganic material dispersed therein
US4415528A (en) * 1981-03-20 1983-11-15 Witec Cayman Patents, Limited Method of forming shaped metal alloy parts from metal or compound particles of the metal alloy components and compositions
US4604259A (en) * 1983-10-11 1986-08-05 Scm Corporation Process for making copper-rich metal shapes by powder metallurgy
JP2842536B2 (ja) * 1988-08-31 1999-01-06 三菱化学株式会社 樹脂組成物
DE4026965A1 (de) * 1990-08-25 1992-02-27 Basf Ag Versinterbare pulver enthaltende, vergiessbare formmasse
WO1993005190A1 (fr) * 1991-09-04 1993-03-18 Nihon Millipore Kogyo Kabushiki Kaisha Procede pour la production de corps metalliques poreux
JPH05254945A (ja) * 1992-03-13 1993-10-05 Hitachi Ltd 反応焼結セラミックスの製造法
US5686676A (en) * 1996-05-07 1997-11-11 Brush Wellman Inc. Process for making improved copper/tungsten composites

Also Published As

Publication number Publication date
ATE209076T1 (de) 2001-12-15
US6080808A (en) 2000-06-27
DE19700277A1 (de) 1998-07-09
TW495532B (en) 2002-07-21
KR100516081B1 (ko) 2005-12-06
ES2168690T3 (es) 2002-06-16
DE59802182D1 (de) 2002-01-03
KR19980070378A (ko) 1998-10-26
JPH10298606A (ja) 1998-11-10
EP0853995A1 (fr) 1998-07-22

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