EP0800882A2 - Procédé de préparation de granules et articles à partir de métal dur ou matériau cermet - Google Patents
Procédé de préparation de granules et articles à partir de métal dur ou matériau cermet Download PDFInfo
- Publication number
- EP0800882A2 EP0800882A2 EP97105701A EP97105701A EP0800882A2 EP 0800882 A2 EP0800882 A2 EP 0800882A2 EP 97105701 A EP97105701 A EP 97105701A EP 97105701 A EP97105701 A EP 97105701A EP 0800882 A2 EP0800882 A2 EP 0800882A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- binder
- hard material
- material phase
- granulate
- metal powder
- 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.)
- Withdrawn
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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
-
- 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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
- B22F3/1025—Removal of binder or filler not by heating only
-
- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/059—Making alloys comprising less than 5% by weight of dispersed reinforcing phases
-
- 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
Definitions
- the present method relates to a method for producing molded parts by injection molding of granules which consist of a material mixture of a hard material phase, a metal powder and an organic binder, and a method for producing such granules.
- Injection molded parts made of hard metal or cermet materials are produced by molding, debinding and sintering an injection molded granulate manufactured according to the needs of the individual case.
- Such methods have been widely described in the literature, e.g. in EP-A 0 413 231, 0 444 475, 0 446 708 and 0 465 940.
- the injection molding granulate is produced by mixing, for example kneading, a hard material phase and a metal component with an organic binder.
- the metal component regularly consists of a so-called binding metal, which leads to better adhesion of the particles of the hard material phase to one another.
- the metallic component and the hard phase have hitherto had to be mixed with one another before being mixed with the organic binder, in order later to obtain a homogeneous particle distribution in the granulate and, for example, to prevent the formation of "binder lakes”.
- This premixing is usually carried out by Grinding, for example in ball mills, usually using a solvent such as alcohol. The need for premixing is described, for example, in EP-B 0 443 048 and EP-B 0 516 165.
- the object of the present invention was therefore to provide a method for producing an injection molding granulate which is less technically complex, but which leads to comparably good results.
- the homogeneity of the granules and the resulting advantageous material properties of the molded part should be preserved as far as possible.
- At least one hard material phase is mixed with a metal powder and a binder and granulated with no premixing of the hard phase and the metal powder before mixing takes place with the binder and the binder has a viscosity of 20 to 200, preferably from 30 to 100 cm 3/10 min according to DIN 53735 at 195 ° C and 2.16 kg load weight.
- the metal powder is a so-called binder metal powder, which improves the adhesion of the particles to one another.
- Both the hard material phase and the metal phase can also consist of several different materials.
- the granules can also contain organic additives for dispersion and surface modification.
- wetting agents, plasticizers or other auxiliaries which influence the rheological properties of the granules during shaping can also be added to the granules.
- the premixing step of the metal component and the hard material phase can, contrary to expectations, be omitted.
- the flow properties of the granules during injection molding are also improved, as a result of which the shaping of complex parts is made considerably easier. Finally, the delivery time is significantly reduced.
- the mixing of the metal component and the hard material phase with the binder can in principle be carried out by all known relevant processes. Typically, the components are extruded or kneaded at temperatures of 150 to 200 ° C., then cooled and granulated.
- Binders which allow the premixing step to be dispensed with are, in particular, highly viscous binders which contain at least 70% by weight of at least one polyacetal, in particular of at least one polyoxymethylene or a polyoxymethylene homo- or copolymer consist of it.
- the viscosity is the first component of the binder of 25 to 50 cm 3/10 min according to DIN 53735 at 195 ° C and 2.16 kg load weight, thus resulting in the specified overall viscosity of the binder.
- Up to 30% by weight of further polymers can be used as the second component of the binder, preferably polybutanediol formal, polyethylene or polypropylene or a mixture of at least two of these polymers.
- Polybutanediol formal preferably has a relative molar mass of 6,000 to 80,000.
- Polyacetal binders which can be used with a suitable viscosity in the context of the invention have also been described in EP 413 231, EP 444 475, EP 446 708 and EP 465 940.
- the volume fraction of the binder in the granules is preferably 30 to 70%.
- a method is preferred in which a powder of at least one carbide, nitride or carbonitride of boron or a transition metal, in particular an element of group IVa, Va or VIa of the periodic table, is used as the hard material phase.
- At least one element or alloy powder of an element from the group Fe, Co, Ni, Cr, Mo, W, preferably Co, Ni or Cr is preferably used as the metal powder.
- Either the metal powder or the hard material phase or both powders preferably have an average grain size of less than 40 ⁇ m, preferably less than 20 ⁇ m.
- a method for producing molded parts by injection molding in which a granulate which has been produced using one of the above methods is shaped, debindered and sintered.
- the injection molded parts can be shaped by guiding the granules into molds using conventional screw or piston injection molding machines and at temperatures of typically 170 to 200.degree and is deformed at pressures between 200 and 2000 bar.
- the binder is preferably removed from the shaped green body in an atmosphere which contains acid, in particular oxalic acid, or boron trifluoride. This applies above all to polyacetal binders of the type described above. For other binders, other debinding conditions may be more favorable.
- the sintering is preferably carried out in an inert gas atmosphere, in a reducing atmosphere or in a vacuum.
- sintering can also be carried out under increased inert gas pressure.
- the sintering conditions must be tailored to the individual case, because these are of great importance for the correct setting of the carbon content in the molded part.
- the carbon content in turn is of crucial importance for the material properties obtained.
- a mixture of the following components was placed in a heatable kneader: 8,800 g of powdery WC which was doped with 0.1% by weight of NbC and had an average particle size of 2.2 ⁇ m; 1200 g of powdered Co with an average particle size of 1.6 microns; 40 g of polyethylene glycol with an average molecular weight of about 800; 35 g of polybutanediol formal with an average molecular weight of about 30,000; 850 g of polyoxymethylene with a proportion of 2% by weight of butanediol formal.
- This mixture was melted at 175 ° C. and homogenized for one hour. It was then cooled and granulated. The granules had a Melt Flow Index according to DIN 53735, measured at 190 ° C and load of 10 kg weight, of 27 cm 3/10 min.
- the granules were injection molded into moldings, which were then debindered in an oxalic acid / nitrogen gas atmosphere at 140 ° C.
- the rate of debinding was 1 mm / h, i.e. with each hour of the debinding process, the molded green part became free of binder all around at a depth of 1 mm.
- the three-point bending strength according to DIN ISO 3327 was 2200 MPa on samples "as fired".
- a mixture of the following components was placed in a heatable kneader: 8,800 g of powdery WC, which was doped with 0.1% by weight of NbC and had an average particle size of 2.2 ⁇ m, and 1200 g of powdery Co with a average particle size of 1.6 ⁇ m; 600 g of montan ester wax, which was so low-viscosity that it was not possible to measure the melt flow index, and 60 g of low-density polyethylene (LDPE) were added as binders.
- This mixture was melted at 120 ° C. and homogenized for one hour. It was then cooled and granulated. The granules had a Melt Flow Index according to DIN 53735, measured at 140 ° C and 2.16 kg load weight, of 21 cm 3/10 min.
- This granulate was injection molded into molded parts.
- the subsequent debinding was carried out as follows: heating the molded part in two steps, first to 350 ° C. at a rate of 10 K / h in a nitrogen atmosphere, then further to 650 ° C. at a rate of 50 K / h in vacuum (at most 0 , 7 mbar); Maintaining the temperature reached for 1 hour; Cooling down.
- the debindered moldings were then sintered in an inert gas atmosphere at 1450 ° C. This gave moldings with a density of 13.9 g / ml.
- the microstructure was not sufficiently homogeneous, "binding lakes” and pores were visible in microstructure images.
- the three-point bending strength according to DIN-ISO 3327 was 1530 MPa for the samples "as fired”.
- a mixture of 88% by weight WC powder and 12% by weight co-powder in alcohol was first wet-milled in a ball mill for 48 hours.
- the powder mixture was then dried and, as in the example according to the invention above, processed together with the other components specified therein to give a granulate.
- the Melt Flow Index of the granules was 16 cm 3/10 min, measured according to DIN 53735 at 190 ° C and 21.6 kg load weight.
- the granules were injection molded as in the example according to the invention.
- the molded green parts obtained were debindered under identical conditions as above, the speed being only 0.5 mm / h. After sintering, molded parts were obtained whose structure and properties were largely identical to the parts produced by the process according to the invention according to the example above.
- Comparative example 2 shows that the process according to the invention can be used to produce homogeneous molded parts which do not require premixing, which are also easier to debinding and have good strength. It is also advantageous that the granulate produced by the process according to the invention is more flowable, which is the formation of complex parts facilitated. Comparative example 1, on the other hand, shows that the premixing in binders customary hitherto can only be omitted with considerable losses in the homogeneity and strength of the molded parts.
Landscapes
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Powder Metallurgy (AREA)
- Glanulating (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19614006 | 1996-04-09 | ||
DE19614006A DE19614006A1 (de) | 1996-04-09 | 1996-04-09 | Verfahren zur Herstellung von Granulat und Formteilen aus Hartmetall- oder Cermet-Materialien |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0800882A2 true EP0800882A2 (fr) | 1997-10-15 |
EP0800882A3 EP0800882A3 (fr) | 1999-02-03 |
Family
ID=7790799
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97105701A Withdrawn EP0800882A3 (fr) | 1996-04-09 | 1997-04-07 | Procédé de préparation de granules et articles à partir de métal dur ou matériau cermet |
Country Status (7)
Country | Link |
---|---|
US (1) | US5860055A (fr) |
EP (1) | EP0800882A3 (fr) |
JP (1) | JPH1036901A (fr) |
KR (1) | KR970069940A (fr) |
CN (1) | CN1083016C (fr) |
DE (1) | DE19614006A1 (fr) |
TW (1) | TW397726B (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2496605C1 (ru) * | 2012-05-10 | 2013-10-27 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" | Способ введения пластификатора и устройство для его осуществления |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2955754B1 (ja) * | 1998-06-01 | 1999-10-04 | 有限会社モールドリサーチ | 金属粉末の射出成形用組成物と、その組成物を用いた射出成形及び焼結法 |
DE19855422A1 (de) | 1998-12-01 | 2000-06-08 | Basf Ag | Hartstoff-Sinterformteil mit einem nickel- und kobaltfreien, stickstoffhaltigen Stahl als Binder der Hartstoffphase |
CH694401A5 (de) | 1999-05-26 | 2004-12-31 | Basf Ag | Nickelarmer, molybdänarmer, biokompatibler, nicht Allergie auslösender, korrosionsbeständiger austenitischer Stahl. |
WO2001000897A1 (fr) | 1999-06-24 | 2001-01-04 | Basf Aktiengesellschaft | Acier austenitique a faible teneur en nickel |
US6355207B1 (en) * | 2000-05-25 | 2002-03-12 | Windfall Products | Enhanced flow in agglomerated and bound materials and process therefor |
US7326274B2 (en) * | 2001-10-18 | 2008-02-05 | Praxis Powder Technology, Inc. | Binder compositions and methods for binder assisted forming |
DE10244486A1 (de) * | 2002-09-24 | 2004-04-01 | Gkn Sinter Metals Gmbh | Mischung zur Herstellung von gesinterten Formteilen |
KR20080027171A (ko) * | 2006-09-22 | 2008-03-26 | 세이코 엡슨 가부시키가이샤 | 소결체의 제조방법 및 소결체 |
CN101764599B (zh) * | 2009-10-15 | 2015-04-29 | 常蔚科技(深圳)有限公司 | 一种传感器外壳及其制造方法 |
CN101764603B (zh) * | 2009-10-15 | 2015-01-28 | 常蔚科技(深圳)有限公司 | 一种传感器外壳及其制造方法 |
CN101764602B (zh) * | 2009-10-15 | 2015-07-01 | 常蔚科技(深圳)有限公司 | 一种传感器外壳及其制造方法 |
CN101764601B (zh) * | 2009-10-15 | 2015-09-30 | 常蔚科技(深圳)有限公司 | 一种传感器外壳及其制造方法 |
CN101764600B (zh) * | 2009-10-15 | 2015-04-29 | 常蔚科技(深圳)有限公司 | 一种传感器外壳及其制造方法 |
JP5830808B2 (ja) | 2010-03-24 | 2015-12-09 | 株式会社ニチリン | フッ素ゴムと合成ゴムとの加硫接着積層体 |
WO2015006697A1 (fr) | 2013-07-11 | 2015-01-15 | Heikkila Kurt E | Particule modifiée en surface et produits extrudés frittés |
CN106624634B (zh) * | 2016-12-07 | 2018-11-02 | 杭州正驰达精密机械有限公司 | 一种高比重钨合金自动锤的生产方法 |
CN114599466A (zh) * | 2019-12-24 | 2022-06-07 | 可隆塑胶株式会社 | 金属粉末注射成型用粘结剂组合物 |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4397889A (en) * | 1982-04-05 | 1983-08-09 | Gte Products Corporation | Process for producing refractory powder |
EP0114746A2 (fr) * | 1983-01-21 | 1984-08-01 | Celanese Corporation | Liants à base de polyacétals pour moulage par injection de matériaux céramiques |
US4624812A (en) * | 1983-01-21 | 1986-11-25 | Celanese Corporation | Injection moldable ceramic composition containing a polyacetal binder and process of molding |
EP0329475A2 (fr) * | 1988-02-18 | 1989-08-23 | Sanyo Chemical Industries Ltd. | Composition moulable |
EP0413231A2 (fr) * | 1989-08-16 | 1991-02-20 | BASF Aktiengesellschaft | Procédé pour la production d'un fritté moule inorganique |
EP0424739A2 (fr) * | 1989-10-24 | 1991-05-02 | BASF Aktiengesellschaft | ProcédÀ© de fabrication de préformes à partir de fibres métalliques ou céramiques |
EP0444475A2 (fr) * | 1990-02-21 | 1991-09-04 | BASF Aktiengesellschaft | Composition thermoplastique pour la préparation de compositions céramiques moulables |
EP0446708A2 (fr) * | 1990-03-08 | 1991-09-18 | BASF Aktiengesellschaft | Matières thermoplastiques pour la préparation d'articles métalliques |
EP0465940A2 (fr) * | 1990-07-07 | 1992-01-15 | BASF Aktiengesellschaft | Masses thermoplastiques pour la fabrication d'articles moulés métalliques |
US5279640A (en) * | 1992-09-22 | 1994-01-18 | Kawasaki Steel Corporation | Method of making iron-based powder mixture |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5603071A (en) * | 1989-09-14 | 1997-02-11 | Sumitomo Electric Industries, Ltd. | Method of preparing cemented carbide or cermet alloy |
US5665289A (en) * | 1990-05-07 | 1997-09-09 | Chang I. Chung | Solid polymer solution binders for shaping of finely-divided inert particles |
TW362999B (en) * | 1992-06-02 | 1999-07-01 | Advanced Materials Technplogies Pte Ltd | Injection-mouldable metal powder-binder feedstock and method of forming metal injection-moulded article |
US5332543A (en) * | 1992-08-26 | 1994-07-26 | Advanced Materials Technologies Pte Ltd | Method for producing articles from particulate materials using a binder derived from an idealized TGA curve |
EP1282166A3 (fr) * | 1993-09-16 | 2003-03-05 | Sumitomo Electric Industries, Ltd. | Boítier métallique pour dispositif à semi-conducteur ayant une haute conductivité thermique et un coéfficient de dilatation thermique similaire à celui du semiconducteur, et procédé pour sa fabrication |
JPH07173503A (ja) * | 1993-11-04 | 1995-07-11 | Kobe Steel Ltd | 粉末冶金用結合剤および粉末冶金用混合粉末 |
DE4408304A1 (de) * | 1994-03-11 | 1995-09-14 | Basf Ag | Sinterteile aus sauerstoffempfindlichen, nicht reduzierbaren Pulvern und ihre Herstellung über Spritzgießen |
US5641920A (en) * | 1995-09-07 | 1997-06-24 | Thermat Precision Technology, Inc. | Powder and binder systems for use in powder molding |
US5678165A (en) * | 1995-12-06 | 1997-10-14 | Corning Incorporated | Plastic formable mixtures and method of use therefor |
-
1996
- 1996-04-09 DE DE19614006A patent/DE19614006A1/de not_active Withdrawn
-
1997
- 1997-03-24 US US08/826,078 patent/US5860055A/en not_active Expired - Fee Related
- 1997-03-31 TW TW086104076A patent/TW397726B/zh not_active IP Right Cessation
- 1997-04-07 EP EP97105701A patent/EP0800882A3/fr not_active Withdrawn
- 1997-04-07 JP JP9087813A patent/JPH1036901A/ja not_active Withdrawn
- 1997-04-08 CN CN97110340A patent/CN1083016C/zh not_active Expired - Fee Related
- 1997-04-08 KR KR1019970012785A patent/KR970069940A/ko not_active Application Discontinuation
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4397889A (en) * | 1982-04-05 | 1983-08-09 | Gte Products Corporation | Process for producing refractory powder |
EP0114746A2 (fr) * | 1983-01-21 | 1984-08-01 | Celanese Corporation | Liants à base de polyacétals pour moulage par injection de matériaux céramiques |
US4624812A (en) * | 1983-01-21 | 1986-11-25 | Celanese Corporation | Injection moldable ceramic composition containing a polyacetal binder and process of molding |
EP0329475A2 (fr) * | 1988-02-18 | 1989-08-23 | Sanyo Chemical Industries Ltd. | Composition moulable |
EP0413231A2 (fr) * | 1989-08-16 | 1991-02-20 | BASF Aktiengesellschaft | Procédé pour la production d'un fritté moule inorganique |
EP0424739A2 (fr) * | 1989-10-24 | 1991-05-02 | BASF Aktiengesellschaft | ProcédÀ© de fabrication de préformes à partir de fibres métalliques ou céramiques |
EP0444475A2 (fr) * | 1990-02-21 | 1991-09-04 | BASF Aktiengesellschaft | Composition thermoplastique pour la préparation de compositions céramiques moulables |
EP0446708A2 (fr) * | 1990-03-08 | 1991-09-18 | BASF Aktiengesellschaft | Matières thermoplastiques pour la préparation d'articles métalliques |
EP0465940A2 (fr) * | 1990-07-07 | 1992-01-15 | BASF Aktiengesellschaft | Masses thermoplastiques pour la fabrication d'articles moulés métalliques |
US5279640A (en) * | 1992-09-22 | 1994-01-18 | Kawasaki Steel Corporation | Method of making iron-based powder mixture |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2496605C1 (ru) * | 2012-05-10 | 2013-10-27 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Национальный исследовательский технологический университет "МИСиС" | Способ введения пластификатора и устройство для его осуществления |
Also Published As
Publication number | Publication date |
---|---|
CN1167836A (zh) | 1997-12-17 |
TW397726B (en) | 2000-07-11 |
JPH1036901A (ja) | 1998-02-10 |
KR970069940A (ko) | 1997-11-07 |
EP0800882A3 (fr) | 1999-02-03 |
DE19614006A1 (de) | 1997-10-16 |
US5860055A (en) | 1999-01-12 |
CN1083016C (zh) | 2002-04-17 |
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