WO1999064191A1 - Procede de production de poudre metallique - Google Patents
Procede de production de poudre metallique Download PDFInfo
- Publication number
- WO1999064191A1 WO1999064191A1 PCT/JP1999/003087 JP9903087W WO9964191A1 WO 1999064191 A1 WO1999064191 A1 WO 1999064191A1 JP 9903087 W JP9903087 W JP 9903087W WO 9964191 A1 WO9964191 A1 WO 9964191A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- metal powder
- gas
- metal
- producing
- powder
- Prior art date
Links
- 239000000843 powder Substances 0.000 title claims abstract description 105
- 239000002184 metal Substances 0.000 title claims abstract description 84
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 47
- 238000001816 cooling Methods 0.000 claims abstract description 29
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006722 reduction reaction Methods 0.000 claims description 43
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 30
- 230000002776 aggregation Effects 0.000 abstract description 8
- 239000011163 secondary particle Substances 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 239000002923 metal particle Substances 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 238000011946 reduction process Methods 0.000 abstract 2
- 238000005660 chlorination reaction Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000000112 cooling gas Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- JQGGAELIYHNDQS-UHFFFAOYSA-N Nic 12 Natural products CC(C=CC(=O)C)c1ccc2C3C4OC4C5(O)CC=CC(=O)C5(C)C3CCc2c1 JQGGAELIYHNDQS-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- -1 and in particular Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
Definitions
- the present invention relates to a conductive paste filler used for electronic components such as multilayer ceramic capacitors, a joining material of Ti material, and a metal powder such as Ni, Cu or Ag suitable for various uses such as a catalyst. And a method for producing the same. Background technology
- Conductive metal powders such as Ni, Cu, and Ag are useful for forming internal electrodes of multilayer ceramic capacitors, and in particular, Ni powder has recently attracted attention as such an application, and in particular, dry manufacturing methods.
- the ultra-fine Ni powder produced by the company is promising. With the demand for thinner and lower resistance internal electrodes as capacitors become smaller and larger in capacity, ultrafine powder with a particle size of 1 m or less and a particle size of 0.5 / _im or less is required. You.
- Japanese Patent Publication No. 59-77 No. 65 discloses a method in which solid nickel chloride is heated and evaporated to form nickel chloride vapor, and hydrogen gas is sprayed at a high speed to grow nuclei in an unstable interface region. Further, in Japanese Patent Application Laid-Open No. Hei 4-36586, the partial pressure of nickel chloride vapor obtained by evaporating solid nickel chloride is set to 0.05 to 0.3, and 1004 to 1405. 3 discloses a method for gas phase reduction.
- the present invention it is possible to suppress the metal powder particles generated in the reduction step from agglomerating and growing into secondary particles after the reduction step, and to stably obtain a metal powder having a desired particle diameter. It is intended to provide a method for producing a powder.
- metal atoms are generated at the moment when the metal chloride gas and the reducing gas come into contact, and the metal atoms collide and aggregate to generate ultrafine particles, which grow. Go on.
- the particle size of the generated metal powder is determined by conditions such as the partial pressure and temperature of the metal chloride gas in the atmosphere of the reduction step. After the metal powder having a desired particle size is thus generated, a step of cooling the metal powder transferred from the reduction step is usually provided in order to wash and recover the metal powder.
- the reduction reaction is usually performed in a temperature range of about 100 ox: about or higher
- the reduction reaction temperature range from the reduction reaction temperature range to the temperature range in which the particle growth stops is reduced.
- a metal powder is produced by contacting a metal chloride gas and a reducing gas in a reduction reaction temperature range, By contacting the metal powder with an inert gas, cooling is performed at a cooling rate of 30 t: Z seconds or more from the reduction reaction temperature range to at least 800.
- agglomeration of metal powder particles generated in the steps after the reduction step is suppressed, and the particle diameter of the generated metal powder is maintained in the reduction step. As a result, it becomes possible to stably obtain the required ultrafine metal powder.
- FIG. 1 is a longitudinal sectional view of an apparatus for producing metal powder used in an embodiment of the present invention.
- FIG. 2 is a SEM photograph of the Ni powder produced according to Example 1 according to the present invention.
- FIG. 3 is an SEM photograph of the Ni powder produced according to Comparative Example 1 for the present invention. BEST MODE FOR CARRYING OUT THE INVENTION
- Examples of the metal powder that can be produced by the method for producing a metal powder of the present invention include metal paste suitable for various uses such as a conductive paste filler such as Ni, Cu or Ag, a joining material for Ti material, and a catalyst. It is also possible to produce metal powders such as Al, Ti, Cr, Mn, Fe, Co, Pd, Cd, Pt, and Bi. Among these, the present invention is particularly suitable for producing Ni powder.
- hydrogen gas used for generating the metal powder
- hydrogen gas hydrogen sulfide gas, or the like
- hydrogen gas is preferable in consideration of the influence on the generated metal powder.
- the inert gas used for quenching the generated metal powder is not particularly limited as long as it does not affect the generated metal powder.
- Nitrogen gas, argon gas, or the like can be preferably used. . Of these, nitrogen gas is more preferable because it is inexpensive.
- a metal chloride gas is brought into contact with and reacting with a reducing gas, and a known method can be employed for this method.
- a solid metal chloride such as solid chlorinated nigel is heated and evaporated to form a metal chloride gas, which is then brought into contact with a reducing gas.
- a method can be employed in which a source gas is continuously generated, the metal chloride gas is directly sent to a reduction step, and the metal chloride gas is brought into contact with a reducing gas.
- the former method using solid metal chloride as a raw material requires a heating and evaporating (sublimation) operation, so that it is difficult to stably generate steam.
- solid nickel chloride has water of crystallization, which requires not only dehydration before use, but also inadequate dehydration causes oxygen contamination of the generated Ni powder.
- the amount of metal chloride gas generated according to the amount of chlorine gas supplied is controlled, so the amount of metal chloride gas supplied to the reduction step is controlled by controlling the amount of chlorine gas supplied. be able to. Furthermore, since metal chloride gas is generated by the reaction between chlorine gas and metal, the use of carrier gas can be reduced unlike the method of generating metal chloride gas by heating and evaporating solid metal chloride. Not only that, depending on the manufacturing conditions, it may not be used. Therefore, the production cost can be kept low by reducing the amount of carrier gas used and the resulting suppression of heating energy.
- the partial pressure of the metal chloride gas in the reduction step can be controlled.
- the particle size of the produced metal powder can be controlled. Therefore, the particle size of the metal powder can be stabilized, and the particle size can be arbitrarily set.
- the form of the metal Ni as the starting material does not matter, but from the viewpoint of preventing an increase in contact efficiency and pressure loss, the particle size is about 5 mm to 20 mm. It is preferably in the form of granules, agglomerates, or plates, and its purity is generally preferably 99.5% or more.
- the lower limit temperature of the salification reaction is set to 800 or more in order to promote the reaction sufficiently, and the upper limit temperature is set to 1483 or lower, which is the melting point of Ni. Practically, the range of 900 to 1100 is preferable. New
- the reduction reaction temperature range in which the metal chloride gas is brought into contact with and reacting with the reducing gas is usually 900 to 1200, preferably 95 to 110. 0, and more preferably 980 to 150.
- the metal powder generated by the reduction reaction as described above is forcibly cooled by an inert gas such as nitrogen gas.
- an inert gas such as nitrogen gas.
- the reduction reaction is performed by using a metal. It is desirable to do this immediately after the powder is produced.
- the temperature is reduced to at least 800 ° C., preferably 600 t, more preferably 400 ° C., from the above-mentioned reduction reaction temperature range.
- the metal powder generated in the reduction reaction region is introduced into a cooling system as soon as possible, and an inert gas such as nitrogen gas is supplied therein, and the mixture is cooled by contact with the metal powder.
- the supply amount of the inert gas at this time is not particularly limited as long as it is supplied so as to have the above-mentioned cooling rate.However, usually, 5 N 1 Z minutes or more, preferably 10 550 N 1 Z minutes. In addition, it is effective to set the temperature of the inert gas to be supplied usually at 0 to 100 t :, more preferably at 0 to 80 t.
- the metal powder After cooling the metal powder produced as described above, the metal powder is obtained by separating and recovering the metal powder from a mixed gas of hydrochloric acid gas and inert gas.
- a mixed gas of hydrochloric acid gas and inert gas for separation and recovery, for example, one or a combination of two or more of bag filter, underwater collection / separation means, oil collection / separation means, and magnetic separation means is suitable, but is not limited thereto. Absent.
- the generated metal powder can be washed with a solvent such as water or a monohydric alcohol having 1 to 4 carbon atoms, if necessary.
- N i C 1 2 nitrogen mixed gas the heating means 2 0 by 1 0 0 0 furnace atmosphere temperature of between been reduction furnace 2, a flow rate of 2 from the nozzle 1 7. 3 m Z Introduced in seconds (converted to 1000).
- hydrogen gas was supplied from the reducing gas supply pipe 21 provided at the top of the reducing furnace 2 into the reducing furnace 2 at a flow rate of 7 N 1 / min to reduce the NiC 12 gas.
- luminous flame F which Ru extending downwardly as similar to burning flame of gaseous fuel such as LPG is formed.
- Ni powder P generated by the reduction reaction was supplied from a cooling gas supply pipe 22 provided at a lower portion of the reduction furnace 2 for 24.5 N1Z. Nitrogen gas was brought into contact, whereby the Ni powder P was cooled from 100 to 400. The cooling rate at this time was 105 and was seconds.
- FIG. 2 shows a SEM photograph of the Ni powder obtained in this example, which was uniform spherical particles without aggregation.
- Example 2 An experiment was performed in the same manner as in Example 1 except that the supply amount of nitrogen gas from the cooling gas supply pipe 22 was 4.5 N 1 Z minutes, and cooling was performed from 1000 to 400 ° C. at a rate of 26 seconds at a rate of 26 seconds.
- the average particle size of the resulting Ni powder was 0.29 ⁇ m (measured by the BET method).
- An SEM photograph of the Ni powder obtained in this comparative example is shown in FIG. 3, where secondary particles due to aggregation of the primary particles were observed.
- the metal powder produced by the reduction reaction is brought into contact with an inert gas to reduce the Z from 30 to at least 800 ° C from the reduction reaction temperature range. Cooling at a cooling rate of at least 2 seconds suppresses agglomeration of metal powder particles in the steps after the reduction step, and maintains the particle size of the metal powder generated in the reduction step. Powder can be manufactured stably.
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE69932142T DE69932142T2 (de) | 1998-06-12 | 1999-06-09 | Verfahren zur herstellung von nickelpulver |
EP99923984A EP1018386B1 (en) | 1998-06-12 | 1999-06-09 | Method for producing nickel powder |
US09/463,563 US6372015B1 (en) | 1998-06-12 | 1999-06-12 | Method for production of metal powder |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP16482498A JP4611464B2 (ja) | 1998-06-12 | 1998-06-12 | 金属粉末の製造方法 |
JP10/164824 | 1998-06-12 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1999064191A1 true WO1999064191A1 (fr) | 1999-12-16 |
Family
ID=15800623
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP1999/003087 WO1999064191A1 (fr) | 1998-06-12 | 1999-06-09 | Procede de production de poudre metallique |
Country Status (7)
Country | Link |
---|---|
US (1) | US6372015B1 (ja) |
EP (1) | EP1018386B1 (ja) |
JP (1) | JP4611464B2 (ja) |
KR (1) | KR100411578B1 (ja) |
CN (1) | CN1264633C (ja) |
DE (1) | DE69932142T2 (ja) |
WO (1) | WO1999064191A1 (ja) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6863708B2 (en) * | 2001-06-14 | 2005-03-08 | Toho Titanium Co., Ltd. | Method for producing metal powder and metal powder, and electroconductive paste and monolithic ceramic capacitor |
US7799112B2 (en) | 2003-11-05 | 2010-09-21 | Ishihara Chemical Co., Ltd. | Production method of pure metal/alloy super-micro powder |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3807873B2 (ja) * | 1999-06-08 | 2006-08-09 | 東邦チタニウム株式会社 | Ni超微粉の製造方法 |
JP3492672B1 (ja) * | 2002-05-29 | 2004-02-03 | 東邦チタニウム株式会社 | 金属粉末の製造方法及び製造装置 |
US7416697B2 (en) | 2002-06-14 | 2008-08-26 | General Electric Company | Method for preparing a metallic article having an other additive constituent, without any melting |
US7410610B2 (en) | 2002-06-14 | 2008-08-12 | General Electric Company | Method for producing a titanium metallic composition having titanium boride particles dispersed therein |
US6737017B2 (en) * | 2002-06-14 | 2004-05-18 | General Electric Company | Method for preparing metallic alloy articles without melting |
US7329381B2 (en) | 2002-06-14 | 2008-02-12 | General Electric Company | Method for fabricating a metallic article without any melting |
US7449044B2 (en) | 2002-09-30 | 2008-11-11 | Toho Titanium Co., Ltd. | Method and apparatus for producing metal powder |
KR100503126B1 (ko) * | 2002-11-06 | 2005-07-22 | 한국화학연구원 | 기상법에 의한 구형 니켈 미세분말의 제조 방법 |
US7531021B2 (en) | 2004-11-12 | 2009-05-12 | General Electric Company | Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix |
CN100413618C (zh) * | 2006-05-16 | 2008-08-27 | 中山大学 | 一种超细金属粉的气相合成装置 |
JP5977267B2 (ja) * | 2012-02-08 | 2016-08-24 | Jx金属株式会社 | 表面処理された金属粉、及びその製造方法 |
TWI547326B (zh) * | 2012-02-08 | 2016-09-01 | Jx Nippon Mining & Metals Corp | A surface-treated metal powder, and a method for producing the same |
WO2013158635A1 (en) * | 2012-04-16 | 2013-10-24 | The Board Of Trustees Of The University Of Alabama For And On Behalf Of The University Of Alabama | Non-rare earth magnets having manganese (mn) and bismuth (bi) alloyed with cobalt (co) |
JP6016729B2 (ja) * | 2013-08-02 | 2016-10-26 | 東邦チタニウム株式会社 | 金属粉末の製造方法及び製造装置 |
CN108467948B (zh) * | 2018-04-19 | 2020-05-22 | 上海泰坦科技股份有限公司 | 一种钯及其制备方法和应用 |
KR102484793B1 (ko) * | 2018-06-28 | 2023-01-05 | 도호 티타늄 가부시키가이샤 | 금속 분말과 그 제조 방법, 및 소결 온도의 예측 방법 |
KR102508600B1 (ko) * | 2021-07-02 | 2023-03-16 | 주식회사 이노파우더 | 다단 플라즈마 토치 어셈블리 및 이를 이용한 금속분말 제조방법 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH05247506A (ja) * | 1992-03-05 | 1993-09-24 | Nkk Corp | 金属磁性粉の製造装置 |
JPH06122906A (ja) * | 1992-10-12 | 1994-05-06 | Nkk Corp | 塩化物の供給方法及び金属磁性粉の製造方法 |
WO1998024577A1 (fr) * | 1996-12-02 | 1998-06-11 | Toho Titanium Co., Ltd. | Procede de production de poudre metallique et equipement associe |
Family Cites Families (6)
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JPS597765A (ja) | 1982-07-05 | 1984-01-14 | Nissan Motor Co Ltd | 燃料噴射式内燃機関 |
JPS59170211A (ja) * | 1983-03-14 | 1984-09-26 | Toho Aen Kk | 超微粉の製造方法 |
JPH0623405B2 (ja) * | 1985-09-17 | 1994-03-30 | 川崎製鉄株式会社 | 球状銅微粉の製造方法 |
US5853451A (en) * | 1990-06-12 | 1998-12-29 | Kawasaki Steel Corporation | Ultrafine spherical nickel powder for use as an electrode of laminated ceramic capacitors |
JP2554213B2 (ja) | 1991-06-11 | 1996-11-13 | 川崎製鉄株式会社 | 球状ニッケル超微粉の製造方法 |
DE4214719C2 (de) * | 1992-05-04 | 1995-02-02 | Starck H C Gmbh Co Kg | Verfahren zur Herstellung feinteiliger Metall- und Keramikpulver |
-
1998
- 1998-06-12 JP JP16482498A patent/JP4611464B2/ja not_active Expired - Lifetime
-
1999
- 1999-06-09 CN CNB998013560A patent/CN1264633C/zh not_active Expired - Lifetime
- 1999-06-09 KR KR10-2000-7001455A patent/KR100411578B1/ko not_active IP Right Cessation
- 1999-06-09 DE DE69932142T patent/DE69932142T2/de not_active Expired - Fee Related
- 1999-06-09 WO PCT/JP1999/003087 patent/WO1999064191A1/ja active IP Right Grant
- 1999-06-09 EP EP99923984A patent/EP1018386B1/en not_active Expired - Lifetime
- 1999-06-12 US US09/463,563 patent/US6372015B1/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH05247506A (ja) * | 1992-03-05 | 1993-09-24 | Nkk Corp | 金属磁性粉の製造装置 |
JPH06122906A (ja) * | 1992-10-12 | 1994-05-06 | Nkk Corp | 塩化物の供給方法及び金属磁性粉の製造方法 |
WO1998024577A1 (fr) * | 1996-12-02 | 1998-06-11 | Toho Titanium Co., Ltd. | Procede de production de poudre metallique et equipement associe |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6863708B2 (en) * | 2001-06-14 | 2005-03-08 | Toho Titanium Co., Ltd. | Method for producing metal powder and metal powder, and electroconductive paste and monolithic ceramic capacitor |
US7799112B2 (en) | 2003-11-05 | 2010-09-21 | Ishihara Chemical Co., Ltd. | Production method of pure metal/alloy super-micro powder |
Also Published As
Publication number | Publication date |
---|---|
CN1275103A (zh) | 2000-11-29 |
DE69932142D1 (de) | 2006-08-10 |
DE69932142T2 (de) | 2007-06-06 |
EP1018386B1 (en) | 2006-06-28 |
US6372015B1 (en) | 2002-04-16 |
JPH11350010A (ja) | 1999-12-21 |
JP4611464B2 (ja) | 2011-01-12 |
CN1264633C (zh) | 2006-07-19 |
KR100411578B1 (ko) | 2003-12-18 |
EP1018386A1 (en) | 2000-07-12 |
EP1018386A4 (en) | 2004-11-17 |
KR20010022853A (ko) | 2001-03-26 |
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