US20040118244A1 - Method and apparatus for producing metal powder - Google Patents

Method and apparatus for producing metal powder Download PDF

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Publication number
US20040118244A1
US20040118244A1 US10/472,702 US47270204A US2004118244A1 US 20040118244 A1 US20040118244 A1 US 20040118244A1 US 47270204 A US47270204 A US 47270204A US 2004118244 A1 US2004118244 A1 US 2004118244A1
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United States
Prior art keywords
powder
metal
titanium
metal powder
production
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Abandoned
Application number
US10/472,702
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English (en)
Inventor
Yoshihiro Hirata
Yoshio Ueda
Hiaroaki Takase
Kazuaki Suzuki
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Phild Co Ltd
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Phild Co Ltd
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Filing date
Publication date
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Assigned to PHILD CO., LTD. reassignment PHILD CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HIRATA, YOSHIHIRO, SUZUKI, KAZUAKI, TAKASE, HIROAKI, UEDA, YOSHIO
Publication of US20040118244A1 publication Critical patent/US20040118244A1/en
Abandoned legal-status Critical Current

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    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848—Melting process before atomisation
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/086—Cooling after atomisation

Definitions

  • This invention relates to a method and apparatus for producing, in an economical manner, metal powder offering high purity and uniform granular shape and size.
  • the invention also relates to a production of titanium powder, among others, as the aforementioned metal powder.
  • Raw element metals are processed into various forms, such as molded shapes, sheet, bar, thin wire or foil, according to applications.
  • metal powder as molding material is drawing the attention in the fields of powder metallurgy, thermal spraying and other molding techniques.
  • powder metallurgy is regarded as an important technology offering wide applications, including production of metal parts, and therefore demand for powder metal—which is the base material for powder metallurgy—is also growing.
  • Electrolysis is one of relatively new methods for metal powder production. It has been reported that smooth, minute and uniform crystalline structures can be deposited under appropriate conditions, and that performing electrolysis outside the range of these conditions produces brittle metal of sponge or powder form.
  • titanium is a relatively new metal compared with iron, copper and aluminum that have been in use since ancient times. Titanium is light and offers excellent strength at high temperature as well as corrosive resistance, and is therefore used widely in industrial applications.
  • the sample applications of titanium include jet engine material and structural member for aircraft/spaceship, material for heat-exchangers used in thermal and nuclear power generation, catalyst material used in polymeric chemical products, articles of daily use such as eyeglass frame and golf club head, and material for health equipment, medical equipment and medical/dental material.
  • the applications of titanium are expected to grow further. Titanium, which is already competing with stainless steel, duralumin and other high-performance metals in terms of applications, is likely to surpass its rivals in the future.
  • Titanium powder produced by the conventional powder production methods designed for general metals is subject to the same problems with other metals; i.e., irregular granular shape and size, poor economy, and so on.
  • development of a production method that can provide titanium powder offering high purity and uniform granular shape and size is eagerly awaited.
  • the hydrogenative dewatering method and rotary electrode method are being put to practical use as improved production methods for titanium metal powder.
  • the hydrogenative dewatering method uses sponge titanium, molten titanium or titanium chips generated from cutting/machining as material.
  • the material titanium is heated in a hydrogen atmosphere to cause it to absorb the hydrogen gas and thus become brittle. This brittle titanium is then crushed and heated again in vacuum so that the hydrogen gas will be released and powder formed.
  • molten titanium or titanium melted then forged, rolled or otherwise worked is formed into a round bar to be used as material.
  • This material round bar is turned at high speed in an atmosphere of argon, helium or other inactive gas, while its tip is melted by a heat source such as an arc or plasma-arc torch. The drips of molten metal are then scattered via centrifugal force to produce spherical powder grains.
  • the grains of titanium powder obtained by the hydrogenative dewatering method have irregular sphericity. Although this powder can be used in die molding, the heating process must be repeated twice. A crushing process using a ball mill or other mechanical means may be incorporated, but oxygen contamination of titanium powder cannot be avoided. In the rotary electrode method, material titanium is melted in an inactive gas and made into powder form. Therefore, grains are spherical and offer good flowability. They are not subject to oxygen contamination, either. However, the solidification property when molded will be reduced. Both methods are a batch system, so the power production cost is high.
  • the atomization method was developed as a titanium powder production method addressing the aforementioned problems relating to quality and production cost.
  • material titanium is melted in a water-cooled copper crucible using a plasma-arc torch or other heat source, in order to cause molten titanium to drip continuously from one end of the crucible.
  • Argon, helium or other inactive gas is then injected onto the molten titanium to atomize it and obtain powder.
  • this method could not reduce the production cost significantly from the levels of the conventional methods, because molten titanium or melted and worked titanium had to be used as material.
  • the purpose of the present invention is to provide element-metal powder material offering excellent uniformity of granular sphericity and consistency of granule size, for use in powder metallurgy and other types of molding.
  • the inventors conducted various studies to resolve the problems associated with the production of element metal powder such as titanium powder, including those pertaining to the purity of element metal, uniformity of granular sphericity, consistency of granule size and production cost.
  • the aforementioned invention relating to a production of high-function water containing titanium provides a method for producing high-function water in which molten titanium is dissolved, wherein the method is characterized by the burning of a mixture gas of oxygen and hydrogen in high-pressure water and the melting of titanium metal using the combustion gas.
  • the present invention differs completely from the conventional production methods for metal powder such as titanium powder, in both concept and structure, in that a mixture gas of oxygen and hydrogen is burned in high-pressure water and the combustion gas is used to melt element titanium metal, thereby allowing metal powder to precipitate in water. It is an improved method for producing metal powder that adopts an approach completely different from those taken by the conventional methods.
  • the present invention allows for a production of element metal powder in a very efficient manner without using thermal melting, arc discharge or laser irradiation to heat material metal and also without a need to let molten metal drip or inject gas onto it to atomize the metal and produce powder.
  • the method proposed by the present invention generates virtually no byproducts or impurities other than the target metal powder. Occurrence of metal oxidation due to heating of material metal is also very small, and since the obtained metal powder has excellent uniformity of granular sphericity and consistency of granule size, the production cost can be reduced significantly.
  • the method also allows for continuous production in addition to batch production, which opens a door to mass-production of metal powder having uniform granule size.
  • the basic structure of the present invention is to burn a mixture gas of oxygen and hydrogen in high-pressure water and use the combustion gas to heat material element metal and then convert it into powder form, thereby producing metal powder of uniform granule size.
  • a schematic drawing of the production process is shown in the production flow chart given in FIG. 1.
  • the present invention consists of components (1) through (5) below, which basically serve to burn a mixture gas of oxygen and hydrogen in high-pressure water and use the combustion gas to melt material metal and then convert it into powder form:
  • a method for producing metal powder by burning a mixture gas of oxygen and hydrogen in high-pressure water, using the combustion gas to heat material element metal, and converting it into powder form.
  • An apparatus for producing metal powder consisting of a pressure-resistant container that comprises a high-pressure water tank, an injector nozzle for mixture gas of oxygen and hydrogen, a material element-metal feeder part, an ignition plug and a combustion chamber.
  • FIG. 1 Flow chart of metal powder production as proposed by the present invention
  • FIG. 2 An apparatus for producing metal powder as proposed by the present invention
  • purified water such as distilled water is filled into the high-pressure water tank inside the pressure-resistant container for titanium-metal powder production, and material titanium metal such as a titanium metal bar is fed from the material element-metal feeder part and pressurized at high pressure.
  • a mixture gas consisting of hydrogen and oxygen is injected from the nozzle, ignited and let completely burn in the combustion chamber.
  • material titanium is instantly melted in the combustion gas and dispersed in water.
  • very fine titanium grains of micron order are produced and dispersed in powder form.
  • the produced fine titanium powder does not melt or float and precipitates in a short period.
  • the present invention can produce titanium powder of high purity at a very high efficiency. To achieve this, it is important to control the amounts of gases to be mixed and burned, reaction pressure and feed rate of material titanium metal.
  • an ideal injection amount of mixture gas is approx. 2 to 4 liters per second when the container can hold one ton of purified water. Applying too high a gas pressure may damage the apparatus structure, while a low pressure may cause the gas to flow upward from the nozzle, causing the heated, molten fine metal grains to be encapsulated in air bubbles and diffused from the water surface. This will reduce the generation efficiency of fine metal grains.
  • the water pressure in the pressure tank should be 1.2 to 1.5 atmospheres.
  • the supplied material titanium metal should preferably have the highest possible purity, in order to prevent impurities from mixing into the produced titanium powder.
  • a mixture gas of hydrogen and oxygen provides the most efficient and stable means of burning titanium metal in water, where high pressure is required to ensure stable combustion. Physical or chemical explanations as to why element titanium metal melts instantly and becomes super-fine grains in a combustion gas in high-pressure water have not been found yet.
  • Material titanium metal may take a shape of bar, sheet, granule or foil, and it may be appropriate to feed titanium metal granules instead of bar if the capacity of the production container is much smaller than one ton.
  • the material element metals that can be used in the production of metal powder using the production apparatus proposed by the present invention include, but not limited to, zirconium, germanium, tin, gold, platinum and silver.
  • the high-pressure water tank used in the apparatus proposed by the present invention is a pressure-resistant tank made of metal, or preferably steel, and ideally other parts such as the combustion chamber should also be made of steel.
  • the gas pump is installed to blow out a mixture gas at high pressure. Material element metal is fed continuously in accordance with the melt amount.
  • Material element metal must be fed into a position where the mixture gas burns completely and fully turns into a steam gas of ultrahigh temperature.
  • the combustion chamber is installed to burn the mixture gas to achieve this purpose. This setup allows for production of pure metal powder free from impurities or byproducts. High pressure is also required to completely burn a pure mixture gas.
  • FIG. 1 shows a flow chart of metal powder production as proposed by the present invention, as described earlier.
  • An apparatus for producing metal powder (A) shown in FIG. 2 consists of a pressure-resistant container (B) that comprises a high-pressure water tank ( 2 ), an injector nozzle for mixture gas of oxygen and hydrogen ( 5 ), a material element-metal feeder part ( 22 ), an ignition plug ( 12 ) and a combustion chamber ( 7 ).
  • the apparatus for producing metal powder (A) consists of a pressure-resistant container for metal powder production (B), and the pressure-resistant container for metal powder production comprises a gas injection pump ( 1 ), a high-pressure water tank ( 2 ), a combustion chamber ( 7 ), a pressure control valve ( 8 ), a metal powder outlet ( 13 ), purified water ( 3 ), material element metal for powder production ( 21 ), an ignition plug ( 12 ), a material element-metal feeder part ( 22 ) and a mixture-gas injector nozzle ( 5 ). ( 4 ) indicates produced metal powder.
  • Purified water ( 3 ) such as distilled water is filled into the high-pressure water tank ( 2 ) of the pressure-resistant container for metal powder production (B), and material titanium metal ( 21 ) such as a titanium metal bar is fed from the material element-metal feeder part ( 22 ), after which the container is pressurized at a high pressure.
  • Hydrogen and oxygen are injected from the nozzle ( 5 ) as a mixture gas and the mixture gas is ignited by the ignition device ( 12 ).
  • the mixture gas is completely burned in the combustion chamber ( 7 ) to obtain a perfect combustion state leaving an ultrahigh-temperature steam gas, and the material titanium melts instantly in this combustion gas and disperses in water.
  • titanium metal powder does not melt or float and precipitates as powder in a short period.
  • the separated powder is then released from the outlet for titanium metal powder ( 13 ) and becomes titanium powder.
  • mixture gas of hydrogen and oxygen must be precisely controlled to achieve a hydrogen-to-oxygen ratio of 2 to 1. While a mixture gas of hydrogen and oxygen is supplied from commercial gas cylinders, adding a water electrolyzer (C) as an adjunct to produce a mixture gas of hydrogen and oxygen via electrolysis of water will generate completely pure gases to facilitate an optimal, efficient supply of mixture gas.
  • a water electrolyzer C
  • adding a water electrolyzer (C) as an adjunct instead of supplying a mixture gas of hydrogen and oxygen from commercial gas cylinders, will generate completely pure gases via electrolysis of water, thereby facilitating a supply of mixture gas in a simple and efficient manner.
  • the electrolyzer (C) is considered an optional adjunct unit to produce and supply a mixture gas of hydrogen and oxygen via electrolysis of water, which consists of feed pipes for hydrogen and oxygen gases ( 9 , 10 ), electrodes ( 19 , 20 ), a partition ( 18 ) and water ( 16 ).
  • the electrolyzer causes electrolysis of acid or alkali raw water to generate oxygen gas at the anode and hydrogen gas at the cathode, and supplies them as a material mixture gas.
  • the element titanium powder contained no byproducts or impurities and exhibited excellent uniformity of granular sphericity and consistency of granule size.
  • the production cost was reduced around a half compared with the conventional technologies.
  • the present invention allows for production of high-purity metal, especially titanium powder, in a very efficient manner.
  • the production method proposed by the present invention achieves pure powder free from byproducts or impurities other than the elemental component, wherein the produced powder offers excellent uniformity of granular sphericity and size and can be produced at significantly less cost. Batch production, continuous production and mass production are also possible.

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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
US10/472,702 2001-03-28 2002-03-26 Method and apparatus for producing metal powder Abandoned US20040118244A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2001-91941 2001-03-28
JP2001091941 2001-03-28
PCT/JP2002/002911 WO2002078883A1 (fr) 2001-03-28 2002-03-26 Procede et appareil de production de poudre metallique

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US20040118244A1 true US20040118244A1 (en) 2004-06-24

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US10/472,702 Abandoned US20040118244A1 (en) 2001-03-28 2002-03-26 Method and apparatus for producing metal powder

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US (1) US20040118244A1 (xx)
EP (1) EP1393841A4 (xx)
JP (1) JP4137643B2 (xx)
KR (1) KR20030080062A (xx)
CN (1) CN1248812C (xx)
BR (1) BR0208466A (xx)
CA (1) CA2442153A1 (xx)
HU (1) HUP0303939A3 (xx)
MX (1) MXPA03008818A (xx)
NO (1) NO20034327L (xx)
NZ (1) NZ528630A (xx)
PL (1) PL365332A1 (xx)
TW (1) TW570851B (xx)
WO (1) WO2002078883A1 (xx)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040091552A1 (en) * 2001-02-27 2004-05-13 Yoshihiro Hirata Method and device for manufacturing advanced water containing ultra-fine gold particles
US20040107798A1 (en) * 2001-03-28 2004-06-10 Yoshihiro Hirata Method and device for manufacturing metallic particulates, and manufactured metallic particulates
US20040237716A1 (en) * 2001-10-12 2004-12-02 Yoshihiro Hirata Titanium-group metal containing high-performance water, and its producing method and apparatus
US20050072272A1 (en) * 2000-05-10 2005-04-07 Yoshihiro Hirata High functional water containing titanium and method and apparatus for producing the same
US7201945B2 (en) 2000-07-04 2007-04-10 Phild Co., Ltd. Healthy fiber products
US20100183691A1 (en) * 2009-01-22 2010-07-22 Xiaosong Zhu Use of Titanium metal fine-particles for increasing the effect of Germicidal medicines used for human skin dermatosis, skin infection and traumatism

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030084964A (ko) * 2001-03-29 2003-11-01 파일드 가부시키가이샤 초미립자 티타늄 분산수로 이루어진 모발 수복액 및 그제조방법과 장치
TWI255695B (en) 2001-10-12 2006-06-01 Phild Co Ltd Method and device for producing ultrafine dispersion of noble metal
JP2006000147A (ja) * 2004-06-15 2006-01-05 Fuairudo Kk シリコーンエラストマーを用いた健康装身具とその製造方法
JP2006110179A (ja) * 2004-10-15 2006-04-27 Fuairudo Kk 腰部加圧用ベルト
KR100830931B1 (ko) 2007-05-23 2008-05-22 (주) 나노기술 진공 배기 및 가스 흡입 방식을 이용한 진공형 고전압 갭스위치 및 이를 이용한 금속 나노 분말 제조 방법

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US2269528A (en) * 1940-03-30 1942-01-13 Rca Corp Method of manufacturing metal spheres
US4933023A (en) * 1982-10-29 1990-06-12 Wahlbeck H G E Method for manufacture of non-allergy creating precious metal objects
US20040091552A1 (en) * 2001-02-27 2004-05-13 Yoshihiro Hirata Method and device for manufacturing advanced water containing ultra-fine gold particles
US20040107798A1 (en) * 2001-03-28 2004-06-10 Yoshihiro Hirata Method and device for manufacturing metallic particulates, and manufactured metallic particulates
US6869626B1 (en) * 1999-11-18 2005-03-22 Phild Co., Ltd. Production method of ultrafine gold particle-dissolved water and device therefor
US20050072272A1 (en) * 2000-05-10 2005-04-07 Yoshihiro Hirata High functional water containing titanium and method and apparatus for producing the same
US6989127B2 (en) * 2001-03-28 2006-01-24 Phild Co., Ltd. Health ornament containing titanium powder and method for manufacturing thereof

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JPS62263903A (ja) * 1986-05-12 1987-11-16 Kyuzo Kamata 金属の超微粒子製造法
JP2001122606A (ja) * 1999-10-22 2001-05-08 Fuairudo Kk フラーレン水の製造方法及びその装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2269528A (en) * 1940-03-30 1942-01-13 Rca Corp Method of manufacturing metal spheres
US4933023A (en) * 1982-10-29 1990-06-12 Wahlbeck H G E Method for manufacture of non-allergy creating precious metal objects
US6869626B1 (en) * 1999-11-18 2005-03-22 Phild Co., Ltd. Production method of ultrafine gold particle-dissolved water and device therefor
US20050072272A1 (en) * 2000-05-10 2005-04-07 Yoshihiro Hirata High functional water containing titanium and method and apparatus for producing the same
US20040091552A1 (en) * 2001-02-27 2004-05-13 Yoshihiro Hirata Method and device for manufacturing advanced water containing ultra-fine gold particles
US20040107798A1 (en) * 2001-03-28 2004-06-10 Yoshihiro Hirata Method and device for manufacturing metallic particulates, and manufactured metallic particulates
US6989127B2 (en) * 2001-03-28 2006-01-24 Phild Co., Ltd. Health ornament containing titanium powder and method for manufacturing thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050072272A1 (en) * 2000-05-10 2005-04-07 Yoshihiro Hirata High functional water containing titanium and method and apparatus for producing the same
US7144589B2 (en) 2000-05-10 2006-12-05 Phild Co., Ltd. High functional water containing titanium and method and apparatus for producing the same
US7201945B2 (en) 2000-07-04 2007-04-10 Phild Co., Ltd. Healthy fiber products
US20040091552A1 (en) * 2001-02-27 2004-05-13 Yoshihiro Hirata Method and device for manufacturing advanced water containing ultra-fine gold particles
US7314499B2 (en) 2001-02-27 2008-01-01 Phild Co., Ltd. Method and device for manufacturing advanced water containing ultra-fine gold particles
US20040107798A1 (en) * 2001-03-28 2004-06-10 Yoshihiro Hirata Method and device for manufacturing metallic particulates, and manufactured metallic particulates
US7108735B2 (en) 2001-03-28 2006-09-19 Phild Co., Ltd. Method and device for manufacturing metallic particulates, and manufactured metallic particulates
US20040237716A1 (en) * 2001-10-12 2004-12-02 Yoshihiro Hirata Titanium-group metal containing high-performance water, and its producing method and apparatus
US7300672B2 (en) * 2001-10-12 2007-11-27 Phild Co., Ltd. Titanium-group metal containing high-performance water, and its producing method and apparatus
US20100183691A1 (en) * 2009-01-22 2010-07-22 Xiaosong Zhu Use of Titanium metal fine-particles for increasing the effect of Germicidal medicines used for human skin dermatosis, skin infection and traumatism

Also Published As

Publication number Publication date
EP1393841A4 (en) 2005-02-23
JP4137643B2 (ja) 2008-08-20
JPWO2002078883A1 (ja) 2004-10-21
WO2002078883A1 (fr) 2002-10-10
BR0208466A (pt) 2004-03-23
TW570851B (en) 2004-01-11
KR20030080062A (ko) 2003-10-10
HUP0303939A3 (en) 2004-08-30
EP1393841A1 (en) 2004-03-03
HUP0303939A2 (hu) 2004-03-29
NZ528630A (en) 2004-08-27
CA2442153A1 (en) 2002-10-10
NO20034327L (no) 2003-11-25
CN1248812C (zh) 2006-04-05
NO20034327D0 (no) 2003-09-26
CN1529644A (zh) 2004-09-15
PL365332A1 (en) 2004-12-27
MXPA03008818A (es) 2004-02-18

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Owner name: PHILD CO., LTD., JAPAN

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:HIRATA, YOSHIHIRO;UEDA, YOSHIO;TAKASE, HIROAKI;AND OTHERS;REEL/FRAME:014991/0265

Effective date: 20031107

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION