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US3196003A - Process of making metal strips and sheets from waste metal - Google Patents

Process of making metal strips and sheets from waste metal Download PDF

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US3196003A
US3196003A US251386A US25138663A US3196003A US 3196003 A US3196003 A US 3196003A US 251386 A US251386 A US 251386A US 25138663 A US25138663 A US 25138663A US 3196003 A US3196003 A US 3196003A
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metal
waste
carbonyl
carbon monoxide
nickel
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US251386A
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William C Jenkin
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Commonwealth Engineering Company of Ohio
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/20—Dry methods smelting of sulfides or formation of mattes from metal carbonyls
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
    • Y10T156/19—Delaminating means
    • Y10T156/1922—Vibrating delaminating means
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/30—Foil or other thin sheet-metal making or treating
    • Y10T29/301—Method

Definitions

  • This invention relates to the making of metal strips and the like of substantially pure metal, and more particularly to the making of such metal strips by gas plating of metal onto a substrate surface from which the metal is then stripped or removed.
  • Pure metal sheets and strips are useful for many purposes, e.g. as wrapping material, clad metal layers, decorative material, etc. Electrolytic processes for producing relatively pure metal deposits are difiicult to practice, and require expensive and complicated equipment. Furthermore, in many instances electroplated metals are quite unsuitable.
  • the invention contemplates the provision of a novel process for producing relatively thin sheet and strip material of substantially pure metal, and without the use of electrolyte solutions of such metal. This is achieved by passing carbon monoxide over a mass of metal freed of oxide and while maintained at a relatively high temperature, that is such as will cause the formation of a metal carbonyl vapor. The resultant metal carbonyl vapors are then passed to a deposition point or substrate, the surface of which has been preheated to permit the deposited metal to be readily stripped or peeled therefrom.
  • the metal which is subjected to the carbon monoxide flow is first cleaned as by mechanically brushing or chemically cleaning to present a clean metal surface free of oxide. While other solid materials may be present it is preferable to provide a metal surface as chemically and mechanically pure as possible, as this makes for a more rapid procedure.
  • a metal mass such as in the form of turnings or shavings, is heated at a temperature of about 500 F. and above, depending upon the metal being reacted, and while thus heated carbon monoxide is brought in contact therewith.
  • the metal mass which is heated and contacted with carbon monoxide may be a solid powder, or metal mesh, it being generally preferable to provide for good contact of the carbon monoxide over :a large area of the metal.
  • Metal turnings or filing-s serve this purpose as well as they may be readily positioned in random fashion to provide intimate gas contact therewith to thereby enhance the gas plating rate.
  • Metal wire, closely bunched, provides a similar good contact for the carbon monoxide.
  • Carbon monoxide is attainable in cylinders commercially, and may be used. A more economical use, however, is effected by reclaiming and using the carbon monoxide as exhausted from the gas plating chamber.
  • FIGURE 1 is a view illustrating an apparatus arrangement useful in the practice of the invention.
  • FIGURE 2 is a view of a pure metal sheet produced in accordance with the invention.
  • FIG- URE 1 designates a gas plating chamber having an inlet 11 and an outlet 12.
  • An endless belt 14 is arranged to be moved through the gas plating chamber.
  • a heater 16 is utilized to heat the endless belt as it is moved through the plating chamber.
  • the endless belt preferably is made of stainless steel and is pretreated in chamber 18 to coat the belt with metal release material such as a metal stearate, for example aluminum stearate or the like.
  • Metal carbnoyl is introduced into the plating chamber 10 and caused to decompose to deposit metal on the precoated endless belt 14. After depositing the thin coating of metal uniformly over the surface of the belt, the metal deposit is stripped away from the belt as at 20, and stored on the roll 21.
  • the metal may be recovered as a thin self-supporting sheet, such as indicated at 22, on the drawings, or be deposited onto a substrate surface.
  • the metal plating gas is preferably prepared in situ during carrying out of the process, and making use of scrap or waste metal as a starting material.
  • the Waste or scrap metal is chemically cleaned of oxides and foreign matter, and then reacted while heated with carbon monoxide to produce the gaseous metal carbonyl, the latter being circulated by conventional means such as a fan, through the gas plating chamber from the metal carbonyl generator as indicated by the arrows in the drawing.
  • metal bearing gas is thermally decomposed to deposit pure metal.
  • the waste gaseous remainder including metal carbonyl, which is undecomposed is recirculated back through the generator and returned with newly generated metal carbonyl.
  • gases such as helium, argon, carbon dioxide, and the like.
  • EXAMPLE 1 Copper metal strip A mass of copper scrap mesh-like waste cuttings is washed with nitric acid (1 part concentrated nitric acid in 3 parts water by volume), and washed with clean Water. The resultant cleaned copper is transferred to a gas plating chamber and subjected to a flow of carbon monoxide while the copper mass is heated to approximately or above. During heating after cleaning the waste copper, the same is kept covered with inert gas such as nitrogen or carbon dioxide prior to passing carbon monoxide thereover. This prevents reoxidation of the chemically clean copper. Copper carbonyl gas which is produced during the reaction is conveyed to the gas plating chamber, as illustrated in the drawings, and brought in contact with the surface of the endless belt moving through the chamber.
  • inert gas such as nitrogen or carbon dioxide
  • the surface of the belt is maintained at about 800 F. to cause the metal bearing gas to decompose and deposit copper metal on the belt surface from which the copper metal deposit is stripped away.
  • Nickel metal strip A mass of nickel powder or fine turnings is treated with cleaning acid as in Example 1, and the resultant clean nickel heated to a temperature of 150 F. Carbon monoxide gas is then circulated in contact with the heated metal. The pressure of the continuing flow of carbon monoxide impels the gas formed by the reaction of the nickel and the carbon monoxide towards the gas plating chamber, such as shown at it) in the drawing.
  • the metal bearing gas formed by contact of the carbon monoxide with the heated nickel metal is passed into contact with the precoated or treated endless belt surface 3 and the nickel carbonyl decomposed at 800 F. to deposit thereover a thin film of nickel. Tests at the exhaust conduit have indicated that decomposition is substantially complete, no nickel being found in the exhaust. The film of nickel deposited on the belt is then stripped therefrom and the cycle repeated.
  • the invention provides a new and commercially practical method of recovering copper, nickel and the like metals from their scrap or secondary metal form.
  • the process broadly consists in converting the scrap or waste metal into a gaseous thermally decomposable compound of the metal and then depositing the metal onto a substrate surface from which it can be readily stripped by heating and decomposing the heat decomposable metal compound to cause the metal to be deposited on the substrate surface.
  • a suitable composition for coating the surface of the endless belt 14-, and such as illustrated in the drawings 25, consists in parts by weight of 100 parts petroleum naphtha (boiling range l50325 C.) and aluminum stearate 20 parts.
  • Other metal fatty acid salts may be used in place of aluminum stearate, for example magnesium palmitate.
  • the gas plating may be carried out under sub-atmospheric pressure conditions, e.g. 1 mm. Hg.
  • the temperature necessary to effect the thermal decomposition of the metal carbonyl will vary depending upon the particular metal compound used.
  • a process of recovering relatively pure metal from waste metal which comprises chemically cleaning said waste metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce metal carbonyl, thereafter bringing the metal carbonyl into contact with a heated endless belt waste copper metal which comprises chemically cleaning said waste copper metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce copper carbonyl, thereafter bringing the copper carbonyl into contact with a. heated substrate surface coated with metal stearate and from which copper metal is strippable and thermally decomposing the copper carbonyl to deposit copper metal onto said substrate, and then stripping the copper metal deposit from the substrate surface.
  • a process of recovering relatively pure nickel from waste nickel metal which comprises chemically cleaning said waste nickel metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce nickel carbonyl, -thereafter bringing. the nickel carbonyl into contact with a heated substrate surface coated with. metal stearate and from which nickel metal is strippable and thermally decomposing the nickel carbonyl to deposit nickel metal onto said substrate, and then stripping the nickel metal deposit from the substrate surface.
  • a process of recovering relatively pure metal from waste metal which comprises chemically cleaning said Waste metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce metal carbonyl, thereafter bringing the metal carbonyl into contact with a heated endless belt substrate surface coated with metal stearate and from which metal is strippable and thermally decomposing the meal'carbonyl to deposit metal onto said substrate, and then stripping the metal deposit from the substrate surface.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

W. C. JENKIN July 20, 1965 PROCESS OF MAKING METAL STRIPS AND SHEETS FROM WASTE METAL Filed Jan. 14, 1963 mvwfi v5.6 www \bqw INVENTOR. v W/LL/AM- C. JEN/(IN United States Patent PROCESS OF MAKING METAL STRIPS AND SHEETS FROM WASTE METAL William C. Jeukin, Dayton, Ohio, assignor to The Cornmonwealth Engineering Company of Ohio, Dayton, Ohio Filed Jan. 14, 1%3, Ser. No. 251,336
4 Claims. (Cl. 75-62) This invention relates to the making of metal strips and the like of substantially pure metal, and more particularly to the making of such metal strips by gas plating of metal onto a substrate surface from which the metal is then stripped or removed.
Pure metal sheets and strips are useful for many purposes, e.g. as wrapping material, clad metal layers, decorative material, etc. Electrolytic processes for producing relatively pure metal deposits are difiicult to practice, and require expensive and complicated equipment. Furthermore, in many instances electroplated metals are quite unsuitable.
The invention contemplates the provision of a novel process for producing relatively thin sheet and strip material of substantially pure metal, and without the use of electrolyte solutions of such metal. This is achieved by passing carbon monoxide over a mass of metal freed of oxide and while maintained at a relatively high temperature, that is such as will cause the formation of a metal carbonyl vapor. The resultant metal carbonyl vapors are then passed to a deposition point or substrate, the surface of which has been preheated to permit the deposited metal to be readily stripped or peeled therefrom.
In practice of the invention the metal which is subjected to the carbon monoxide flow is first cleaned as by mechanically brushing or chemically cleaning to present a clean metal surface free of oxide. While other solid materials may be present it is preferable to provide a metal surface as chemically and mechanically pure as possible, as this makes for a more rapid procedure.
A metal mass, such as in the form of turnings or shavings, is heated at a temperature of about 500 F. and above, depending upon the metal being reacted, and while thus heated carbon monoxide is brought in contact therewith. The metal mass which is heated and contacted with carbon monoxide may be a solid powder, or metal mesh, it being generally preferable to provide for good contact of the carbon monoxide over :a large area of the metal. Metal turnings or filing-s serve this purpose as well as they may be readily positioned in random fashion to provide intimate gas contact therewith to thereby enhance the gas plating rate. Metal wire, closely bunched, provides a similar good contact for the carbon monoxide.
Carbon monoxide is attainable in cylinders commercially, and may be used. A more economical use, however, is effected by reclaiming and using the carbon monoxide as exhausted from the gas plating chamber.
The invention will be more fully understood by reference to the following detailed description and accompanying drawings wherein FIGURE 1 is a view illustrating an apparatus arrangement useful in the practice of the invention; and
FIGURE 2 is a view of a pure metal sheet produced in accordance with the invention.
Referring now to the drawing, the numeral in FIG- URE 1 designates a gas plating chamber having an inlet 11 and an outlet 12. An endless belt 14 is arranged to be moved through the gas plating chamber. A heater 16 is utilized to heat the endless belt as it is moved through the plating chamber. The endless belt preferably is made of stainless steel and is pretreated in chamber 18 to coat the belt with metal release material such as a metal stearate, for example aluminum stearate or the like.
Metal carbnoyl is introduced into the plating chamber 10 and caused to decompose to deposit metal on the precoated endless belt 14. After depositing the thin coating of metal uniformly over the surface of the belt, the metal deposit is stripped away from the belt as at 20, and stored on the roll 21.
The metal may be recovered as a thin self-supporting sheet, such as indicated at 22, on the drawings, or be deposited onto a substrate surface.
For economical reasons, the metal plating gas is preferably prepared in situ during carrying out of the process, and making use of scrap or waste metal as a starting material. The Waste or scrap metal is chemically cleaned of oxides and foreign matter, and then reacted while heated with carbon monoxide to produce the gaseous metal carbonyl, the latter being circulated by conventional means such as a fan, through the gas plating chamber from the metal carbonyl generator as indicated by the arrows in the drawing. During the process metal bearing gas is thermally decomposed to deposit pure metal. The waste gaseous remainder including metal carbonyl, which is undecomposed is recirculated back through the generator and returned with newly generated metal carbonyl. As an inert carrier gas for facilitating circulation of the plating gas, there may be introduced gases such as helium, argon, carbon dioxide, and the like.
While the prior art discloses the use of nickel carbonyl in the production of nickel metal coatings, and technical applications of copper carbonyl has been described, for example, in the Italian publication Chimica (Milan) No. 7, July 1952, pages 284 and 285, it has not been heretofore known to produce these metals in the form of sheets, endless strips and the like starting with the impure metals.
The following examples are illustrative of the inven- -tion and how the pure metal may be recovered.
EXAMPLE 1 Copper metal strip A mass of copper scrap mesh-like waste cuttings is washed with nitric acid (1 part concentrated nitric acid in 3 parts water by volume), and washed with clean Water. The resultant cleaned copper is transferred to a gas plating chamber and subjected to a flow of carbon monoxide while the copper mass is heated to approximately or above. During heating after cleaning the waste copper, the same is kept covered with inert gas such as nitrogen or carbon dioxide prior to passing carbon monoxide thereover. This prevents reoxidation of the chemically clean copper. Copper carbonyl gas which is produced during the reaction is conveyed to the gas plating chamber, as illustrated in the drawings, and brought in contact with the surface of the endless belt moving through the chamber.
The surface of the belt is maintained at about 800 F. to cause the metal bearing gas to decompose and deposit copper metal on the belt surface from which the copper metal deposit is stripped away.
EXAMPLE 2 Nickel metal strip A mass of nickel powder or fine turnings is treated with cleaning acid as in Example 1, and the resultant clean nickel heated to a temperature of 150 F. Carbon monoxide gas is then circulated in contact with the heated metal. The pressure of the continuing flow of carbon monoxide impels the gas formed by the reaction of the nickel and the carbon monoxide towards the gas plating chamber, such as shown at it) in the drawing.
The metal bearing gas formed by contact of the carbon monoxide with the heated nickel metal is passed into contact with the precoated or treated endless belt surface 3 and the nickel carbonyl decomposed at 800 F. to deposit thereover a thin film of nickel. Tests at the exhaust conduit have indicated that decomposition is substantially complete, no nickel being found in the exhaust. The film of nickel deposited on the belt is then stripped therefrom and the cycle repeated.
a The invention provides a new and commercially practical method of recovering copper, nickel and the like metals from their scrap or secondary metal form. The process broadly consists in converting the scrap or waste metal into a gaseous thermally decomposable compound of the metal and then depositing the metal onto a substrate surface from which it can be readily stripped by heating and decomposing the heat decomposable metal compound to cause the metal to be deposited on the substrate surface.
A suitable composition for coating the surface of the endless belt 14-, and such as illustrated in the drawings 25, consists in parts by weight of 100 parts petroleum naphtha (boiling range l50325 C.) and aluminum stearate 20 parts. Other metal fatty acid salts may be used in place of aluminum stearate, for example magnesium palmitate.
Where desired, the gas plating may be carried out under sub-atmospheric pressure conditions, e.g. 1 mm. Hg. The temperature necessary to effect the thermal decomposition of the metal carbonyl will vary depending upon the particular metal compound used.
It will be understood that the foregoing description of the invention may be changed or modified to adapt it to dififerent metals and conditions as to temperature of decomposition, etc., and such obvious modifications withinthe skill of the art is comprehended to fall within the scope of the invention as defined by the claims.
What is claimed is:
1. A process of recovering relatively pure metal from waste metal which comprises chemically cleaning said waste metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce metal carbonyl, thereafter bringing the metal carbonyl into contact with a heated endless belt waste copper metal which comprises chemically cleaning said waste copper metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce copper carbonyl, thereafter bringing the copper carbonyl into contact with a. heated substrate surface coated with metal stearate and from which copper metal is strippable and thermally decomposing the copper carbonyl to deposit copper metal onto said substrate, and then stripping the copper metal deposit from the substrate surface.
3. A process of recovering relatively pure nickel from waste nickel metal which comprises chemically cleaning said waste nickel metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce nickel carbonyl, -thereafter bringing. the nickel carbonyl into contact with a heated substrate surface coated with. metal stearate and from which nickel metal is strippable and thermally decomposing the nickel carbonyl to deposit nickel metal onto said substrate, and then stripping the nickel metal deposit from the substrate surface.
4. A process of recovering relatively pure metal from waste metal which comprises chemically cleaning said Waste metal, subjecting the resultant clean metal to heat while protected from oxidation to the action of carbon monoxide to produce metal carbonyl, thereafter bringing the metal carbonyl into contact with a heated endless belt substrate surface coated with metal stearate and from which metal is strippable and thermally decomposing the meal'carbonyl to deposit metal onto said substrate, and then stripping the metal deposit from the substrate surface.
References Cited by the Examiner UNITED STATES PATENTS 2,159,412 5/39 Wallis 22-57.4- 2,378,053 6/45 Wallis et a1. 22-57.4 2,612,440 9/52 Altmann .56 2,685,121 8/54- Davis 2917 2,701,901 2/55 Pawlyk 22-57.4. 2,981,128 4/61 Flemming -60 3,042,558 7/62 Kllble 207-10 BENJAMIN HENKIN, Primary Examiner.
RICHARD N. EANES, Examiner.

Claims (1)

1. A PROCESS OF RECOVERING RELATIVELY PURE METAL FROM WASTE METAL WHICH COMPRISES CHEMICALLY CLEANING SAID WASTE METAL, SUBJECTING THE RESULTANT CLEAN METATO TO HEAT WHILE PROTECTED FROM OXIDATION TO THE ACTION OF CARBON MONOXIDE TO PRODUCE METAL CARBONYL, THERAFTER BRINGING THE METAL CARBONYL INTO CONTACT WITH A HEATED ENDLESS BELT SUBSTRATE SURFACE FROM WHICH METAL IS STRIPPABLE AND THERMALLY DECOMPOSING THE METAL CARBONYL TO DEPOSIT METAL
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3608615A (en) * 1970-08-20 1971-09-28 Phelps Dodge Corp Foil production
EP0705913A1 (en) * 1994-08-26 1996-04-10 Kabushiki Kaisha Kyokutou Giken Method for manufacturing plastic forming dies

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2159412A (en) * 1936-09-09 1939-05-23 Int Nickel Co Process relating to the production of nickel carbonyl
US2378053A (en) * 1942-01-22 1945-06-12 Int Nickel Co Production of iron carbonyl
US2612440A (en) * 1950-05-03 1952-09-30 Gen Aniline & Film Corp Production of metal carbonyl powders of small size
US2685121A (en) * 1949-05-07 1954-08-03 Ohio Commw Eng Co Method and apparatus for manufacture of metal films
US2701901A (en) * 1952-04-03 1955-02-15 Ohio Commw Eng Co Method of manufacturing thin nickel foils
US2981128A (en) * 1956-04-17 1961-04-25 Socony Mobil Oil Co Inc Process and lubricant composition for rolling aluminum
US3042558A (en) * 1959-05-28 1962-07-03 Aluminum Res Corp Cold forming lubricant and method of applying same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2159412A (en) * 1936-09-09 1939-05-23 Int Nickel Co Process relating to the production of nickel carbonyl
US2378053A (en) * 1942-01-22 1945-06-12 Int Nickel Co Production of iron carbonyl
US2685121A (en) * 1949-05-07 1954-08-03 Ohio Commw Eng Co Method and apparatus for manufacture of metal films
US2612440A (en) * 1950-05-03 1952-09-30 Gen Aniline & Film Corp Production of metal carbonyl powders of small size
US2701901A (en) * 1952-04-03 1955-02-15 Ohio Commw Eng Co Method of manufacturing thin nickel foils
US2981128A (en) * 1956-04-17 1961-04-25 Socony Mobil Oil Co Inc Process and lubricant composition for rolling aluminum
US3042558A (en) * 1959-05-28 1962-07-03 Aluminum Res Corp Cold forming lubricant and method of applying same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3608615A (en) * 1970-08-20 1971-09-28 Phelps Dodge Corp Foil production
EP0705913A1 (en) * 1994-08-26 1996-04-10 Kabushiki Kaisha Kyokutou Giken Method for manufacturing plastic forming dies

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