US3066042A - Method of coating metal - Google Patents

Method of coating metal Download PDF

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Publication number
US3066042A
US3066042A US855508A US85550859A US3066042A US 3066042 A US3066042 A US 3066042A US 855508 A US855508 A US 855508A US 85550859 A US85550859 A US 85550859A US 3066042 A US3066042 A US 3066042A
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Prior art keywords
coating
molybdenum
platinum
metal
heat treating
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US855508A
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Ogden Joseph
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Engelhard Industries Inc
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Engelhard Industries Inc
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Priority to US855508A priority Critical patent/US3066042A/en
Priority to GB40598/60A priority patent/GB922105A/en
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Classifications

    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/001—Interlayers, transition pieces for metallurgical bonding of workpieces
    • B23K35/005—Interlayers, transition pieces for metallurgical bonding of workpieces at least one of the workpieces being of a refractory metal
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/06—Metallic material
    • C23C4/08—Metallic material containing only metal elements
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18—After-treatment
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
    • C21D7/04—Modifying the physical properties of iron or steel by deformation by cold working of the surface
    • C21D7/06—Modifying the physical properties of iron or steel by deformation by cold working of the surface by shot-peening or the like

Definitions

  • the present invention deals with a method of coating metal and more particularly with a method of coating refractory metal with a platinum-group metal.
  • molybdenum at high temperatures has high strength properties which makes it desirable for high temperature, high stress applications, e.g. for jet engine turbine blades, glass melting apparatus, and other structures for use under high temperatures.
  • molybdenum as such, cannot be advant-ageously utilized because of its high rate of oxidation at high temperatures.
  • platinum is generally used as a cladding metal and is applied to the molybdenum by bonding a strip or sheet of platinum to the molybdenum or by bonding a tube of platinum onto a core of molybdenum wire or rod to form a composite material. Otherwise, the molybdenum is provided with a fitted platinum sheath and the structure formed therefrom is welded only at the structural joints.
  • the composite material is unsatisfactory for many applications because of the exposure of the molybdenum at the edges of the strip, sheet or rod.
  • the sheathed molybdenum is unsatisfactory because there is no strong bond between the molybdenum and platinum, and the platinum is subject to fracture under stresses with the subsequent failure of the molybdenum.
  • the present invention relates to the spraying of platinum or other platinum group metals such as palladium and rhodium or alloys thereof onto a molybdenum body, or a body of other refractory metal, e.g. tantalum, tungsten, titanium, in a manner whereby the platinum group metal completely covers the body with a strong mechanical and metallurgical bond therebetween and otherwise provides a suitable protective cladding for use at elevated temperatures.
  • platinum or other platinum group metals such as palladium and rhodium or alloys thereof onto a molybdenum body, or a body of other refractory metal, e.g. tantalum, tungsten, titanium
  • a sheet, strip, rod, bar or other structure composed of molybdenum is first cleaned by well known chemical cleaning or etching methods after which molten platinum is sprayed onto the molybdenum by the known metallizing gun spray method to form a thin layer coating on the molybdenum.
  • the coating is preferably plastically deformed, e.g. the coating is shot peened, by known shot peening procedure, whereby the entire layer is substantially plastically deformed sutficiently to condition the layer for improved solid diffusion of the layer by a subsequent heat treating; and to otherwise place the layer and the molybdenum in more intimate contact with each other.
  • the coated molybdenum is heat treated, i.e.
  • the coated molybdenum is not sufiiciently protected for high temperature application. Therefore, the spraying, peening and heat treating are repeated whereby a sufficiently thick protective coating is provided by the spraying in layers with intermediate peening and heat treatment. The process is repeated until the coating has the desired thickness, i.e. from tenths of a thousandth of an inch to any thickness required.
  • Desired thickness is determined by the life expectancy of the end product. It has been discovered that while substantially thick spray coatings may be provided by continuous spraying, such continuous coatings are inferior to the coatings provided by the aforesaid method of the invention'and otherwise, the intermediate shot peening not only improves the solid diffusion of the layers under the heat treatment, but also provides for a stronger mechanical and metallurgical bond between the platinum layer and the molybdenum.
  • Example A surface of a 2" x 2" molybdenum plate .025" in thickness was cleaned and etched and was sprayed with molten platinum and provided with a platinum layer 0.003" in thickness.
  • the coated surface was shot peened and then annealed in dry hydrogen for one hour at a temperature of 1000" C.
  • the coated plate was cooled in air and the same operation repeated four times until a layer aprpoximately 0.012" in thickness was built up on the molybdenum plate.
  • the layer was found to be substantially non-porous.
  • the coating may be plastically deformed by other methods such as pressing or rolling.
  • the method of coating a refractory metal body composed of a metal selected from the group consisting of molybdenum, tantalum, tungsten and titanium comprising cleaning a surface of the body, spraying a molten platinum group metal on the cleaned surface in the form 3 of a thin coat, shot peening the coating, heat treating the shot peened coating at a temperature from 600 C. to 1400 C. to promote solid diffusion of the coating, and alternately continuing the spraying, shot peening and heat treating until a sufiiciently thick coating'of platinum 5 group metal is built up on the metal body.

Abstract

A method of coating a refractory metal body consisting essentially of Mo, Ta, W or Ti, comprises the steps of (1) cleaning the body, (2) spraying molten platinum group metals (e.g. Pt, Pd, Rh, or their alloys) on to the surface, (3) plastically deforming the coating (by shotpeening, pressing or rolling), and (4) heat treating the coated body at 600-1400 DEG C. for a time sufficient to promote solid diffusion of the coating (e.g. 1-10 hours). These steps (1)-(4) are repeated until a sufficient thickness of coating metal has been built up. The heat treating step may be carried out in dry hydrogen.

Description

United States Patent 3,066,042 Patented Nov. 27, 1962 3,066,042 METHOD OF COATING METAL Joseph Ogden, Maywood, N.J., assiguor, by inesne assignments, to Engelhard Industries, Inc., Newark, N.J., a corporation of Delaware N Drawing. Filed Nov. 27, 1959, Ser. No. 855,508 1 Claim. (Cl. 117-65.2)
The present invention deals with a method of coating metal and more particularly with a method of coating refractory metal with a platinum-group metal.
It is well known that molybdenum at high temperatures has high strength properties which makes it desirable for high temperature, high stress applications, e.g. for jet engine turbine blades, glass melting apparatus, and other structures for use under high temperatures.
However, molybdenum, as such, cannot be advant-ageously utilized because of its high rate of oxidation at high temperatures.
In order to protect molybdenum from oxidation at high temperatures, platinum is generally used as a cladding metal and is applied to the molybdenum by bonding a strip or sheet of platinum to the molybdenum or by bonding a tube of platinum onto a core of molybdenum wire or rod to form a composite material. Otherwise, the molybdenum is provided with a fitted platinum sheath and the structure formed therefrom is welded only at the structural joints. The composite material is unsatisfactory for many applications because of the exposure of the molybdenum at the edges of the strip, sheet or rod. The sheathed molybdenum is unsatisfactory because there is no strong bond between the molybdenum and platinum, and the platinum is subject to fracture under stresses with the subsequent failure of the molybdenum.
While the spraying of a thin layer of platinum metal onto molybdenum has been considered, the sprayed layer coating is porous and does not adequately protect the molybdenum.
The present invention relates to the spraying of platinum or other platinum group metals such as palladium and rhodium or alloys thereof onto a molybdenum body, or a body of other refractory metal, e.g. tantalum, tungsten, titanium, in a manner whereby the platinum group metal completely covers the body with a strong mechanical and metallurgical bond therebetween and otherwise provides a suitable protective cladding for use at elevated temperatures.
A simplified flow diagram of the method of the invention is as follows:
Cleaning refractory metal plate Spraying molten platinum on cleaned plate to form a first coating Shot peening the platinum coating Heat treating shot peened coating Spraying a second platinum coating on first coating Shot peening second platinum coating Heat treating shot peened second coating It is an object of the invention to provide a method of cladding a refractory body with a platinum group metal.
It is another object of the invention to provide a method of applying a plurality of sprayed layers of a platinum group metal onto .a refractory body whereby the body is adequately protected against oxidation at high temperatures.
Other objects and advantages of the invention will become apparent from the description hereinafter following.
In accordance with the invention, a sheet, strip, rod, bar or other structure composed of molybdenum is first cleaned by well known chemical cleaning or etching methods after which molten platinum is sprayed onto the molybdenum by the known metallizing gun spray method to form a thin layer coating on the molybdenum. Thereafter, the coating is preferably plastically deformed, e.g. the coating is shot peened, by known shot peening procedure, whereby the entire layer is substantially plastically deformed sutficiently to condition the layer for improved solid diffusion of the layer by a subsequent heat treating; and to otherwise place the layer and the molybdenum in more intimate contact with each other. Thereafter, the coated molybdenum is heat treated, i.e. annealed, in a reducing atmosphere, e.g. in dry hydrogen, at a temperature of from 600 C. to 1400 C. for about one to ten hours depending upon the temperature employed, whereby the consequent solid ditfusion of the layer eliminates the pores inherent in the sprayed platinum layer. After the aforesaid treatment of the first sprayed platinum layer, the coated molybdenum is not sufiiciently protected for high temperature application. Therefore, the spraying, peening and heat treating are repeated whereby a sufficiently thick protective coating is provided by the spraying in layers with intermediate peening and heat treatment. The process is repeated until the coating has the desired thickness, i.e. from tenths of a thousandth of an inch to any thickness required. Desired thickness is determined by the life expectancy of the end product. It has been discovered that while substantially thick spray coatings may be provided by continuous spraying, such continuous coatings are inferior to the coatings provided by the aforesaid method of the invention'and otherwise, the intermediate shot peening not only improves the solid diffusion of the layers under the heat treatment, but also provides for a stronger mechanical and metallurgical bond between the platinum layer and the molybdenum.
Example A surface of a 2" x 2" molybdenum plate .025" in thickness was cleaned and etched and was sprayed with molten platinum and provided with a platinum layer 0.003" in thickness. The coated surface was shot peened and then annealed in dry hydrogen for one hour at a temperature of 1000" C. The coated plate was cooled in air and the same operation repeated four times until a layer aprpoximately 0.012" in thickness was built up on the molybdenum plate. The layer was found to be substantially non-porous.
While shot peening is specifically referred to, the coating may be plastically deformed by other methods such as pressing or rolling.
While specific embodiments of the invention are described, modifications are contemplated within the scope of the appended claims:
What is claimed is:
The method of coating a refractory metal body composed of a metal selected from the group consisting of molybdenum, tantalum, tungsten and titanium, comprising cleaning a surface of the body, spraying a molten platinum group metal on the cleaned surface in the form 3 of a thin coat, shot peening the coating, heat treating the shot peened coating at a temperature from 600 C. to 1400 C. to promote solid diffusion of the coating, and alternately continuing the spraying, shot peening and heat treating until a sufiiciently thick coating'of platinum 5 group metal is built up on the metal body.
References Cited in the file of this patent UNITED STATES PATENTS Robinson Apr. 6, 1937 Colbert et a1 Dec. 16, 1947 Rosenblatt et a1 Oct. 4, 1955 Mozley et al June 25, 1957 Wrotnowski Mar. 29, 1960
US855508A 1959-11-27 1959-11-27 Method of coating metal Expired - Lifetime US3066042A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3197861A (en) * 1960-06-01 1965-08-03 Continental Can Co Production of non-porous vacuum metallized coatings on strip material
US3494748A (en) * 1966-12-16 1970-02-10 Xerox Corp Oxidation resistant coating and article
US4051275A (en) * 1974-06-21 1977-09-27 Forestek Clarence W Embedding and compacting particles in porous surfaces
FR2392731A1 (en) * 1977-05-31 1978-12-29 Secr Defence Brit METHOD AND APPARATUS FOR FORMING A METAL ARTICLE
US4159353A (en) * 1978-01-19 1979-06-26 Corning Glass Works Platinum coating dense refractories
WO2003072845A1 (en) * 2002-02-28 2003-09-04 Koncentra Holding Ab Thermal spraying of a piston ring
WO2003072844A1 (en) * 2002-02-28 2003-09-04 Man B & W Diesel A/S Thermal spraying of a machine part
CN114107857A (en) * 2021-11-30 2022-03-01 西北有色金属研究院 High-temperature high-pressure shot peening strengthening method for improving ablation resistance of surface of refractory metal electrode

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3589373A (en) * 1968-10-28 1971-06-29 Amf Inc Cigarette making machine

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2075910A (en) * 1926-07-07 1937-04-06 Ass Elect Ind Thermionic cathode
US2432657A (en) * 1944-05-27 1947-12-16 Libbey Owens Ford Glass Co Process of evaporating metals
US2719797A (en) * 1950-05-23 1955-10-04 Baker & Co Inc Platinizing tantalum
US2797174A (en) * 1952-05-23 1957-06-25 Lockheed Aircraft Corp Method for providing protective metal coatings on metal
US2930106A (en) * 1957-03-14 1960-03-29 American Felt Co Gaskets

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2075910A (en) * 1926-07-07 1937-04-06 Ass Elect Ind Thermionic cathode
US2432657A (en) * 1944-05-27 1947-12-16 Libbey Owens Ford Glass Co Process of evaporating metals
US2719797A (en) * 1950-05-23 1955-10-04 Baker & Co Inc Platinizing tantalum
US2797174A (en) * 1952-05-23 1957-06-25 Lockheed Aircraft Corp Method for providing protective metal coatings on metal
US2930106A (en) * 1957-03-14 1960-03-29 American Felt Co Gaskets

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3197861A (en) * 1960-06-01 1965-08-03 Continental Can Co Production of non-porous vacuum metallized coatings on strip material
US3494748A (en) * 1966-12-16 1970-02-10 Xerox Corp Oxidation resistant coating and article
US4051275A (en) * 1974-06-21 1977-09-27 Forestek Clarence W Embedding and compacting particles in porous surfaces
FR2392731A1 (en) * 1977-05-31 1978-12-29 Secr Defence Brit METHOD AND APPARATUS FOR FORMING A METAL ARTICLE
US4224356A (en) * 1977-05-31 1980-09-23 The Secretary For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland Deposition of metals on a base
US4159353A (en) * 1978-01-19 1979-06-26 Corning Glass Works Platinum coating dense refractories
WO2003072845A1 (en) * 2002-02-28 2003-09-04 Koncentra Holding Ab Thermal spraying of a piston ring
WO2003072844A1 (en) * 2002-02-28 2003-09-04 Man B & W Diesel A/S Thermal spraying of a machine part
US20050073107A1 (en) * 2002-02-28 2005-04-07 Koncentra Holding Ab Thermal spraying of a piston ring
CN100360701C (en) * 2002-02-28 2008-01-09 肯桑特拉控股股份公司 Heat spraying of piston ring
US7332199B2 (en) * 2002-02-28 2008-02-19 Koncentra Marine & Power Ab Thermal spraying of a piston ring
CN114107857A (en) * 2021-11-30 2022-03-01 西北有色金属研究院 High-temperature high-pressure shot peening strengthening method for improving ablation resistance of surface of refractory metal electrode
CN114107857B (en) * 2021-11-30 2022-04-26 西北有色金属研究院 High-temperature high-pressure shot peening strengthening method for improving ablation resistance of surface of refractory metal electrode

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