US3900592A - Method for coating a substrate to provide a titanium or zirconium nitride or carbide deposit having a hardness gradient which increases outwardly from the substrate - Google Patents

Method for coating a substrate to provide a titanium or zirconium nitride or carbide deposit having a hardness gradient which increases outwardly from the substrate Download PDF

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Publication number
US3900592A
US3900592A US382308A US38230873A US3900592A US 3900592 A US3900592 A US 3900592A US 382308 A US382308 A US 382308A US 38230873 A US38230873 A US 38230873A US 3900592 A US3900592 A US 3900592A
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United States
Prior art keywords
substrate
coating
titanium
produce
carbide
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Expired - Lifetime
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US382308A
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English (en)
Inventor
Kurt D Kennedy
Glen R Scheuermann
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Airco Inc
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Airco Inc
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Priority to US382308A priority Critical patent/US3900592A/en
Priority to DE19742431448 priority patent/DE2431448B2/de
Priority to JP8555474A priority patent/JPS5319325B2/ja
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Publication of US3900592A publication Critical patent/US3900592A/en
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/027—Graded interfaces
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • 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
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/24983—Hardness

Definitions

  • a method for coating a substrate with titanium nitride or titanium carbide or zirconium nitride or zirconium carbide is described wherein physical vapor deposition in a vacuum is used, and wherein the substrate is biased by an electrical potential and the composition of the deposit is changed by introducing a gas during the deposition to produce a hardness gradient in the deposit which increases outwardly from the substrate.
  • Titanium Nitride #1100, 325x Vickers Pneumatic Hardness Tests Kglmm 100 qram load 50 gram load 100 qram load 10 gram load METHOD FOR COATING A SUBSTRATE TO PROVIDE A TITANIUM OR ZIRCONIUM NITRIDE OR CARBIDE DEPOSIT HAVING A HARDNESS GRADIENT WHICH INCREASES OUTWARDLY FROM THE SUBSTRATE
  • This invention relates to coated substrates and, more particularly, to the coating of a substrate to produce a high hardness coating.
  • the production of high hardness coatings on substrates may be desired in a wide variety of applications.
  • a titasium carbide coating on the surface of tungsten carbide cutting tools or wear parts produces significantly longer cutting or wear life than is possible with the uncoated tools or parts.
  • Another example is the coating of wear surfaces in the combustion chambers of internal combustion engines, particularly those of the rotary type, with high hardness coatings of titanium nitride or titanium carbide.
  • Another object of the invention is to provide a method for coating a substrate in which very high hardness of the coating is obtained.
  • lt is another object of the invention to provide a method for coating a substrate in which relatively higher deposition rates may be achieved than in many prior art methods.
  • 7 V v A further object of the invention is to provide a method for coating a substrate in which a very strong mechanical bond between a high hardness coating and a relatively softer substrate is achieved.
  • the method of the invention comprises placing the substrate in an evacuated environment and evaporating titanium or zirconium metal in the evacuated environment to produce a vapor and causing the vapor to deposit on the substrate.
  • the composition of the vapor is changed by reacting it with a gas during deposition to produce a hardness gradient in the deposit which increases outwardly from the substrate.
  • an electrical potential is applied to the substrate during the deposition process sufficient to produce a voltage difference of at least 200 volts between the substrate and the crucible.
  • the method is applicable to coating a variety of substrates, including metals such as aluminum, magnesium, iron, and alloys thereof, and to coating metal composites such as tungsten carbide.
  • substrates including metals such as aluminum, magnesium, iron, and alloys thereof
  • metal composites such as tungsten carbide.
  • the particular materials used depends upon the use of the product being manufactured. For example, a coating of titanium nitride on a titanium carbide substrate will produce a very hard product suitable for use in cutting tools and wear parts.
  • Coatings deposited in accordance with the invention may comprise titanium nitride, titanium carbide, zirconium nitride or zirconium carbide for wear parts, cutting tools, or corrosion resistance, etc.
  • the invention is applicable to any situation wherein it is desirable to produce a hard coating on a relatively softer substrate.
  • the equipment utilized to carry out the method of the invention may be of any suitable type in which a vapor of the material to be deposited is produced in a vacuum. Heating of the coating material in order to vaporize same may be accomplished by such means as resistance heating, induction heating, or preferably electron beam heating. Equipment for accomplishing high vacuum vapor deposition is known in the art andis commercially available on the market from the Airco Temescal Division of Airco, 'lnc., Berkeley, Calif. The particular structure of the equipment is not critical to the invention and therefore will not be further de-' the initial pressure in the chamber is of the order of 1 millitorr or less.
  • an electrical potential is applied to the substrate during deposition.
  • the electrical potential is sufficient to produce a glow discharge.
  • an electrical bias of negative 200 volts or greater will produce the desired glow I discharge.
  • the electrical biasing will also tend to heat the substrate, which is desirable in most cases to enhance the quality of the deposit.
  • the titanium or zirconium of which a nitride or carbide is to be deposited is evaporated within the evacuated environment.
  • the term titanium is meant to include pure titanium and titanium base alloys as well.
  • the tenn zirconium is meant to include pure zirconium and zirconium base alloys as well.
  • the metal thusevaporated will pass in the vapor form within the evacuated environment and when vapor particles thereof strike the substrate, they will condense on the substrate and thereby form a deposit on the surface thereof. The particular conditions under which this occurs are well known to those skilled in the art and therefore will not be further detailed herein.
  • the respective dimensional responses of the substrate and the coating to thermal or mechanical forces may be substantially different. As a result, very high shear forces may concentrate at the interface between the coating and the substrate. If this interface is weak for any reason, such as poor adhesion or the presence of discontinuities or foreign substances, failure can result.
  • the method of the invention creates a hardness gradient in the coating. Ideally, this is accomplished by making the mechanical and thermal properties of the coating and the substrate at the interface identical. Transition from the mechanical and thermal properties at the interface to the higher strength properties on the outer surface of the deposit are made to occur gradually from the interface to the outersurface.
  • the elimination of thermal and mechani cal property discontinuities distributes shear stresses over a volume, rather than concentrating them at a surface plane at the interface, thus rendering the resultant product more resistant to thermal or mechanical cycling.
  • the composition of the vapor produced in the evacuated environment is changed gradually during the deposition process to produce a hardness gradient in the deposit which increases outwardly from the substrate.
  • This is accomplished by the introduction of a reactant gas to the vapor gradually increasing the gas pressure, such as from about one micron to about 50 microns.
  • the reactant gas may such as to produce a nitride or carbide, and may be acetylene, nitrogen, methane, etc., for example.
  • the photomicrograph enlarged 325 times illustrates the cross section of a substrate coated in accordance with the invention and illustrating the results of Vickers Pneumatic hardness tests in kilograms per square millimeter taken across the cross section.
  • the substrate is indicatedv at the very bottom of the illustration and five regions of the coating are indicated at A, B, C, .Dand E in the photograph. These regions represent different partial pressures of nitrogen present during the evaporation process.
  • Region A in which no nitrogen bleed was used, is pure titanium.
  • Region B was deposited at 3 to 4 microns partial pressure nitrogen, region C at 4 to 6.5 microns partial pressure of nitrogen, region D at microns partial pressure of nitrogen, and region E at 12 microns partial pressure of nitrogen. Deposition rates for all regions was 0.0008 inch per minute except for region. E, in which the rate was 0.0003 inch.
  • Evaporation 'occurred from a pure titanium ingot with a 25 kilowatt electron beam at'a starting pressure of 0.01 micron in the vacuum chamber.
  • the temperature of the substrate was l600F.
  • Pressure of the nitrogen was increased to the 12 micron maximum in a time period of 40 minutes and then was held constant in the region E.
  • pure titanium deposited at the substrate surface in the region A offered relatively low hardness values, and the Vickers hardness values increased substantially in the regions B through D.
  • the outer surface offered the maximum Vickers hardness of 2,450 kilograms per square millimeter under a 100 gram load.
  • the illustration indicates that the surface hardness is substantially increased by depositing titanium nitride in accordance with the invention.
  • TITANIUM-NITRIDE HARDNESS AS A FUNCTION OF BIAS AND NITROGEN PRESSURE
  • the substrate temperature was l,600F and the deposition rate was 1 i 0.3 mils per minute in all cases.
  • Zirconium has been deposited in accordance with the invention and similar results have been achieved. Hardness values of zirconium nitride deposited by evaporating zirconium with a N bleed were as follows:
  • Zirconium carbide may be produced in a similar manner.
  • the invention provides an improved method for coating a substrate in which very high hardness of the coating is obtained. Relatively high deposition rates may also be achieved in comparison with many prior art methods. A very strong mechanical bond is obtained between the high hardness coating and the relatively softer substrate.
  • a method for coating a substrate with a nitride or carbide of titanium or zirconium comprising, placing the substrate in an evacuated environment, evaporating titanium or zirconium from a crucible in the evacuated environment to produce a vapor and causing the vapor to deposit on the substrate initially as titanium or zirconium, applying an electrical potential during deposition sufficient to produce a voltage difference of at least 200 volts between the substrate and the crucible, and introducing a reactant gas with a gradually increasing partial pressure to the vapor to change the composition of the deposit from its initial composition to increasing nitride or carbide in the direction outwardly from the substrate to produce a hardness gradient in the deposit which increases outwardly from the substrate.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Ceramic Products (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
US382308A 1973-07-25 1973-07-25 Method for coating a substrate to provide a titanium or zirconium nitride or carbide deposit having a hardness gradient which increases outwardly from the substrate Expired - Lifetime US3900592A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US382308A US3900592A (en) 1973-07-25 1973-07-25 Method for coating a substrate to provide a titanium or zirconium nitride or carbide deposit having a hardness gradient which increases outwardly from the substrate
DE19742431448 DE2431448B2 (de) 1973-07-25 1974-07-01 Verfahren zum beschichten eines substrates mit einem nitrid oder carbid von titan oder zirkonium durch reaktives aufdampfen
JP8555474A JPS5319325B2 (de) 1973-07-25 1974-07-25

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US382308A US3900592A (en) 1973-07-25 1973-07-25 Method for coating a substrate to provide a titanium or zirconium nitride or carbide deposit having a hardness gradient which increases outwardly from the substrate

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JP (1) JPS5319325B2 (de)
DE (1) DE2431448B2 (de)

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US4107352A (en) * 1977-01-13 1978-08-15 Westinghouse Canada Limited Chemical vapor deposition
US4109061A (en) * 1977-12-08 1978-08-22 United Technologies Corporation Method for altering the composition and structure of aluminum bearing overlay alloy coatings during deposition from metallic vapor
US4226082A (en) * 1976-06-07 1980-10-07 Nobuo Nishida Ornamental part for watches and method of producing the same
US4254159A (en) * 1977-12-23 1981-03-03 Balzers Aktiengesellschaft Fur Hochvakuumtechnik Und Dunne Schichten Method of producing gold-color coatings
US4260658A (en) * 1979-06-21 1981-04-07 Kobe, Inc. Erosion resistant surface
US4333962A (en) * 1979-09-04 1982-06-08 Balzers Aktiengesellschaft Method for producing gold color coatings
US4346123A (en) * 1979-08-02 1982-08-24 Balzers Aktiengesellschaft Method of depositing hard wear-resistant coatings on substrates
US4415602A (en) * 1981-07-24 1983-11-15 Canadian Industrial Innovation Centre/Waterloo Reactive plating method and product
US4466991A (en) * 1946-07-17 1984-08-21 Vsesojuzny Nauchno-Issledovatelsky Instrumentalny Institut Cutting tool hardening method
US4514240A (en) * 1980-10-30 1985-04-30 Societe Europeenne De Propulsion Method for adhesively bonding parts made of refractory materials
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DE3535022A1 (de) * 1985-02-08 1986-08-14 Citizen Watch Co., Ltd., Tokio/Tokyo Verfahren zur herstellung von ueberzugsschichten durch ionenstrahlplattieren
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DE3731127A1 (de) * 1987-03-12 1988-09-22 Vac Tec Syst Verfahren und vorrichtung zur vakuum-lichtbogenplasma-ablagerung dekorativer und abnutzungsfester beschichtungen
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Cited By (91)

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Publication number Priority date Publication date Assignee Title
US4466991A (en) * 1946-07-17 1984-08-21 Vsesojuzny Nauchno-Issledovatelsky Instrumentalny Institut Cutting tool hardening method
US4035541A (en) * 1975-11-17 1977-07-12 Kennametal Inc. Sintered cemented carbide body coated with three layers
US4226082A (en) * 1976-06-07 1980-10-07 Nobuo Nishida Ornamental part for watches and method of producing the same
US4107352A (en) * 1977-01-13 1978-08-15 Westinghouse Canada Limited Chemical vapor deposition
US4109061A (en) * 1977-12-08 1978-08-22 United Technologies Corporation Method for altering the composition and structure of aluminum bearing overlay alloy coatings during deposition from metallic vapor
US4254159A (en) * 1977-12-23 1981-03-03 Balzers Aktiengesellschaft Fur Hochvakuumtechnik Und Dunne Schichten Method of producing gold-color coatings
US4260658A (en) * 1979-06-21 1981-04-07 Kobe, Inc. Erosion resistant surface
US4346123A (en) * 1979-08-02 1982-08-24 Balzers Aktiengesellschaft Method of depositing hard wear-resistant coatings on substrates
US4333962A (en) * 1979-09-04 1982-06-08 Balzers Aktiengesellschaft Method for producing gold color coatings
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JPS5034610A (de) 1975-04-03

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