US2902417A - Application of solid lubricant coatings to surfaces - Google Patents

Application of solid lubricant coatings to surfaces Download PDF

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Publication number
US2902417A
US2902417A US610848A US61084856A US2902417A US 2902417 A US2902417 A US 2902417A US 610848 A US610848 A US 610848A US 61084856 A US61084856 A US 61084856A US 2902417 A US2902417 A US 2902417A
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group
solid lubricant
alloys
molybdenum
adherent
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US610848A
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Jere E Brophy
Robert W Ingraham
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International Business Machines Corp
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International Business Machines Corp
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Priority to US610848A priority Critical patent/US2902417A/en
Priority to FR1189169D priority patent/FR1189169A/en
Priority to GB29223/57A priority patent/GB862818A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/0302—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
    • H01F1/0311—Compounds
    • H01F1/0313—Oxidic compounds
    • H01F1/0315—Ferrites
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces

Definitions

  • This invention relates to a method of providing adherent coatings of solid lubricating materials to surfaces of metal, and non-metals, and in particular to metallic members comprised primarily of fine hardened wires as well as other delicately configured hardened metallic parts.
  • Another object is to provide an improved process for producing adherent coatings of solid lubricant on nonmetals, for example, plastics, ferrites, ceramics, glass and the like.
  • a further object is to provide an improved process for treating the surfaces of fine wires and delicate member, made of hardened alloys, to produce thereon adherent coatings of solid lubricating compounds such as molybdenum disulphide, tungsten disulphide, molybdenum selenide, molybdenum telluride and tungsten telluride.
  • solid lubricating compounds such as molybdenum disulphide, tungsten disulphide, molybdenum selenide, molybdenum telluride and tungsten telluride.
  • Figure l is a sectional view of an electroplating arrangement
  • Figure 2 is a sectional View of a heat-treating apparatus for heat treating parts under pressure.
  • Fig. 1 there is shown an electroplating arrangement suitable for electroplating, for example, molybdenum metal on delicate wire members.
  • the arrangement comprises a tank 1 containing an electrolyte bath 2 which may, for example, consist of 109.2 grams of ammonium formate, 25.2 grams of molybdenum oxide and 2000 milliliters of distilled water.
  • a platinum anode 3 is placed near the wire members 4.
  • Current is supplied from a DC. source 5 which has its positive terminal connected to the anode 3 and its negative terminal connected to a cathode bar 6 from which are suspended conducting hangers 7 for supporting the members 4 in the electrolyte bath.
  • Current supplied to the members 4 is approximately 1 ampere per square inch at 25 C.
  • the surface deposit is usually from .00005" to .0001" and is obtained in a very short period of time.
  • the plated members are washed in water and dried after which they are placed in the heat-treating apparatus shown in Fig. 2.
  • This heat-treating apparatus comprises essentially an oven of the type well known in the art which oven is constituted of an insulating enclosure 10 and a floor 1 1.
  • the latter is provided with an inlet 12 whereby a converting gas is introduced into the oven.
  • An outlet 13 including a valve 14 is also provided. The outlet is open when the gas is first admitted so that atmosphere or gases from a previous heat treatment are removed after which the outlet valve 14 is closed.
  • the gas is then pumped into the oven through the inlet until the required pressure is indicated on a pressure gauge -15 adapted to read the internal pressure in the oven.
  • suitable access means not shown, is provided through which the members are passed into and removed from the interior of the oven.
  • the members 4 are arranged on a suitable support 16 so that the desired surfaces are fully exposed to the oven gas under pressure.
  • Suitable means, not shown, are provided to heat the oven gas to the desired degree of temperature.
  • a temperature gauge 17 is provided to indicate the degree of oven temperature.
  • the heat treatment for converting the molybdenum coating on thin hardened steel wires involved a gas pressure of 400 lbs. p.s.i., a temperature of C. for a period of roughly 110 hours.
  • the temperature was kept at 60 C. for approximately 300 hours at a gas pressure of 400 lbs. p.s.i.
  • Yet other heavier parts were maintained at a temperature of C. for a period of 2 hours at a gas pressure of 400 lbs. p.s.i.
  • the converting gas involved in the above treatments was hydrogen sulphide.
  • hydrogen selenide and hydrogen telluride gases may be employed when the coatings consist of molybdenum selenide, tungsten selenide, molybdenum telluride and tungsten telluride.
  • the invention may be applied with equal facility to the preparation of coatings on material other than steel, for example hardened beryllium compounds, magnetic alloys in which a desired permeability is to be maintained after treatment, aluminum alloys, alloys of copper, alloys of zinc and alloys of silver.
  • the temperature ranges of each of the alloys mentioned above should be below their respective melting points and since molybdenum disulphide melts at 1185 C., the temperature range should be below this point for those alloys whose melting points are above 1185 C., the time and gas pressure in each instance depending upon the thickness in the coating desired.
  • the latter should not be subjected during the coating process to temperatures at which such changes would occur, such temperatures being above the critical points which are of course different for different metals and alloys of metals, the critical point being that temperature at which no change in structure, characteristics and form takes place.
  • the process is especially adaptable to such materials as plastics, ceramics, ferrites, glass, barium titanate and the like.
  • these materials must, of course, be subjected to a preliminary coating process whereby a conductive coating is formed on the surfaces prior to subjecting them to the process constituting the invention.
  • This preliminary coating process may be effected for example by dipping the material in graphite, or by the application of a silver flashing.
  • the method of applying to a surface of a member composed of an alloy selected from the group consisting of steel, copper-base alloys and aluminum-base alloys, an adherent coating of a solid lubricant of a metallic compound selected from the group consisting of sulphides, selenides and tellurides of tungsten and molybdenum comprising electroplating the surface of the member to deposit thereon an adherent electroplate of the metal component of the compound and then subjecting the electroplated surface to a converting gas consisting of at least one of the group consisting of sulphide, selenide and telluride gases at a pressure ranging from in excess of atmospheric pressure to about 400 p.s.i. and at a temperature range of from approximately 60 C. to about 125 C. for a period of from 30 hours to 110 hours depending upon the thickness desired of the metallic compound coating being formed on the surface of the member.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Power Engineering (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Lubricants (AREA)

Description

United States Patent APPLICATION OF SOLID LUBRICANT COATINGS TO SURFACES Jere E. Brophy and Robert W. Ingraham, Endicott, N.Y., assignors to International Business Machines Corporze tion, New York, N.Y., a corporation of New York Application September 19, 1956, Serial No. 610,848
3 Claims. (Cl. 204-37) This invention relates to a method of providing adherent coatings of solid lubricating materials to surfaces of metal, and non-metals, and in particular to metallic members comprised primarily of fine hardened wires as well as other delicately configured hardened metallic parts.
The method of applying solid lubricating coatings comprised of disulphides, selenides and tellurides of such elements as molybdenum and tungsten is set forth in the patent to C. M. Laffon, In, No. 2,420,886. This method is well suited in its application to unhardened metals but not to hardened metals and alloys, for example, alloys of steel, copper and aluminum, because the intense heat called for in this process would not only undo and thus reform the structure of the alloy but would also cause distortion in the shape of the delicate parts.
It is therefore an object of the invention to provide an improved process for producing adherent coatings of solid lubricant on hardened alloys of steel, copper and aluminum.
Another object is to provide an improved process for producing adherent coatings of solid lubricant on nonmetals, for example, plastics, ferrites, ceramics, glass and the like.
A further object is to provide an improved process for treating the surfaces of fine wires and delicate member, made of hardened alloys, to produce thereon adherent coatings of solid lubricating compounds such as molybdenum disulphide, tungsten disulphide, molybdenum selenide, molybdenum telluride and tungsten telluride.
Other objects of the invention will be pointed out in the following description and claims and illustrated in the accompanying drawings, which disclose, by way of examples, the principle of the invention and the best mode, which has been contemplated, of applying that principle.
In the drawings:
Figure l is a sectional view of an electroplating arrangement, and
Figure 2 is a sectional View of a heat-treating apparatus for heat treating parts under pressure.
In Fig. 1 there is shown an electroplating arrangement suitable for electroplating, for example, molybdenum metal on delicate wire members. The arrangement comprises a tank 1 containing an electrolyte bath 2 which may, for example, consist of 109.2 grams of ammonium formate, 25.2 grams of molybdenum oxide and 2000 milliliters of distilled water. A platinum anode 3 is placed near the wire members 4.
Current is supplied from a DC. source 5 which has its positive terminal connected to the anode 3 and its negative terminal connected to a cathode bar 6 from which are suspended conducting hangers 7 for supporting the members 4 in the electrolyte bath. Current supplied to the members 4 is approximately 1 ampere per square inch at 25 C. The surface deposit is usually from .00005" to .0001" and is obtained in a very short period of time.
After the electroplating treatment, the plated members are washed in water and dried after which they are placed in the heat-treating apparatus shown in Fig. 2.
This heat-treating apparatus comprises essentially an oven of the type well known in the art which oven is constituted of an insulating enclosure 10 and a floor 1 1. The latter is provided with an inlet 12 whereby a converting gas is introduced into the oven. An outlet 13 including a valve 14 is also provided. The outlet is open when the gas is first admitted so that atmosphere or gases from a previous heat treatment are removed after which the outlet valve 14 is closed. The gas is then pumped into the oven through the inlet until the required pressure is indicated on a pressure gauge -15 adapted to read the internal pressure in the oven. It is understood that suitable access means, not shown, is provided through which the members are passed into and removed from the interior of the oven. The members 4 are arranged on a suitable support 16 so that the desired surfaces are fully exposed to the oven gas under pressure. Suitable means, not shown, are provided to heat the oven gas to the desired degree of temperature. A temperature gauge 17 is provided to indicate the degree of oven temperature.
In accordance with one aspect of the invention, the heat treatment for converting the molybdenum coating on thin hardened steel wires, for example, involved a gas pressure of 400 lbs. p.s.i., a temperature of C. for a period of roughly 110 hours.
For other delicate hardened steel parts, the temperature was kept at 60 C. for approximately 300 hours at a gas pressure of 400 lbs. p.s.i. Yet other heavier parts were maintained at a temperature of C. for a period of 2 hours at a gas pressure of 400 lbs. p.s.i. The converting gas involved in the above treatments was hydrogen sulphide.
For the purpose of the invention, hydrogen selenide and hydrogen telluride gases may be employed when the coatings consist of molybdenum selenide, tungsten selenide, molybdenum telluride and tungsten telluride.
The invention may be applied with equal facility to the preparation of coatings on material other than steel, for example hardened beryllium compounds, magnetic alloys in which a desired permeability is to be maintained after treatment, aluminum alloys, alloys of copper, alloys of zinc and alloys of silver. The temperature ranges of each of the alloys mentioned above should be below their respective melting points and since molybdenum disulphide melts at 1185 C., the temperature range should be below this point for those alloys whose melting points are above 1185 C., the time and gas pressure in each instance depending upon the thickness in the coating desired.
To prevent changing the crystalline structure in the hardened surfaces of parts, the latter should not be subjected during the coating process to temperatures at which such changes would occur, such temperatures being above the critical points which are of course different for different metals and alloys of metals, the critical point being that temperature at which no change in structure, characteristics and form takes place.
The process is especially adaptable to such materials as plastics, ceramics, ferrites, glass, barium titanate and the like. In this group of non-metals, especially the ferrites and the titanates, the latter would lose their electrical characteristics if they were heated above their respective Curie temperatures. These materials must, of course, be subjected to a preliminary coating process whereby a conductive coating is formed on the surfaces prior to subjecting them to the process constituting the invention. This preliminary coating process may be effected for example by dipping the material in graphite, or by the application of a silver flashing.
a 2,902,417 p i While there have been shown and described and pointed out the fundamental novel features of the invention as applied to a preferred embodiment, it Will be understood that various omissions and substitutions and changes in the-form and details of the device illustrated and in its operation may be made by those skilled in the art, Without departing from the spirit of the invention. It is the intention, therefore, to be limited only as indicated by the scope of the following claims.
What is claimed is:
l. The method of applying to a surface of a member composed of an alloy selected from the group consisting of steel, copper-base alloys and aluminum-base alloys, an adherent coating of a solid lubricant of a metallic compound selected from the group consisting of sulphides, selenides and tellurides of tungsten and molybdenum, comprising electroplating the surface of the member to deposit thereon an adherent electroplate of the metal component of the compound and then subjecting the electroplated surface to a converting gas consisting of at least one of the group consisting of sulphide, selenide and telluride gases at a pressure ranging from in excess of atmospheric pressure to about 400 p.s.i. and at a temperature range of from approximately 60 C. to about 125 C. for a period of from 30 hours to 110 hours depending upon the thickness desired of the metallic compound coating being formed on the surface of the member.
2. The method of applying to a surface of a member composed of hardened steel, an adherent coating of a solid lubricant of a metallic compound selected from the group consisting of sulphides, selenides and tellurides of tungsten and molybdenum, comprising electroplating the surface of the member to deposit thereon an adherent electroplate of the metal component of the compound and then subjecting the electroplated surface to a converting gas consisting of at least one of the group consisting of sulphide, selenide and telluride gases at a pressure ranging from in excess of atmospheric pressure to 4 about 400 p.s.i. and at a temperature range of from approximately C. to about 125 C. for a period of from 30 hours to hoursdepending upon the thickness desired of the metallic compound coating being formed on the surface of the member.
3. The method of applying to a surface of wire members composed of an alloy selected from the group consisting of steel, copper-based alloys and aluminum-base alloys, an adherent coating of a solid lubricant of a metallic compound selected from the group consisting of sulphides, selenides and tellurides of tungsten and molybdenum, comprising electroplating the surfaces of the members to deposit thereon an adherent electroplate of the metal component of the compound and then subjecting the electroplated surfaces to a converting gas consisting of at least one of the group consisting of sulphide, helenide and telluride gases at a pressure ranging from in excess of atmospheric pressure to about 400 p.s.i. and at a temperature range of from about 60 C. to approximately C. for a period of from 30 hours to 110 hours depending upon the thickness desired of the metallic compound coating being formed on the surfaces 0 the members.
References Cited in the file of this patent UNITED STATES PATENTS 1,908,188 Ruben May 9, 1933 2,245,561 Nelson et a1. June 17, 1941 2,381,911 Kathe Aug. 14, 1945 2,395,743 Kannenberg et al Feb. 26, 1946 2,417,133 Schweikher Mar. 11, 1947 2,420,886 Lafioon May 20, 1947 2,430,581 Passel Nov. 11, 1947 2,512,141 Ma et al. June 20, 1950 2,540,635 Steier Feb. 6, 1951 2,697,645 Mitchell Dec. 21, 1954 2,776,254 Bart Jan. 1, 1957 2,784,123 Rappaport Mar. 5, 1957

Claims (1)

1. THE METHOD OF APPLYILNG TO A SURFACE OF A MEMBER COMPOSED OF AN ALLOY SELECTED FROM THE GROUP CONSISTING OF STEEL, COPPER-BASE ALLOYS AND ALUMINUM-BASE ALLOYS, AN ADHERENT COATING OF A SOLID LUBRICANT OF A METALLIC COMPOUND SELECTED FROM THE GROUP CONSISTING OF SULPHIDES, SEL ENIDES AND TELLURIDES OF TUNGSTEN AND MOLYBDENUM, COMPRISING ELECTROPLATING THE SURFACE OF THE MEMBER TO DEPOSIT THEREON AN ADHERENT ELECTROPLATE OF THE METAL COMPONENT OF THE COMPOUND AND THEN SUBJECTING THE ELECTROPLATED SURFACE TO A CONVERTING GAS CONSISTING OF AT LEAST ONE OF THE GROUP CONSISTING OF SULPHIDE, SELENIDE AND TELLURIDE GASES AT A PRESSURE RANGING FROM IN EXCESS OF ATMOSPHERIC PRESSURE TO ABOUT 400 P.S.I. AND AT A TEMPERATURE RANGE OF FROM APPROXIMATELY 60*C. OT ABOUT 125* C. FOR A PERIOD OF FROM 30 HOURS TO 110 HOURS DEPENDING UPON THE THICHNESS DESIRED OF THE METALLIC COMPOUND COATING BEING FORMED ON THE SURFACE OF THE MEMBER.
US610848A 1956-09-19 1956-09-19 Application of solid lubricant coatings to surfaces Expired - Lifetime US2902417A (en)

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US610848A US2902417A (en) 1956-09-19 1956-09-19 Application of solid lubricant coatings to surfaces
FR1189169D FR1189169A (en) 1956-09-19 1957-09-11 Solid lubricating coatings
GB29223/57A GB862818A (en) 1956-09-19 1957-09-17 Application of solid lubricant coatings to surfaces

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3625839A (en) * 1969-05-12 1971-12-07 Jean Leon Spehner Process for applying deposits having lubricant properties to workpieces

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1908188A (en) * 1927-10-28 1933-05-09 Ruben Rectifier Corp Electric current rectifier
US2245561A (en) * 1939-02-08 1941-06-17 Carnation Co Coated container
US2381911A (en) * 1940-09-16 1945-08-14 Bertram C Kathe Electrodeposition
US2395743A (en) * 1942-12-22 1946-02-26 Bell Telephone Labor Inc Method of making dry rectifiers
US2417133A (en) * 1940-11-23 1947-03-11 Du Pont Electrodepositing and heat-treating molybdenum-oxygen deposits
US2420886A (en) * 1942-12-03 1947-05-20 Westinghouse Electric Corp Application of solid lubricant coatings to surfaces
US2430581A (en) * 1944-11-29 1947-11-11 Rca Corp Metallizing nonmetallic bodies
US2512141A (en) * 1945-06-14 1950-06-20 Westinghouse Electric Corp Coating articles with molybdenum
US2540635A (en) * 1948-05-27 1951-02-06 Rca Corp Cesiated monoscope
US2697645A (en) * 1951-08-03 1954-12-21 Glacier Co Ltd Bearing assembly
US2776254A (en) * 1950-09-07 1957-01-01 Siegfried G Bart Rubber bonding process
US2784123A (en) * 1952-05-01 1957-03-05 Rca Corp Secondary electron emitter and process of preparing same

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1908188A (en) * 1927-10-28 1933-05-09 Ruben Rectifier Corp Electric current rectifier
US2245561A (en) * 1939-02-08 1941-06-17 Carnation Co Coated container
US2381911A (en) * 1940-09-16 1945-08-14 Bertram C Kathe Electrodeposition
US2417133A (en) * 1940-11-23 1947-03-11 Du Pont Electrodepositing and heat-treating molybdenum-oxygen deposits
US2420886A (en) * 1942-12-03 1947-05-20 Westinghouse Electric Corp Application of solid lubricant coatings to surfaces
US2395743A (en) * 1942-12-22 1946-02-26 Bell Telephone Labor Inc Method of making dry rectifiers
US2430581A (en) * 1944-11-29 1947-11-11 Rca Corp Metallizing nonmetallic bodies
US2512141A (en) * 1945-06-14 1950-06-20 Westinghouse Electric Corp Coating articles with molybdenum
US2540635A (en) * 1948-05-27 1951-02-06 Rca Corp Cesiated monoscope
US2776254A (en) * 1950-09-07 1957-01-01 Siegfried G Bart Rubber bonding process
US2697645A (en) * 1951-08-03 1954-12-21 Glacier Co Ltd Bearing assembly
US2784123A (en) * 1952-05-01 1957-03-05 Rca Corp Secondary electron emitter and process of preparing same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3625839A (en) * 1969-05-12 1971-12-07 Jean Leon Spehner Process for applying deposits having lubricant properties to workpieces

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FR1189169A (en) 1959-09-30
GB862818A (en) 1961-03-15

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