US3765929A - In situ fluorination of graphite in iron alloy - Google Patents

In situ fluorination of graphite in iron alloy Download PDF

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Publication number
US3765929A
US3765929A US00240268A US3765929DA US3765929A US 3765929 A US3765929 A US 3765929A US 00240268 A US00240268 A US 00240268A US 3765929D A US3765929D A US 3765929DA US 3765929 A US3765929 A US 3765929A
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United States
Prior art keywords
inert gas
chamber
carbon
reaction chamber
centigrade
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US00240268A
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English (en)
Inventor
J Martin
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International Business Machines Corp
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International Business Machines Corp
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Publication date
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Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16CSHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/02Parts of sliding-contact bearings
    • F16C33/04Brasses; Bushes; Linings
    • F16C33/06Sliding surface mainly made of metal
    • F16C33/14Special methods of manufacture; Running-in
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/10Carbon fluorides, e.g. [CF]nor [C2F]n
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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 using gases
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16CSHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C2220/00Shaping
    • F16C2220/60Shaping by removing material, e.g. machining

Definitions

  • This invention pertains to bearings and more particularly to creating self-lubricating bearing surfaces at the surface of high carbon alloy iron materials by fluorinating the carbon particles exposed at the surface to form carbon monofluoride.
  • a self-lubricating bearing surface is created at the surface of high carbon alloy materials such as cast iron having free carbon particles exposed, by reacting such carbon particles to form carbon monofluoride.
  • the present invention provides a self-lubricating bearing on a cast iron surface by converting the exposed particles of free carbon to carbon monofluoride.
  • a part formed of high carbon iron alloy is machined to a desired dimension with an allowance for a slight growth of the carbon particles along the surface during the fluorination process. This compensation is necessary to avoid any post fluorination surface treatment that would involve material removal.
  • the resulting surface is a machined cast iron surface with exposed particles of carbon monofluoride that project a few ten thousandths of an inch from the surrounding iron matrix and form the self-lubricating bearing surface.
  • the surface of a high carbon iron alloy to be treated is prepared by machining the surface with accommodation for material growth where appropriate. For example, it is has been found necessary when practicing the present invention to oversize a bore by 0.0005 of an inch to accommodate the material growth during the conversion of carbon to carbon monofluoride.
  • the prepared part is placed in a nickel or nickel lined chamber for the fluorination process.
  • the fluoride promptly forms a film of nickel fluoride along the surface of the chamber which is adherent, invisible and which precludes further reaction between the nickel surface and the fluorine gas.
  • the chamber is thereupon purged of oxygen and moisture by the introduction of an inert gas such as helium or nitrogen.
  • the chamber is also slowly heated simultaneously with the purge to a temperature usually not exceeding 200 centigrade to assure that any moisture is vaporized and removed from the chamber.
  • fluorine gas is introduced as a partial pressure in an inert gas such as helium or nitrogen.
  • the concentration of fluorine in the inert gas is not allowed to exceed a per cent partial pressure and the usual practice is to use a partial pressure in the range of 3 to 4 percent or a partial pressure of about 25 torr.
  • the temperature is elevated to a value not exceeding 700 centigrade.
  • the temperature limitation likewise is imposed to assure that the fluorine will react selectively with the carbon particles and to the exclusion of the iron.
  • the fluorination process is continued until the exposed graphite or carbon particles resident at the surface are converted to carbon monofluoride.
  • the part is removed from the chamber and rinsed in a mild alkaline solution to neutralize any hydrofluoric acid that might be resident on the surface and is thereafter dried by exposure to a forced flow of air.
  • the part is dipped in a water replacing oil to remove any residual moisture.
  • EXAMPLE 1 A high carbon alloy sample is placed in a 1,000 cc nickel lined reaction chamber. The chamber is thereupon purged with helium at the rate of 50 ccs per minute for a period of 1 hour to remove moisture and oxygen while slowly heating the chamber to 200 centigrade. Fluorine is thereafter introduced into the chamber at a partial pressure of 25 torr in helium at a rate of 50 cc of the gas mixture per minute and the temperature is simultaneously gradually raised to 640 C. Then the introduction of the gas mixture is continued for a period of l hour, while maintaining the reaction chamber at a temperature of 640 centigrade. The sample is then removed and rinsed in a mildly alkaline water solution to neutralize any HF present and thereafter dried in blowing air. The sample is finally dipped in a water replacing oil in preparation for storage and shipment.
  • EXAMPLE 2 A high carbon iron alloy sample with exposed particles at the surface is placed in a 1,000 cc nickel lined reaction chamber. The chamber is thereafter purged with nitrogen at the rate of 50 ccs per minute for a period of 1 hour to remove moisture and oxygen while slowly heating the chamber to 200 centigrade. Fluorine is then introduced into the chamber at a partial pressure of 25 torr in nitrogen at a rate of 50 cc of the gas mixture per minute while simultaneously, gradually raising the chamber temperature to 640 C. Thereafter the introduction of the gas mixture is continued for a period of 1 hour while maintaining the reaction chamber at 640 centrigrade. The sample is then removed and rinsed in a mildly alkaline water solution to neutralize any HF present and thereafter dried in blowing air. The sample is thereupon treated with a water replacing oil in preparation for storage and shipment.
  • EXAMPLE 3 A high carbon iron alloy sample is placed in a 1,000 cc nickel lined reaction chamber. The chamber is then purged by the introduction of helium at the rate of 50 ccs per minute for a period of 1 hour to remove moisture and oxygen while slowly heating the chamber to 200 centigrade. Fluorine is thereupon introduced into the chamber at a partial pressure of 25 torr in helium at the rate of 50 cc per minute while simultaneously, gradually raising the reaction chamber temperature to 400C. Thereafter the introduction of the gas mixture is continued for a period of 4 hours while maintaining the reaction chamber at a temperature of 400 centigrade. The sample is then removed and rinsed in a mildly alkaline solution to neutralize any HF present and thereafter dried in blowing air. The sample is Finally dipped in a water replacing oil in preparation for shipment.
  • selflubricating bearing surfaces may be formed on other parts composed of iron and presenting free carbon particles at the surface in accordance with the above described technique.
  • powdered metal parts which possess free carbon particles could be similarly treated.
  • the method of forming a self-lubricating bearing surface on a high carbon iron alloy part comprising placing said part in a reaction chamber which is resistant to reaction with fluorine gas; purging said reaction chamber with an inert gas to remove substantially all moisture and oxygen; and introducing fluorine gas at a partial pressure not exceeding 76 torr in an inert gas while maintaining said chamber at a temperature not exceeding 700 centigrade until the exposed carbon particles at the surface of said part are substantially completely converted to carbon monofluoride.
  • reaction chamber has a nickel surface which develops a reaction resistant nickel fluoride film thereon in the presence of fluorine gas.
  • the method of forming a self-lubricating bearing surface on a high carbon iron alloy part comprising placing said part in a reaction chamber that is resistant to fluorine gas; purging said reaction chamber with an inert gas while slowly raising the temperature of said chamber to an excess of centigrade to remove substantially all moisture and oxygen therefrom; and introducing fluorine gas at a partial pressure not exceeding 10 percent of the total pressure in an inert gas into said reaction chamber while not exceeding a temperature 700 centigrade until the carbon particles exposed at the surface of said part are substantially completely converted to carbon monofluoride.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Vapour Deposition (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Compressor (AREA)
US00240268A 1972-03-31 1972-03-31 In situ fluorination of graphite in iron alloy Expired - Lifetime US3765929A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US24026872A 1972-03-31 1972-03-31

Publications (1)

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US3765929A true US3765929A (en) 1973-10-16

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US00240268A Expired - Lifetime US3765929A (en) 1972-03-31 1972-03-31 In situ fluorination of graphite in iron alloy

Country Status (6)

Country Link
US (1) US3765929A (enrdf_load_stackoverflow)
JP (1) JPS5243173B2 (enrdf_load_stackoverflow)
CA (1) CA985667A (enrdf_load_stackoverflow)
FR (1) FR2178867B1 (enrdf_load_stackoverflow)
GB (1) GB1407748A (enrdf_load_stackoverflow)
IT (1) IT978355B (enrdf_load_stackoverflow)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4386137A (en) * 1981-09-10 1983-05-31 Nobuatsu Watanabe Process for producing a graphite fluoride type film on the surface of an aluminum substrate
US4467075A (en) * 1983-08-05 1984-08-21 Union Carbide Corporation Surface treatment of a solid polymeric material with a reactive gas
US4484954A (en) * 1982-08-03 1984-11-27 Union Carbide Corporation Halogenation treatment
EP0488497A3 (en) * 1990-11-30 1993-01-20 Daidousanso Co., Ltd. Method of plating steel
EP0678589A1 (en) * 1994-04-18 1995-10-25 Daido Hoxan Inc. Method of carburizing austenitic metal and carburized austenitic metal products
US5556483A (en) * 1994-04-18 1996-09-17 Daido Hoxan, Inc. Method of carburizing austenitic metal
US5792282A (en) * 1995-04-17 1998-08-11 Daido Hoxan, Inc. Method of carburizing austenitic stainless steel and austenitic stainless steel products obtained thereby
US6165597A (en) * 1998-08-12 2000-12-26 Swagelok Company Selective case hardening processes at low temperature

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3998180A (en) * 1975-04-07 1976-12-21 Union Carbide Corporation Vapor deposition apparatus including fluid transfer means

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3091549A (en) * 1960-05-18 1963-05-28 Crane Co Resinous coating of siliconized iron
US3567521A (en) * 1968-08-05 1971-03-02 Mc Donnell Douglas Corp Polymer coating of metal surfaces
US3607747A (en) * 1968-05-27 1971-09-21 Nippon Carbon Co Ltd Lubricant comprising a novel lubricating improver of inorganic graphite fluoride

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3091549A (en) * 1960-05-18 1963-05-28 Crane Co Resinous coating of siliconized iron
US3607747A (en) * 1968-05-27 1971-09-21 Nippon Carbon Co Ltd Lubricant comprising a novel lubricating improver of inorganic graphite fluoride
US3567521A (en) * 1968-08-05 1971-03-02 Mc Donnell Douglas Corp Polymer coating of metal surfaces

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4386137A (en) * 1981-09-10 1983-05-31 Nobuatsu Watanabe Process for producing a graphite fluoride type film on the surface of an aluminum substrate
US4484954A (en) * 1982-08-03 1984-11-27 Union Carbide Corporation Halogenation treatment
EP0102885A3 (en) * 1982-08-03 1985-11-21 Union Carbide Corporation Process for the surface halogenation of polymeric or metallic materials
US4467075A (en) * 1983-08-05 1984-08-21 Union Carbide Corporation Surface treatment of a solid polymeric material with a reactive gas
EP0488497A3 (en) * 1990-11-30 1993-01-20 Daidousanso Co., Ltd. Method of plating steel
US5399211A (en) * 1990-11-30 1995-03-21 Daidousanso Co., Ltd. Method of plating steel
EP0678589A1 (en) * 1994-04-18 1995-10-25 Daido Hoxan Inc. Method of carburizing austenitic metal and carburized austenitic metal products
US5556483A (en) * 1994-04-18 1996-09-17 Daido Hoxan, Inc. Method of carburizing austenitic metal
US5593510A (en) * 1994-04-18 1997-01-14 Daido Hoxan, Inc. Method of carburizing austenitic metal
US5792282A (en) * 1995-04-17 1998-08-11 Daido Hoxan, Inc. Method of carburizing austenitic stainless steel and austenitic stainless steel products obtained thereby
US6165597A (en) * 1998-08-12 2000-12-26 Swagelok Company Selective case hardening processes at low temperature

Also Published As

Publication number Publication date
FR2178867B1 (enrdf_load_stackoverflow) 1975-08-22
JPS498427A (enrdf_load_stackoverflow) 1974-01-25
IT978355B (it) 1974-09-20
FR2178867A1 (enrdf_load_stackoverflow) 1973-11-16
JPS5243173B2 (enrdf_load_stackoverflow) 1977-10-28
CA985667A (en) 1976-03-16
GB1407748A (en) 1975-09-24

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