US3765929A - In situ fluorination of graphite in iron alloy - Google Patents
In situ fluorination of graphite in iron alloy Download PDFInfo
- 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
- Authority
- US
- United States
- Prior art keywords
- inert gas
- chamber
- carbon
- reaction chamber
- centigrade
- Prior art date
- 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
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910000640 Fe alloy Inorganic materials 0.000 title claims abstract description 11
- 238000003682 fluorination reaction Methods 0.000 title description 8
- 229910002804 graphite Inorganic materials 0.000 title description 4
- 239000010439 graphite Substances 0.000 title description 4
- 238000011065 in-situ storage Methods 0.000 title description 3
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 17
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011737 fluorine Substances 0.000 claims abstract description 16
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 16
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 238000010926 purge Methods 0.000 claims description 11
- 239000001307 helium Substances 0.000 claims description 10
- 229910052734 helium Inorganic materials 0.000 claims description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 4
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000009834 vaporization Methods 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims description 2
- 230000001050 lubricating effect Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910001018 Cast iron Inorganic materials 0.000 description 4
- 229910001339 C alloy Inorganic materials 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000004308 accommodation Effects 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000012255 powdered metal Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
- F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
- F16C33/02—Parts of sliding-contact bearings
- F16C33/04—Brasses; Bushes; Linings
- F16C33/06—Sliding surface mainly made of metal
- F16C33/14—Special methods of manufacture; Running-in
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/10—Carbon fluorides, e.g. [CF]nor [C2F]n
-
- 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
- C23C8/06—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 using gases
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
- F16C2220/00—Shaping
- F16C2220/60—Shaping 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.
Landscapes
- 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)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US24026872A | 1972-03-31 | 1972-03-31 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3765929A true US3765929A (en) | 1973-10-16 |
Family
ID=22905853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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)
| 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)
| 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)
| 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 |
-
1972
- 1972-03-31 US US00240268A patent/US3765929A/en not_active Expired - Lifetime
-
1973
- 1973-01-23 IT IT7319465A patent/IT978355B/it active
- 1973-02-20 FR FR7306807A patent/FR2178867B1/fr not_active Expired
- 1973-02-22 JP JP48020760A patent/JPS5243173B2/ja not_active Expired
- 1973-02-28 CA CA165,476A patent/CA985667A/en not_active Expired
- 1973-03-13 GB GB1210773A patent/GB1407748A/en not_active Expired
Patent Citations (3)
| 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)
| 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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