EP1386018B1 - Procede de traitement de pieces en alliage ferreux pour ameliorer leurs proprietes frottantes, sans perte de leur durete ni deformation - Google Patents

Procede de traitement de pieces en alliage ferreux pour ameliorer leurs proprietes frottantes, sans perte de leur durete ni deformation Download PDF

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Publication number
EP1386018B1
EP1386018B1 EP02727644A EP02727644A EP1386018B1 EP 1386018 B1 EP1386018 B1 EP 1386018B1 EP 02727644 A EP02727644 A EP 02727644A EP 02727644 A EP02727644 A EP 02727644A EP 1386018 B1 EP1386018 B1 EP 1386018B1
Authority
EP
European Patent Office
Prior art keywords
condition
coating
ferrous alloy
fractal dimension
improve
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
Application number
EP02727644A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1386018A2 (fr
Inventor
Stéphane CHOMER
Jean-Paul Terrat
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hydromecanique et Frottement SAS
Original Assignee
HEF SAS
Hydromecanique et Frottement SAS
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Filing date
Publication date
Application filed by HEF SAS, Hydromecanique et Frottement SAS filed Critical HEF SAS
Publication of EP1386018A2 publication Critical patent/EP1386018A2/fr
Application granted granted Critical
Publication of EP1386018B1 publication Critical patent/EP1386018B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12951—Fe-base component
    • Y10T428/12958—Next to Fe-base component
    • 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
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the present invention relates to a process for treating ferrous alloy parts to improve their friction properties, mainly their resistance to seizing and sticking, without risk of loss of hardness or deformation.
  • the invention applies to steel or cast iron parts with high mechanical properties, that is to say, whose tempering temperature is below 200 ° C.
  • the lubricant film must have a thickness greater than the height of the surface roughnesses.
  • the thickness of the film depends to a great extent on the superficial physicochemical properties and surface morphology at the microscopic scale.
  • the machining rough steel has surface characteristics such that the thickness of the lubricant films is generally insufficient to provide continuous lubrication when the loads or speeds become large.
  • Phosphating is mainly intended to increase the seizing resistance of the lubricated contacts, the sulphurization additionally confers solder inhibition properties on the surface by the formation of iron sulphide (hexagonal FeS), and the anti-seizing properties are then greater than those obtained with phosphatation.
  • hexagonal FeS iron sulphide
  • the physicochemical properties of compounds such as iron phosphate or iron sulphide are at the origin of the best wetting of lubricants, the surface energy of these constituents being much greater than that of steel. These constituents furthermore have a low shear strength and an excellent accommodation aptitude, which enables them to improve the running-in conditions and wear resistance of the contacts subjected to surface fatigue.
  • the low temperature sulphurization is carried out in a mixture of molten salts at a temperature around 200 ° C with the assistance of anodic electrolysis leading to the formation of FeS hexagonal iron sulphide. This latter process is taught in the Applicant's patent FR-A-2,050,754 .
  • An object of the invention is to obtain ferrous alloy parts having improved friction properties under extreme conditions of pressure and speed, mainly their resistance to seizing and bonding without loss of hardness or deformation.
  • the Applicant has found, surprisingly, that for ferrous alloy parts comprising an iron sulphide coating, the fractal dimension of the surface of the iron sulphide coating played a role. preponderant, and in any case much more influential than that of stoichiometry, crystalline structure or purity.
  • the Applicant has therefore developed a method for obtaining a ferrous alloy piece supporting a very high seizing load with a very low dispersion and a high number of cycles, consisting in depositing on said part a sulphide coating.
  • a sulphide coating of iron having a suitable thickness and ratio Fe / S, characterized in that the coating is selected from those whose surface has a fractal dimension of at least 2.6.
  • the parts obtained according to the method of the present invention support a galling load according to the FAVILLE LEVALLY machine test according to ASTM-D-2670 at least equal to about 3000 daN with a tolerance of at most equal to about 5%. and a number of cycles according to the Hamsler test of at least about 300.
  • the coating is selected from those whose surface has a fractal dimension of between 2.65 and 2.75.
  • the coating is selected from those having a stoichiometry corresponding to a Fe / S ratio of between about 0.69 and 0.85.
  • the coating will also be favorably selected from those having a thickness of less than about 15 microns, more preferably less than about 6 microns.
  • the fractal dimension is obtained from a roughness meter, for example a contactless type confocal 3D roughness tester, the characteristics of which are as follows: Lateral resolution 300 nm Vertical resolution 30 nm Vertical travel 1 mm
  • the data obtained using the rugosimeter are then introduced into a specific calculation algorithm that extracts the mathematical quantities required to obtain the fractal dimension.
  • the iron sulphide coatings of the ferrous alloy parts are obtained by treatments known to those skilled in the art, for example by electrolytic sulphidation in molten salt bath according to the patent FR-A-1,406,530 , or sulfurization in brine or sulphurization salt bath as the Applicant has demonstrated in his experiments.
  • test pieces After treatment, the test pieces comprise an iron sulphide coating.
  • the specimens are then oiled and then subjected to the FAVILLE LEVALLY machine test (according to ASTM-D-2670) by rotating the treated cylinder between two hardened and tempered 16NC6 steel jaws without additional treatment.
  • the test consists of increasing the load applied on the cylinder until seizure occurs.
  • the seizure load is then determined, the tests having been repeated 5 times in order to evaluate the average seizing load and the measurement dispersion.
  • Each cylinder is characterized prior to testing to determine the fractal size of the coating surface after treatment.
  • the fractal dimension is obtained from a contactless confocal type 3D rugosimeter, the characteristics of which are as follows: Lateral resolution 300 nm Vertical resolution 30 nm Vertical travel 1 mm
  • the data obtained using the rugosimeter are then introduced into a specific calculation algorithm that extracts the mathematical quantities required to obtain the fractal dimension.
  • the coatings whose surface has a fractal dimension of at least 2.6 are selected.
  • the parts (cylinders) according to the invention have a galling load according to the machine test FAVILLE LEVALLY according to ASTM-D-2670 at least equal to about 3000 daN.
  • the cylinders coated with iron sulfide according to the invention have a seizure load about 3 times higher than the best results obtained until now with slightly fractal iron sulfide.
  • the dispersion of the results is 4 times smaller when the iron sulphide has a fractal size (dimension) greater than 2.6.
  • Tests were carried out according to DIN 51350 (parts 1 to 5) on a machine called a "4-ball machine" to complete the seizure tests and to check the influence of the Fe / S ratio and the thickness of the sulphide layer. of iron.
  • the parts After treatment, the parts have an iron sulphide coating.
  • the tests are carried out in a bath of pure mineral oil at 60 ° C.
  • the average seizing charges and the dispersions obtained with 5 tests are grouped in the following table.
  • the fractal dimension of the surface of the coating was measured using the same device as that described in Example 1. The results are given in Table II. ⁇ u> Table II ⁇ / u> Treatment Fractal dimension of the surface of the coating (D) Fe / S ratio ( ⁇ 0.2) Layer thickness ( ⁇ 1 ⁇ m) Medium galling load (DaN) Dispersion (%) Condition 1, 15 min. at 2.8 A / dm 2 2.23 0.81 5 300 20 Condition 1, 15 min.
  • the coatings are selected from those whose surface has a fractal dimension of at least 2.6.
  • the cylinders were processed and selected under the conditions 1, 2 and 3 described above.
  • the fractal dimension of the coating surface of each cylinder was measured using the device described in Example 1.
  • the coatings are selected from those whose surface has a fractal dimension of at least 2.6.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Lubricants (AREA)
  • Heat Treatment Of Articles (AREA)
  • Heat Treatment Of Steel (AREA)
  • Chemically Coating (AREA)
  • Paper (AREA)
  • Adornments (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
EP02727644A 2001-04-04 2002-03-28 Procede de traitement de pieces en alliage ferreux pour ameliorer leurs proprietes frottantes, sans perte de leur durete ni deformation Expired - Lifetime EP1386018B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0104580 2001-04-04
FR0104580A FR2823227B1 (fr) 2001-04-04 2001-04-04 Procede de traitement de pieces en alliage ferreux pour ameliorer leurs proprietes frottantes, sans perte de leur durete ni deformation
PCT/FR2002/001091 WO2002081769A2 (fr) 2001-04-04 2002-03-28 Procede de traitement de pieces en alliage ferreux pour ameliorer leurs proprietes frottantes, sans perte de leur durete ni deformation

Publications (2)

Publication Number Publication Date
EP1386018A2 EP1386018A2 (fr) 2004-02-04
EP1386018B1 true EP1386018B1 (fr) 2010-05-19

Family

ID=8861931

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02727644A Expired - Lifetime EP1386018B1 (fr) 2001-04-04 2002-03-28 Procede de traitement de pieces en alliage ferreux pour ameliorer leurs proprietes frottantes, sans perte de leur durete ni deformation

Country Status (12)

Country Link
US (1) US7172794B2 (ja)
EP (1) EP1386018B1 (ja)
JP (1) JP4545376B2 (ja)
AT (1) ATE468419T1 (ja)
AU (1) AU2002257854A1 (ja)
CA (1) CA2443005C (ja)
DE (1) DE60236425D1 (ja)
ES (1) ES2344832T3 (ja)
FR (1) FR2823227B1 (ja)
MY (1) MY137691A (ja)
TW (1) TWI275664B (ja)
WO (1) WO2002081769A2 (ja)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2860806B1 (fr) * 2003-10-14 2006-01-06 Stephanois Rech Mec Procede de traitement par sulfuration de pieces en alliage ferreux
FR2909102B1 (fr) * 2006-11-24 2009-03-06 Hef Soc Par Actions Simplifiee Procede de sulfuration de pieces en alliage ferreux en solution aqueuse.
WO2011001640A1 (ja) * 2009-06-29 2011-01-06 新日本製鐵株式会社 Ｚｎ－Ａｌめっき鉄線及びその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5981934A (en) * 1996-09-12 1999-11-09 Canon Kabushiki Kaisha Photovoltaic element having a transparent conductive layer with specified fractal dimension and fractal property
US6689424B1 (en) * 1999-05-28 2004-02-10 Inframat Corporation Solid lubricant coatings produced by thermal spray methods

Also Published As

Publication number Publication date
WO2002081769A3 (fr) 2002-12-12
US7172794B2 (en) 2007-02-06
CA2443005C (fr) 2009-02-03
US20040146753A1 (en) 2004-07-29
EP1386018A2 (fr) 2004-02-04
WO2002081769A2 (fr) 2002-10-17
TWI275664B (en) 2007-03-11
FR2823227B1 (fr) 2004-04-02
CA2443005A1 (fr) 2002-10-17
DE60236425D1 (de) 2010-07-01
MY137691A (en) 2009-02-27
JP2004526059A (ja) 2004-08-26
JP4545376B2 (ja) 2010-09-15
AU2002257854A1 (en) 2002-10-21
ATE468419T1 (de) 2010-06-15
ES2344832T3 (es) 2010-09-08
FR2823227A1 (fr) 2002-10-11

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