EP2768932A1 - Friction piece operating in a lubricated medium - Google Patents

Friction piece operating in a lubricated medium

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Publication number
EP2768932A1
EP2768932A1 EP12780220.5A EP12780220A EP2768932A1 EP 2768932 A1 EP2768932 A1 EP 2768932A1 EP 12780220 A EP12780220 A EP 12780220A EP 2768932 A1 EP2768932 A1 EP 2768932A1
Authority
EP
European Patent Office
Prior art keywords
friction
coating
modtc
wear
dcx
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.)
Granted
Application number
EP12780220.5A
Other languages
German (de)
French (fr)
Other versions
EP2768932B8 (en
EP2768932B1 (en
Inventor
Philippe Maurin-Perrier
Christophe Heau
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 EP2768932A1 publication Critical patent/EP2768932A1/en
Application granted granted Critical
Publication of EP2768932B1 publication Critical patent/EP2768932B1/en
Publication of EP2768932B8 publication Critical patent/EP2768932B8/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/02—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a non-macromolecular organic compound
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M135/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium
    • C10M135/12—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M135/14—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond
    • C10M135/18—Thio-acids; Thiocyanates; Derivatives thereof having a carbon-to-sulfur double bond thiocarbamic type, e.g. containing the groups
    • 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
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/72—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/061—Carbides; Hydrides; Nitrides
    • C10M2201/0613—Carbides; Hydrides; Nitrides used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066—Thiocarbamic type compounds
    • C10M2219/068—Thiocarbamate metal salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2080/00—Special pretreatment of the material to be lubricated, e.g. phosphatising or chromatising of a metal

Definitions

  • the invention relates to the technical field of tribology in a lubricated medium.
  • the invention relates to friction parts operating in a lubricated medium comprising a friction modifier, such as automobile components.
  • DLC coatings are also known to fulfill a second function which is to protect the coatings against wear.
  • Such an additive is advantageously MoDTC which, in a hot rubbing contact, reacts chemically to give rise to the formation of MoS 2 type compounds perfectly known to those skilled in the art to act as a solid lubricant.
  • the invention thus lies in the combination of the effects of chromium nitride and MoDTC to significantly reduce the coefficient of friction, without impairing the hardness.
  • Friction tests were performed to evaluate the behavior in a lubricated medium comprising a MoDTC friction modifier, a DLC coating and a chromium nitride coating, recalling, in a well-known manner, that in the In the case of a DLC coating, in order to reinforce its mechanical strength, it is possible to deposit an underlayer, for example, of chromium nitride.
  • Table below shows the tests carried out on four coatings, namely, DCX- 0, DCX-1, DCX-2, DCX-3, the DCX-3 coating being in accordance with the invention.
  • the set of layers comprises a coating of chromium nitride produced by magnetron reactive sputtering.
  • the steel specimens are first cleaned, which are then positioned on supports placed in the vacuum deposition chamber.
  • the inside of the machine and the parts to be coated are heated at a temperature of 150 ° C for 2 hours in order to degas the parts and the machine deposit.
  • the pieces are subjected to an ionic etching in an argon atmosphere, the purpose of which is to remove the thin layers of natural oxide and thus allow a strong adhesion of the coating.
  • the deposition of chromium nitride is obtained by reactive magnetron sputtering of a Cr target in an argon / nitrogen mixture.
  • the nitrogen flow rate is slaved to an optical measurement of the emission of Cr in the plasma, so that the deposit contains 40 +/- 5 atomic% of nitrogen.
  • a deposit of CrN exhibiting cfc crystallization of the NaCl type, the microhardness of which is 1800 +/- 200 Hv is obtained.
  • a coating of DLC type aC: H by PACVD technique is deposited by cracking a hydrocarbon in a plasma, here acetylene.
  • DCX-1 the final deposition of an aC-type layer by magnetron sputtering of a graphite target.
  • DCX-2 a pure oxygen plasma is generated and the deposit is bombarded by ions from the plasma for 10 minutes, which makes it possible to modify the surface chemistry of the deposit.
  • the plane consists of a steel specimen, polished to a Ra level of 0.02 ⁇ .
  • the ball is made of steel
  • the load applied on the ball is 10N, which gives a diameter
  • the ball is animated by an alternating movement, whose race is
  • the sliding speed follows a sinus-like profile, whose average value is 3.5 cm / s.
  • the test is conducted for a period of 15,000 cycles at a temperature of 110.degree.
  • the sliding speed, pressure and temperature conditions are such that the friction reducing additive reacts to fulfill its role.
  • the attached graph ( Figure 1) summarizes the average wear rates (used volume based on the number of cycles of friction). For each coating, 3 tests were carried out, the average wear was calculated. The error bars represent, not an error, but the smallest value and the largest value for these 3 tests.
  • the DCX-3 coating according to the invention has zero wear in test fm, the friction diameter is very slightly greater than the initial contact diameter.
  • Chromium nitride has a hardness of the order of 1800 Hv.
  • the low coefficient of friction is mainly due to the friction reduction additive: the MoDTC.
  • the combination DLC facing a steel friction antagonist, MoDTC is not compatible to perform both functions, namely, resist wear on the one hand, and get a coefficient of friction as low as possible on the other hand, while the combination claimed, namely, chromium nitride and MoDTC advantageously allows these two functions to be performed.
  • the invention also relates to the use of parts thus coated and working in a lubricated medium containing MoDTC in the automotive field, in particular for engines and gearboxes.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Physical Vapour Deposition (AREA)
  • Lubricants (AREA)
  • Sliding-Contact Bearings (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Gears, Cams (AREA)

Abstract

The lubricated medium comprises a friction modifier. A coating is applied to the part. According to the invention, the coating is chromium nitride and the friction modifier is MoDTC. Chromium nitride is selected to have NaCl type crystallisation with a microhardness of 1800 +/- 200 HV.

Description

PIECE DE FROTTEMENT FONCTIONNANT EN MILIEU  FRICTION PIECE OPERATING IN THE ENVIRONMENT
LUBRIFIE  LUBRICATES
L'invention concerne le domaine technique de la tribologie en milieu lubrifié. The invention relates to the technical field of tribology in a lubricated medium.
Plus particulièrement, l'invention concerne les pièces de frottement fonctionnant en milieu lubrifié comportant un modificateur de frottement, comme par exemple des composants automobile. More particularly, the invention relates to friction parts operating in a lubricated medium comprising a friction modifier, such as automobile components.
Il est notoirement connu pour un homme du métier d'utiliser des revêtements minces du type DLC afin de réduire le frottement de composants mécaniques fonctionnant en milieu lubrifié. It is well known to a person skilled in the art to use DLC-type thin coatings in order to reduce the friction of mechanical components operating in a lubricated medium.
Les revêtements DLC sont également connus pour remplir une deuxième fonction qui est de protéger les revêtements contre l'usure.  DLC coatings are also known to fulfill a second function which is to protect the coatings against wear.
Toujours en ayant pour objectif de permettre une réduction significative du coefficient de frottement, on a proposé de rajouter un additif modificateur de frottement. Un tel additif est avantageusement le MoDTC qui, dans un contact frottant à chaud, réagit chimiquement pour donner lieu à la formation de composés du type MoS2 parfaitement connus par un homme du métier pour agir en tant que lubrifiant solide. Still with the aim of allowing a significant reduction in the coefficient of friction, it has been proposed to add a friction modifier additive. Such an additive is advantageously MoDTC which, in a hot rubbing contact, reacts chemically to give rise to the formation of MoS 2 type compounds perfectly known to those skilled in the art to act as a solid lubricant.
A partir de cet état de la technique, il peut paraître intéressant de combiner les effets du DLC et du MoDTC pour bénéficier de l'effet de synergie des deux, afin de réduire encore plus le coefficient de frottement. From this state of the art, it may seem interesting to combine the effects of DLC and MoDTC to benefit from the synergistic effect of both, to further reduce the coefficient of friction.
Toutefois, il est apparu, suite à des essais réalisés, qu'une telle combinaison ne donne pas des résultats satisfaisant. Notamment, il a été observé, que les revêtements DLC qui contiennent de l'hydrogène, présentent un taux d'usure important, en présence du MoDTC. Lorsque le revêtement DLC n'est pas hydrogéné, le phénomène d'usure est moins important mais dans ce cas, l'application, relève d'une technique complexe et coûteuse. However, it has appeared, following tests carried out, that such a combination does not give satisfactory results. In particular, it has been observed that DLC coatings which contain hydrogen have a high wear rate, in the presence of the MoDTC. When the DLC coating is not hydrogenated, the phenomenon of wear is less important, but in this case the application is a complex and expensive technique.
D'une manière surprenante et inattendue des essais ont démontré que dans un milieu lubrifié, comportant un modificateur de frottement MoDTC, le fait de remplacer le revêtement DLC par un revêtement de nitrure de chrome, donne des résultats particulièrement satisfaisants tant au niveau de la réduction du coefficient de frottement que de la protection de la pièce considérée contre l'usure.  Surprisingly and unexpectedly, tests have shown that in a lubricated medium, with a MoDTC friction modifier, the fact of replacing the DLC coating with a chromium nitride coating gives particularly satisfactory results in terms of the reduction. coefficient of friction than the protection of the part under consideration against wear.
Autrement dit, à l'inverse du DLC utilisé dans un milieu lubrifié et comportant un modificateur de frottement MoDTC où apparaît un phénomène d'usure, un tel phénomène n'intervient pas avec le nitrure de chrome. L'invention réside donc dans la combinaison des effets du nitrure de chrome et du MoDTC permettant de réduire de manière significative le coefficient de frottement, sans pour autant altérer la dureté.  In other words, unlike the DLC used in a lubricated medium and comprising a MoDTC friction modifier where there is a wear phenomenon, such a phenomenon does not interfere with the chromium nitride. The invention thus lies in the combination of the effects of chromium nitride and MoDTC to significantly reduce the coefficient of friction, without impairing the hardness.
Cette sélection du nitrure de chrome va à rencontre des connaissances générales de l'homme du métier qui utilise désormais et quasiment exclusivement le DLC en milieu lubrifié, ne comportant pas de modificateur de frottement en lieu et place du nitrure de chrome.  This selection of chromium nitride goes against the general knowledge of the skilled person who now uses and almost exclusively DLC in lubricated medium, with no friction modifier instead of chromium nitride.
Des essais de frottement ont été effectués afin d'évaluer le comportement dans un milieu lubrifié comportant un modificateur de frottement MoDTC, d'un revêtement DLC et d'un revêtement de nitrure de chrome, en rappelant, de manière parfaitement connue, que dans le cas d'un revêtement DLC, afin de renforcer sa résistance mécanique, on peut desposer une sous-couche, par exemple, de nitrure de chrome. On renvoie au tableau ci-après qui montre les tests effectués sur quatre revêtements, à savoir, DCX- 0, DCX-1 , DCX-2, DCX-3, le revêtement DCX-3 étant conforme à l'invention. Friction tests were performed to evaluate the behavior in a lubricated medium comprising a MoDTC friction modifier, a DLC coating and a chromium nitride coating, recalling, in a well-known manner, that in the In the case of a DLC coating, in order to reinforce its mechanical strength, it is possible to deposit an underlayer, for example, of chromium nitride. Reference is made to the table below which shows the tests carried out on four coatings, namely, DCX- 0, DCX-1, DCX-2, DCX-3, the DCX-3 coating being in accordance with the invention.
L'ensemble des couches comporte un revêtement de nitrure de chrome élaboré par pulvérisation cathodique réactive magnétron. Pour l'ensemble des revêtements, on procède dans un premier temps au nettoyage des éprouvettes en acier qui sont ensuite positionnées sur des supports placés dans l'enceinte de dépôt sous vide. Pendant le pompage et l'évacuation de l'enceinte, on procède à un chauffage de l'intérieur de la machine et des pièces à revêtir, à une température de 150°C pendant 2h, dans le but de dégazer les pièces et la machine de dépôt. Ensuite, les pièces sont soumises à un décapage ionique dans une atmosphère d'argon, dont le but est d'éliminer les couches minces d'oxyde naturel et ainsi de permettre une forte adhérence du revêtement. Le dépôt de nitrure de chrome est obtenu par pulvérisation cathodique magnétron réactive d'une cible de Cr dans un mélange argon/azote. Le débit d'azote est asservi à une mesure optique de l'émission du Cr dans le plasma, de sorte que le dépôt contient 40+/-5 % atomique d'azote. Ainsi, on obtient un dépôt de CrN présentant une cristallisation cfc type NaCl, dont la microdureté est de 1800+/-200 Hv. Pour les revêtements DCX-0, DCX-1 et DCX-2, on dépose un revêtement de DLC type a-C:H par technique PACVD, en craquant un hydrocarbure dans un plasma, ici, de l'acétylène. Dans le cas de DCX-1 , on procède au dépôt final d'une couche de type a-C par pulvérisation cathodique magnétron d'une cible de graphite. Dans le cas de DCX-2, on génère un plasma d'oxygène pur et on bombarde le dépôt par des ions issus du plasma pendant lOminutes, ce qui permet de modifier la chimie de surface du dépôt. The set of layers comprises a coating of chromium nitride produced by magnetron reactive sputtering. For all the coatings, the steel specimens are first cleaned, which are then positioned on supports placed in the vacuum deposition chamber. During the pumping and evacuation of the enclosure, the inside of the machine and the parts to be coated are heated at a temperature of 150 ° C for 2 hours in order to degas the parts and the machine deposit. Then, the pieces are subjected to an ionic etching in an argon atmosphere, the purpose of which is to remove the thin layers of natural oxide and thus allow a strong adhesion of the coating. The deposition of chromium nitride is obtained by reactive magnetron sputtering of a Cr target in an argon / nitrogen mixture. The nitrogen flow rate is slaved to an optical measurement of the emission of Cr in the plasma, so that the deposit contains 40 +/- 5 atomic% of nitrogen. Thus, a deposit of CrN exhibiting cfc crystallization of the NaCl type, the microhardness of which is 1800 +/- 200 Hv, is obtained. For coatings DCX-0, DCX-1 and DCX-2, a coating of DLC type aC: H by PACVD technique is deposited by cracking a hydrocarbon in a plasma, here acetylene. In the case of DCX-1, the final deposition of an aC-type layer by magnetron sputtering of a graphite target. In the case of DCX-2, a pure oxygen plasma is generated and the deposit is bombarded by ions from the plasma for 10 minutes, which makes it possible to modify the surface chemistry of the deposit.
Ces essais ont été réalisés avec un tribomètre alternatif en configuration bille sur plan. Pour ces essais, le plan est constitué d'une éprouvette en acier, polie à un niveau de Ra de 0,02 μηι. La bille est en acier These tests were carried out with an alternative tribometer in ball-plane configuration. For these tests, the plane consists of a steel specimen, polished to a Ra level of 0.02 μηι. The ball is made of steel
100Cr6 et a un diamètre de 10 mm. Pour tous les essais, les revêtements sont appliqués sur la bille. 100Cr6 and has a diameter of 10 mm. For all the tests, the coatings are applied on the ball.
La charge appliquée sur la bille est de 10N, ce qui donne un diamètre The load applied on the ball is 10N, which gives a diameter
Hertzien de contact de 140 μηι et une pression moyenne de 0,68 GPa. 140 Hz contact air and a mean pressure of 0.68 GPa.
La bille est animée d'un mouvement alternatif, dont la course est de The ball is animated by an alternating movement, whose race is
10 mm. La vitesse de glissement suit un profil de type sinus, dont la valeur moyenne est de 3,5 cm/s. 10 mm. The sliding speed follows a sinus-like profile, whose average value is 3.5 cm / s.
Le test est conduit pendant une durée de 15 000 cycles à une température de 1 10°C. Les conditions de vitesse de glissement, de pression et de température, sont telles que l'additifs de réduction de frottement réagit pour remplir sont rôle. A l'issue du test, on observe la bille et on mesure le diamètre de la trace de frottement ou trace d'usure, à partir duquel, on calcule le volume usé. Le graphique annexé (figure 1) résume les vitesses d'usure moyenne (volume usé ramené au nombre de cycles de frottement). Pour chaque revêtement, 3 essais ont été effectués, l'usure moyenne a été calculée. Les barres d'erreur représentent, non pas une erreur, mais la valeur la plus petite et la valeur la plus grande pour ces 3 essais.  The test is conducted for a period of 15,000 cycles at a temperature of 110.degree. The sliding speed, pressure and temperature conditions are such that the friction reducing additive reacts to fulfill its role. At the end of the test, we observe the ball and measure the diameter of the trace of friction or trace of wear, from which, we calculate the used volume. The attached graph (Figure 1) summarizes the average wear rates (used volume based on the number of cycles of friction). For each coating, 3 tests were carried out, the average wear was calculated. The error bars represent, not an error, but the smallest value and the largest value for these 3 tests.
Pour chacun des essais et pour les différents revêtements, les mesures ont été effectuées en présence d'une huile automobile du commerce contenant le modificateur de frottement MoDTC.  For each of the tests and for the various coatings, the measurements were performed in the presence of a commercial automotive oil containing the MoDTC friction modifier.
Il ressort de ce graphique les observations suivantes : - Pour le revêtement DCX-0, l'usure est particulièrement importante, ce qui n'est, du reste, pas le cas pour le même type de revêtement en milieu lubrifié ne comportant pas de modificateur de frottement MoDTC. This graph shows the following observations: - For the DCX-0 coating, wear is particularly important, which is not the case for the same type of coating in a lubricated medium that does not include a MoDTC friction modifier.
- Pour le revêtement DCX-1 , l'ajout d'une couche carbone amorphe non-hydrogéné par-dessus le DLC, tend à réduire la vitesse d'usure d'un facteur d'environ 2,9.  - For the DCX-1 coating, the addition of a non-hydrogenated amorphous carbon layer over the DLC tends to reduce the wear rate by a factor of about 2.9.
- Pour le revêtement DCX-2, on voit que la modification de la surface DLC par un plasma d'oxygène, n'a pas d'influence significative sur la vitesse d'usure du DLC, alors que l'énergie de surface est complètement modifiée.  - For the DCX-2 coating, it can be seen that the modification of the DLC surface by an oxygen plasma has no significant influence on the wear rate of the DLC, whereas the surface energy is completely changed.
- Le revêtement DCX-3, conforme à l'invention, présente une usure nulle en fm d'essai, le diamètre de frottement est très légèrement supérieur au diamètre initial de contact. Le nitrure de chrome présente une dureté de l'ordre de 1800 Hv.  - The DCX-3 coating according to the invention has zero wear in test fm, the friction diameter is very slightly greater than the initial contact diameter. Chromium nitride has a hardness of the order of 1800 Hv.
Le tableau ci-dessous résume les valeurs de vitesse d'usure moyenne qui apparaissent sur le graphe annexé.  The table below summarizes the average wear speed values that appear on the appended graph.
Le tableau ci-dessous donne les coefficients de frottement en fm d'essai. The table below gives the coefficients of friction in test fm.
Il ressort de ces tableaux, que toutes les solutions comportant un revêtement présentent des coefficients de frottement moyens similaires. It can be seen from these tables that all solutions with a coating have similar average coefficients of friction.
La forte dispersion dans le cas du DCX-0 est liée à l'usure. On note que les coefficients de frottement les plus bas sont obtenus pour les dépôts les plus usés. The high dispersion in the case of DCX-0 is related to wear. It is noted that the lowest coefficients of friction are obtained for the most used deposits.
Le faible coefficient de frottement est essentiellement dû à l'additif de réduction de frottement : le MoDTC. The low coefficient of friction is mainly due to the friction reduction additive: the MoDTC.
A titre d'exemple et comme le montre la dernière ligne des tableaux, le test d'une bille non revêtue face à un plan non revêtu donne un coefficient de frottement de 0,040+/-0,005. La vitesse d'usure moyenne est de 0,45. Bien que cette solution résiste aussi à l'usure, grâce aux additifs anti-usure de l'huile, elle donne toutefois un coefficient de frottement plus élevé de 30 %. By way of example and as shown in the last row of the tables, the test of an uncoated ball facing an uncoated plane gives a coefficient of friction of 0.040 +/- 0.005. The average wear speed is 0.45. Although this solution is also resistant to wear, thanks to the anti-wear additives of the oil, it gives however a coefficient of friction higher than 30%.
A titre de comparaison, le frottement d'une bille revêtue DLC (DCX- 0) face à un plan, acier en utilisant une huile SAE 5W30 (sans aucun modificateur de frottement), donne une vitesse d'usure de 0,3+/-0,05 μηι3/ cycle, par contre le coefficient de frottement se stabilise à 0,12. Dans une huile SAE 5W30 comportant un additif de réduction de frottement de type acide gras, la vitesse d'usure est de 0,32+/-0,05 μηι3/ cycle et le coefficient de frottement est de 0,08. For comparison, the friction of a DLC-coated ball (DCX-0) facing a plane, steel using SAE 5W30 oil (without any friction modifier), gives a wear rate of 0.3 +. -0.05 μηι 3 / cycle, against the coefficient of friction is stabilized at 0.12. In a SAE 5W30 oil comprising a fatty acid type friction reducing additive, the wear rate is 0.32 +/- 0.05 μηι 3 / cycle and the coefficient of friction is 0.08.
Il ressort de ce qui précède, que les revêtements de DLC de type DCX-0 résistent bien à l'usure dans des huiles sans MoDTC en observant que ces huiles ne permettent pas d'obtenir des coefficients de frottement aussi bas que celles contenant du MoDTC. It follows from the foregoing that DLC coatings of DCX-0 type are resistant to wear in oils without MoDTC by observing that these oils do not make it possible to obtain coefficients of friction as low as those containing MoDTC. .
Autrement dit, la combinaison DLC face à un antagoniste de frottement en acier, MoDTC n'est pas compatible pour réaliser les deux fonctions, à savoir, résister à l'usure d'une part, et obtenir un coefficient de frottement aussi bas que possible d'autre part, alors que la combinaison revendiquée, à savoir, nitrure de chrome et MoDTC permet avantageusement de réaliser ces deux fonctions. In other words, the combination DLC facing a steel friction antagonist, MoDTC is not compatible to perform both functions, namely, resist wear on the one hand, and get a coefficient of friction as low as possible on the other hand, while the combination claimed, namely, chromium nitride and MoDTC advantageously allows these two functions to be performed.
L'invention concerne également l'utilisation de pièces ainsi revêtues et travaillant dans un milieu lubrifié contenant du MoDTC dans le domaine de l'automobile, notamment pour les moteurs et les boîtes de vitesses.  The invention also relates to the use of parts thus coated and working in a lubricated medium containing MoDTC in the automotive field, in particular for engines and gearboxes.

Claims

R E V E N D I C A T I O N S R E V E N D I C A T IO N S
-1- Pièce de frottement fonctionnant en milieu lubrifié comportant un modificateur de frottement, un revêtement étant appliqué sur ladite pièce caractérisé en ce que le revêtement est du nitrure de chrome et le modificateur de frottement, du MoDTC, le nitrure de chrome étant sélectionné pour présenter une cristallisation type NaCl dont la microdureté est de 1800 +/- 200 HV -1- friction piece operating in a lubricated medium comprising a friction modifier, a coating being applied to said part characterized in that the coating is chromium nitride and the friction modifier, MoDTC, chromium nitride being selected for have a NaCl crystallization with a microhardness of 1800 +/- 200 HV
-2- Utilisation de la pièce de frottement selon la revendication 1 dans le domaine est l'automobile. -2- Use of the friction piece according to claim 1 in the field is the automobile.
-3- Utilisation selon la revendication 2 dans le domaine des moteurs. -3- Use according to claim 2 in the field of motors.
-4- Utilisation selon la revendication 2 dans le domaine des boîtes de vitesses. Use according to claim 2 in the field of gearboxes.
EP12780220.5A 2011-10-21 2012-10-03 System comprising two friction members and a lubricating medium Active EP2768932B8 (en)

Applications Claiming Priority (2)

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FR1159546A FR2981728B1 (en) 2011-10-21 2011-10-21 FRICTION PIECE OPERATING IN A LUBRICATED ENVIRONMENT
PCT/FR2012/052236 WO2013057407A1 (en) 2011-10-21 2012-10-03 Friction piece operating in a lubricated medium

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FR2981728A1 (en) 2013-04-26
AU2012324719A1 (en) 2014-05-01
JP2021063296A (en) 2021-04-22
AU2012324719B2 (en) 2017-07-20
JP2014532841A (en) 2014-12-08
CA2851036A1 (en) 2013-04-25
KR101980309B1 (en) 2019-05-20
TW201341521A (en) 2013-10-16
WO2013057407A1 (en) 2013-04-25
BR112014008486A2 (en) 2017-04-25
JP2017040373A (en) 2017-02-23
MX356600B (en) 2018-06-06
JP7042760B2 (en) 2022-03-28
KR20140093214A (en) 2014-07-25
EP2768932B8 (en) 2022-02-16
CA2851036C (en) 2019-03-05
CN103917630B (en) 2017-02-15
BR112014008486B1 (en) 2019-10-29
RU2608612C2 (en) 2017-01-23
EP2768932B1 (en) 2022-01-12
RU2014119581A (en) 2015-11-20
ZA201402408B (en) 2015-03-25
IN2014KN00811A (en) 2015-10-02
JP7442427B2 (en) 2024-03-04
FR2981728B1 (en) 2014-07-04
US9284509B2 (en) 2016-03-15
TWI570233B (en) 2017-02-11
MX2014004750A (en) 2015-01-16
CN103917630A (en) 2014-07-09
JP2019060499A (en) 2019-04-18
US20140274826A1 (en) 2014-09-18

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