WO2023090275A1 - 固体潤滑材、摺動部材及び固体潤滑材の形成方法 - Google Patents

固体潤滑材、摺動部材及び固体潤滑材の形成方法 Download PDF

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WO2023090275A1
WO2023090275A1 PCT/JP2022/042155 JP2022042155W WO2023090275A1 WO 2023090275 A1 WO2023090275 A1 WO 2023090275A1 JP 2022042155 W JP2022042155 W JP 2022042155W WO 2023090275 A1 WO2023090275 A1 WO 2023090275A1
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Prior art keywords
plane
solid lubricant
planes
peak intensity
ray diffraction
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English (en)
French (fr)
Japanese (ja)
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一生 竹中
善秀 宮川
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Idemitsu Kosan Co Ltd
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Idemitsu Kosan Co Ltd
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Priority to JP2023561574A priority Critical patent/JPWO2023090275A1/ja
Priority to US18/707,724 priority patent/US20250197753A1/en
Priority to CN202280075858.7A priority patent/CN118251513A/zh
Priority to EP22895557.1A priority patent/EP4435139A4/en
Publication of WO2023090275A1 publication Critical patent/WO2023090275A1/ja
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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating 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
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • F16C33/10—Construction relative to lubrication
    • F16C33/1095—Construction relative to lubrication with solids as lubricant, e.g. dry coatings, powder
    • 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
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C10M2201/0623—Oxides; Hydroxides; Carbonates or bicarbonates used as base material
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/023—Multi-layer lubricant coatings
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/08—Solids
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/14—Composite materials or sliding materials in which lubricants are integrally molded
    • 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
    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • the present invention relates to a solid lubricant, a sliding member, and a method of forming a solid lubricant.
  • Patent Document 1 disclose zinc oxide coatings as solid lubricants.
  • the (100), (101), (102) and (104) planes are used more than the (002) and (103) planes while including the (002) and (103) planes.
  • a low-friction ZnO coating is disclosed that includes a minor proportion.
  • the friction coefficient of the solid lubricant is low. In addition to this, it is also required to improve the durability of solid lubricants. In particular, depending on the environment in which the solid lubricant is used, further durability of the solid lubricant may be desired.
  • a solid lubricant according to one aspect has a material having a hexagonal crystal structure.
  • the ratio of the surface other than the (002) surface to the (002) surface at the interface with the base material to be coated is (002) to the (002) surface on the surface of the solid lubricant higher than the proportion of non-facets.
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane at the interface with the base material of the solid lubricant is the surface of the solid lubricant is higher than the ratio of the X-ray diffraction peak intensity for planes other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane in .
  • a method for forming a solid lubricant according to one aspect relates to a method for forming a solid lubricant having a material having a hexagonal crystal structure.
  • the ratio of planes other than (002) planes to (002) planes at the interface with the substrate to be coated is higher than the ratio of planes other than (002) planes to (002) planes at the surface.
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane at the interface with the substrate is the X-ray diffraction for the (002) plane at the surface coating the substrate with zinc oxide such that the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the peak intensity of the substrate is higher than that of the X-ray diffraction peak intensity of the (002) plane.
  • a sliding member according to one aspect has the above-described solid lubricant.
  • FIG. 1 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the first embodiment.
  • FIG. 2 is a graph showing the results of X-ray diffraction near the interface with the substrate for zinc oxide coatings as various solid lubricants.
  • FIG. 3 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the second embodiment.
  • FIG. 4 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the third embodiment.
  • FIG. 5 is a graph showing the results of surface-side X-ray diffraction tests for various zinc oxide coatings.
  • FIG. 1 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the first embodiment.
  • FIG. 2 is a graph showing the results of X-ray dif
  • FIG. 6 is a view showing laser microscope photographs of the surface of the base material in Example 2 and Reference Example 1 after the reciprocating friction test.
  • FIG. 7 is a graph showing the measurement results of the coefficient of friction of the surfaces of the substrates in Examples 1 and 2 and Reference Example 1 during the reciprocating friction test.
  • FIG. 1 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the first embodiment.
  • the structure may have a base material 200, a solid lubricant 100, and a lubricant 300.
  • solid lubricant 100 is provided on substrate 200 .
  • the substrate 200 is the material on which the solid lubricant is to be provided.
  • the material forming the base material 200 is not particularly limited, and may be a metal member such as a steel plate, for example.
  • lubricant 300 resides on a solid lubricant. Alternatively, lubricant 300 may not be used.
  • Solid lubricant 100 includes a material having a hexagonal crystal structure.
  • solid lubricant 100 comprises a material selected from the group comprising ZnO, BeO, SiO2 , GeO2 , Al2O3 , WO3 , MoO3 and MoS2 .
  • the material having a hexagonal crystal structure is an oxide material.
  • oxide materials include ZnO, BeO , SiO2 , GeO2 , Al2O3 , WO3 , MoO3 and the like.
  • the material forming the solid lubricant 100 is zinc oxide (ZnO).
  • the solid lubricant 100 may have a foundation layer 110 on the base material 200 side and a surface layer 120 on the surface side.
  • the underlying layer 110 and the surface layer 120 may not be separated by a clear boundary.
  • the solid lubricant 100 can be formed by a film forming technique such as sputtering film forming.
  • the base layer 110 and the surface layer 120 of the solid lubricant 100 may be layers formed under different film forming conditions, for example.
  • the underlying layer 110 is located at the interface with the base material 200 .
  • the surface layer 120 faces away from the underlying layer 110 .
  • the crystal orientation of the underlayer 110 is different from the crystal orientation of the surface layer 120 .
  • the ratio of the surfaces other than the (002) surface to the (002) surface of the solid lubricant at the interface with the substrate to be coated is the (002) surface to the (002) surface of the solid lubricant surface. higher than the proportion of non-facets.
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane of the solid lubricant at the interface with the base material to be coated is It is higher than the ratio of the X-ray diffraction peak intensity of the plane other than the (002) plane to the X-ray diffraction peak intensity of the (002) plane on the surface.
  • the ratio of (100) planes and (101) planes to (002) planes of the solid lubricant at the interface with the substrate to be coated is higher than the ratio of (101) planes.
  • the ratio of the X-ray diffraction peak intensity for the (100) plane and (101) plane to the X-ray diffraction peak intensity for the (002) plane of the solid lubricant at the interface with the substrate to be coated is the solid lubricant It is higher than the ratio of the X-ray diffraction peak intensity for the (100) and (101) planes to the X-ray diffraction peak intensity for the (002) plane on the surface of the material.
  • the (002) plane of a material having a hexagonal crystal structure is the closest packed plane, and the (002) plane of the material is considered to be a low-friction plane. Therefore, when most of the interface between the base material and the solid lubricant corresponds to the (002) surface (low friction surface) of the solid lubricant, the solid lubricant is easily separated from the base material, and the durability of the solid lubricant is improved. is expected to decrease.
  • a relatively large number of surfaces other than the (002) surface of the solid lubricant are included in the interface between the base material and the solid lubricant. Therefore, it is considered that the solid lubricant is less likely to separate from the substrate, and the durability of the solid lubricant is improved. Considering this action, it is considered that the durability of the solid lubricant can be improved regardless of whether lubricating oil is present on the surface of the solid lubricant.
  • the surface of the solid lubricant has a relatively high percentage of (002) planes, the low friction properties of the solid lubricant can be maintained.
  • the ratio of the (002) plane in each layer of the solid lubricant and the X-ray diffraction peak intensity for the (002) plane can be changed by adjusting the film formation conditions during the film formation of the solid lubricant.
  • Fig. 2 is a table showing the results of an X-ray diffraction test for zinc oxide coating as a solid lubricant.
  • the upper line in the graph of FIG. 2 indicates that the zinc oxide coating was formed on the substrate by sputtering using a zinc oxide target material under the condition that the oxygen partial pressure was 20% relative to argon. is the result of
  • the lower line in the graph of FIG. 2 shows the film formed on the substrate by sputtering using a target material made of zinc oxide under the condition that the oxygen partial pressure is 0% relative to argon (the condition that does not contain oxygen). This is the result when a zinc oxide coating is formed on .
  • the ratio of This means that the ratio of (100) and (101) planes to (002) planes on the surface of the coating is high.
  • the ratio of the X-ray diffraction peak intensity for the (002) plane to the X-ray diffraction peak intensity for the other planes, and the ratio for the (002) plane You can adjust the proportions of other surfaces. Therefore, it is possible to realize the zinc oxide coating described above by appropriately adjusting the oxygen partial pressure during the sputtering of the underlying layer and the surface layer.
  • the ratio of the surface other than the (002) surface to the (002) surface at the interface with the base material to be coated is higher than the ratio of the surface other than the (002) surface to the (002) surface.
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane at the interface with the substrate to be coated is Coating the substrate with a solid lubricant such that the ratio of the X-ray diffraction peak intensity for the plane other than the (002) plane to the X-ray diffraction peak intensity for the plane other than the (002) plane is higher.
  • the ratio of (100) and (101) to (002) faces at the interface with the substrate to be coated is equal to (100) and (101) to (002) faces at the surface.
  • ratio of the X-ray diffraction peak intensity for the (100) and (101) planes to the X-ray diffraction peak intensity for the (002) plane at the interface with the substrate to be coated is higher than the fraction of the planes, or
  • the substrate is coated with a solid lubricant so that the ratio of the X-ray diffraction peak intensity for the (100) plane and the (101) plane to the X-ray diffraction peak intensity for the (002) plane on the surface is higher.
  • the solid lubricant 100 is formed to have at least the base layer 110 positioned at the interface with the base material 200 and the surface layer 120 facing away from the base layer.
  • the deposition conditions for forming the surface layer 120 may be different from the deposition conditions for forming the underlying layer 110 .
  • the solid lubricant may be coated by any film forming technique such as a sputtering film forming method.
  • the ratio of the other planes to the (002) plane in each layer of the solid lubricant and the ratio of the X-ray diffraction peak intensity for the (002) plane and the other planes are determined by the film formation conditions at the time of coating the solid lubricant. can be changed by adjusting the film formation conditions at the time of coating the solid lubricant.
  • the solid lubricant is coated by a sputtering deposition method.
  • the content of the different gas relative to the rare gas at the position near the interface with the base material during the sputtering film formation is changed from the content of the different gas relative to the rare gas at the position near the surface during the sputtering film formation.
  • the crystal orientation of the solid lubricant can be changed.
  • the content of oxygen relative to the rare gas at the position near the interface with the substrate during sputtering deposition is the same as the content of oxygen relative to the rare gas at the position near the surface during sputtering deposition. higher than the amount is preferred.
  • the ratio of the other planes to the (002) plane in each layer of the solid lubricant and the peak intensity of the X-ray diffraction of the (002) plane and the other planes ratio can be achieved. It is also possible to adjust these ratios by changing the oxygen content relative to the noble gas.
  • the target material is not particularly limited as long as it can form a solid lubricant.
  • the target material may be an oxide material containing molecules constituting the oxide material, or a material obtained by removing oxygen from the molecules constituting the oxide material.
  • the target material may be a material containing the same molecules as the oxide material that constitutes the solid lubricant.
  • the target material when the solid lubricant consists of zinc oxide, the target material may be zinc oxide or zinc, for example. From the viewpoint of reducing the oxygen content in the gas surrounding the target material, the target material is preferably zinc oxide.
  • the gas surrounding the target material may be a rare gas or a mixture of oxygen and rare gas.
  • the noble gas may be argon, for example.
  • FIG. 3 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the second embodiment.
  • the same reference numerals are assigned to the same configurations as in the first embodiment. It should be noted that descriptions of configurations similar to those of the first embodiment may be omitted.
  • the solid lubricant 100 may have a base layer 110, an intermediate layer 130, and a surface layer 120.
  • the underlying layer 110 is a layer that is in contact with the base material 200 .
  • the surface layer 120 is a surface that can slide on other members.
  • the intermediate layer 130 is located between the underlayer 110 and the surface layer 120 .
  • the base layer 110, the intermediate layer 130 and the surface layer 120 may be layers formed under different film forming conditions, for example.
  • the solid lubricant 100 may have multiple intermediate layers 130 between the base layer 110 and the surface layer 120 .
  • the plurality of intermediate layers 130 may be layers formed under different deposition conditions.
  • the underlying layer 110, the intermediate layer 130 and the surface layer 120 do not have to be separated by clear boundaries in the second embodiment as well.
  • the crystal orientation of the underlying layer 110 is different from the crystal orientation of the surface layer 120 .
  • the crystal orientation of intermediate layer 130 may be different from the crystal orientation of underlayer 110 and surface layer 120 , or may be the same as the crystal orientation of one of underlayer 110 and surface layer 120 .
  • the ratio of surfaces other than the (002) surface to the (002) surface of the solid lubricant at the interface (underlayer) with the base material to be coated is the surface of the solid lubricant It is higher than the ratio of planes other than the (002) plane to the (002) plane in the (surface layer).
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane of the solid lubricant at the interface with the base material to be coated is It is higher than the ratio of the X-ray diffraction peak intensity of the plane other than the (002) plane to the X-ray diffraction peak intensity of the (002) plane on the surface.
  • a highly durable solid lubricant can be expected.
  • FIG. 4 is a schematic diagram showing an example of the configuration of a solid lubricant and a structure using the solid lubricant according to the third embodiment.
  • the same reference numerals are assigned to the same configurations as in the first embodiment. It should be noted that descriptions of configurations similar to those of the first embodiment may be omitted.
  • the solid lubricant 100 is formed of layers without clear boundaries.
  • the crystal orientation of the material forming the solid lubricant gradually changes in the thickness direction.
  • the ratio of the surface other than the (002) surface to the (002) surface of the solid lubricant at the interface with the substrate to be coated is the (002) surface to the (002) surface of the solid lubricant surface. higher than the proportion of non-facets.
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane of the solid lubricant at the interface with the base material to be coated is It is higher than the ratio of the X-ray diffraction peak intensity of the plane other than the (002) plane to the X-ray diffraction peak intensity of the (002) plane on the surface.
  • the solid lubricant 100 according to the third embodiment can be formed by gradually changing the film forming conditions of the solid lubricant while laminating the solid lubricant.
  • the solid lubricant can be formed by gradually changing the content of oxygen relative to the noble gas during sputtering deposition while advancing the deposition of the solid lubricant.
  • the content of oxygen in the rare gas at the time of film formation by sputtering may be gradually reduced as the solid lubricant 100 is laminated.
  • Example 1 Next, a solid lubricant according to Example 1 will be described.
  • a zinc oxide coating is provided on the substrate as a solid lubricant.
  • a zinc oxide coating includes an underlayer and a surface layer, as shown in FIG.
  • the underlayer and surface layer of the zinc oxide coating were formed using "Inter-back type sputtering apparatus SIH-300 manufactured by ULVAC, Inc.”.
  • the target material was zinc oxide.
  • Example 1 the film formation gas during the film formation of the underlayer of the zinc oxide coating was a mixture of 80% argon partial pressure and 20% oxygen partial pressure (see Table 1).
  • the film forming gas for forming the surface layer is argon, and substantially does not contain oxygen.
  • the flow rate of film-forming gas was 50 ml/min.
  • the film formation temperature was 25° C. and the film formation pressure was 0.5 Pa.
  • the discharge power was 200 W when forming the underlayer, and the discharge power was 2000 W when forming the surface layer.
  • the film thickness of the underlayer was 40 nm, and the film thickness of the surface layer was 1700 nm. Note that the film thickness described above is a value measured by spectroscopic ellipsometry (the same applies hereinafter).
  • Example 2 A solid lubricant according to Example 2 will be described.
  • a zinc oxide coating is provided on the substrate as a solid lubricant.
  • the zinc oxide coating according to Example 2 was formed under the same conditions as in Example 1, except for the film thickness of the zinc oxide underlayer (see Table 1).
  • the film thickness of the underlayer was 80 nm, and the film thickness of the surface layer was 1700 nm.
  • Reference Example 1 A solid lubricant according to Reference Example 1 will be described.
  • a zinc oxide coating is provided on the substrate as a solid lubricant.
  • the zinc oxide coating according to Reference Example 1 was formed under the same conditions as in Example 1, except for the components of the film formation gas during the formation of the underlayer.
  • the film forming gas used in forming the underlayer and the surface layer was argon, and substantially did not contain oxygen (see Table 1).
  • the film thickness of the underlayer was 60 nm, and the film thickness of the surface layer was 1700 nm.
  • the oxygen partial pressure in the film formation gas during the formation of the underlayer is higher than the oxygen partial pressure in the film formation gas during the formation of the surface layer. Therefore, as explained in FIG. 2, the ratio of non-(002) planes to (002) planes of zinc oxide at the interface with the substrate to be coated is (002) planes to (002) planes at the zinc oxide surface. ) is higher than the proportion of faces other than the faces.
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane of zinc oxide at the interface with the substrate to be coated is It is higher than the ratio of the X-ray diffraction peak intensity for the planes other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane.
  • the ratio of the surface other than the (002) surface to the (002) surface of zinc oxide at the interface with the base material to be coated is considered to be substantially the same as the ratio of
  • the ratio of the X-ray diffraction peak intensity for a plane other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane of zinc oxide at the interface with the substrate to be coated is It is considered to be substantially the same as the ratio of the peak intensity of X-ray diffraction for planes other than the (002) plane to the peak intensity of X-ray diffraction for the plane (002).
  • FIG. 5 is a graph showing the results of surface-side X-ray diffraction tests for various zinc oxide coatings.
  • an X-ray diffraction test was performed by irradiating the surface side of the zinc oxide coatings according to Examples 1 and 2 and Reference Example 1 with X-rays.
  • the peak intensity of X-ray diffraction for the (002) plane of zinc oxide is high.
  • the zinc oxide surface layers were formed under the same film formation conditions. Therefore, the X-ray diffraction peak intensities in Examples 1 and 2 and Reference Example 1 are substantially the same.
  • the ratio of the X-ray diffraction peak intensity of the plane other than the (002) plane to the X-ray diffraction peak intensity of the (002) plane of zinc oxide at the interface with the substrate to be coated was , is higher than the ratio of the X-ray diffraction peak intensity for the planes other than the (002) plane to the X-ray diffraction peak intensity for the (002) plane on the zinc oxide surface.
  • the ratio of non-(002) to (002) faces at the interface with the substrate to be coated is higher than the ratio of non-(002) to (002) faces at the surface. do.
  • a reciprocating friction test was performed on the substrates having the zinc oxide coatings according to Example 2 and Reference Example 1.
  • a ball of steel (SUJ-2) having a diameter of 0.5 inches is reciprocated over the surface of the substrate provided with the zinc oxide coating.
  • the reciprocating friction test was conducted with machine oil applied on the zinc oxide coating.
  • the ball made of steel reciprocated on the base material while being pressed against the base material with a load of 3 kgf.
  • the temperature during the test was room temperature.
  • the ball made of steel had a stroke width of 20 mm and a stroke speed of 10 mm/s.
  • a steel ball was reciprocated on the substrate 200 having the zinc oxide coating.
  • FIG. 6 is a view showing laser micrographs of the surfaces of the substrates in Example 2 and Reference Example 1 after the reciprocating friction test. From FIG. 6, it can be seen that the zinc oxide coating in Example 2 was hardly peeled off even after the reciprocating friction test. In contrast, the zinc oxide coating according to Reference Example 1 was partially peeled off after the reciprocating friction test. From this result, it can be seen that the durability of the zinc oxide coating according to Example 2 is improved.
  • FIG. 7 is a graph showing the measurement results of the coefficient of friction of the surfaces of the substrates in Examples 1 and 2 and Reference Example 1 during the reciprocating friction test. From FIG. 7, it can be seen that in Examples 1 and 2, the coefficient of friction is stable even if the number of sliding times of the ball made of steel increases. On the other hand, in Reference Example 1, the coefficient of friction suddenly increases at the point of 20-odd times of sliding, and gradually increases after the number of sliding exceeds 70 times. Thus, the friction coefficients of the zinc oxide coatings according to Examples 1 and 2 maintain more stable values than the friction coefficient of the zinc oxide coating according to Reference Example 1.
  • Example 2 when comparing Example 1 and Example 2, it can be seen that the coefficient of friction of the zinc oxide coating maintains a lower value as the film thickness of the underlayer increases. In particular, the coefficient of friction of the zinc oxide coating according to Example 2 can stably maintain a low value.
  • the solid lubricant of the present invention can be suitably applied to sliding members having sliding surfaces.
  • the solid lubricant is provided on the sliding surface of the sliding member, and the sliding surface corresponds to the surface of the substrate 200 described above.
  • sliding members include bearings, seals, flywheels, scissors, plunger pumps, pistons, gears, crankshafts, artificial joints, and the like.

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PCT/JP2022/042155 2021-11-16 2022-11-11 固体潤滑材、摺動部材及び固体潤滑材の形成方法 Ceased WO2023090275A1 (ja)

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US18/707,724 US20250197753A1 (en) 2021-11-16 2022-11-11 Solid lubricant material, sliding member and method for forming solid lubricant material
CN202280075858.7A CN118251513A (zh) 2021-11-16 2022-11-11 固体润滑材料、滑动构件和固体润滑材料的形成方法
EP22895557.1A EP4435139A4 (en) 2021-11-16 2022-11-11 SOLID LUBRICANT, SLIDING ELEMENT AND METHOD FOR PRODUCING A SOLID LUBRICANT

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JPWO2023090275A1 (https=) 2023-05-25

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