WO2021153425A1 - ピストンリング及びその製造方法 - Google Patents

ピストンリング及びその製造方法 Download PDF

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Publication number
WO2021153425A1
WO2021153425A1 PCT/JP2021/002102 JP2021002102W WO2021153425A1 WO 2021153425 A1 WO2021153425 A1 WO 2021153425A1 JP 2021002102 W JP2021002102 W JP 2021002102W WO 2021153425 A1 WO2021153425 A1 WO 2021153425A1
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WIPO (PCT)
Prior art keywords
film
piston ring
range
base material
amount
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Ceased
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PCT/JP2021/002102
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English (en)
French (fr)
Japanese (ja)
Inventor
弘樹 斉藤
啓二 本多
祐司 島
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Riken Corp
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Riken Corp
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Application filed by Riken Corp filed Critical Riken Corp
Priority to CN202180009792.7A priority Critical patent/CN115003936B/zh
Priority to US17/793,654 priority patent/US12188564B2/en
Priority to EP21747026.9A priority patent/EP4080033A4/en
Priority to JP2021523533A priority patent/JP7085692B2/ja
Publication of WO2021153425A1 publication Critical patent/WO2021153425A1/ja
Priority to JP2022047479A priority patent/JP2022087131A/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • F16J—PISTONS; CYLINDERS; SEALINGS
    • F16J9/00—Piston-rings, e.g. non-metallic piston-rings, seats therefor; Ring sealings of similar construction
    • F16J9/26—Piston-rings, e.g. non-metallic piston-rings, seats therefor; Ring sealings of similar construction characterised by the use of particular materials
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02F—CYLINDERS, PISTONS OR CASINGS, FOR COMBUSTION ENGINES; ARRANGEMENTS OF SEALINGS IN COMBUSTION ENGINES
    • F02F5/00—Piston rings, e.g. associated with piston crown

Definitions

  • This disclosure relates to a piston ring and a method for manufacturing the piston ring.
  • Piston rings are used in the engines of automobiles, etc.
  • the piston ring is mounted in a groove provided on the outer peripheral surface of the piston.
  • the piston ring is required to contribute to high performance of the engine and reduction of fuel consumption due to, for example, wear resistance and seizure resistance characteristics. Conventionally, various efforts have been made to improve the wear resistance of the piston ring.
  • Patent Document 1 the invention described in Patent Document 1 is intended to provide a sliding member having excellent wear resistance even under harsh conditions in an engine to which direct fuel injection or exhaust gas recirculation (EGR) is applied.
  • the base material of this sliding member is coated with a film having a mixed structure of a crystalline phase and an amorphous phase made of a metal nitride or a metal carbide or a metal carbonitride.
  • Patent Document 2 The invention described in Patent Document 2 is intended to provide a piston ring for an internal combustion engine having both wear resistance, crack resistance and peel resistance.
  • This piston ring contains Cr, N and Si as constituent elements, has the same crystal structure as CrN, and is solid-solved in the crystal lattice at a Si atomic ratio of 1% or more and 9.5% or less.
  • a hard film composed of the above-mentioned crystal phases is formed at least on the outer peripheral sliding surface.
  • Patent Documents 1 and 2 both disclose that a film is formed by an ion plating method.
  • a CrN-based film, a TiN-based film, or a laminated film thereof obtained by the ion plating method improves the wear resistance and peeling resistance of the piston ring.
  • the usage environment of the piston ring will become more severe in the future, there is still room for improvement in wear resistance and peeling resistance of these films.
  • Cr-Si-N-based film has fine crystal grains due to the addition of Si, and as a result, it is dense and has a large hardness. It was known to have a hardness.
  • the development policy at that time was to improve the wear resistance of the film by increasing the hardness.
  • cracks generated in the film could not be sufficiently suppressed, and there is a history that it has not been put into practical use.
  • the present disclosure provides a piston ring provided with a film containing Si and N, which has a sufficiently high level of peel resistance, crack resistance, and wear resistance, and a method for manufacturing the piston ring.
  • the conventional Cr—Si—N coating has a large hardness, but has a problem that cracks are likely to occur in the coating. Cracks in the film cause peeling. Since the piston ring is exposed to continuous sliding and repetitive loads, it has been considered difficult to apply the conventional Cr—Si—N coating to the piston ring.
  • the present inventors have set the conditions of the physical vapor deposition method in which a film capable of achieving all of peel resistance, crack resistance and wear resistance at a sufficiently high level is formed. It has been identified and the following invention has been completed.
  • the method for manufacturing a piston ring includes (A) a step of cleaning the surface of the base material of the piston ring, and (B) Si and N so as to cover at least a part of the surface of the base material in the chamber.
  • the pressure in the chamber is set in the range of 2 to 6 Pa so that a film satisfying the following conditions is formed, including the step of forming a film containing Set the bias voltage in the range of 5 to -18V.
  • ⁇ Film conditions> The amount of Si is in the range of 1.1 to 7.5 at%.
  • -The crystallite size is in the range of 10 to 30 nm.
  • -The residual stress of compression is 400 to 800 MPa.
  • the pressure condition (2 to 6 Pa) in the chamber allows a higher pressure than the conventional Cr—Si—N film forming condition, and the bias voltage condition (-5 to -18V).
  • the absolute value (5 to 18) of is smaller than the film forming conditions of the conventional Cr—Si—N-based film.
  • the piston ring according to the present disclosure is provided so as to cover at least a part of the surface of the base material and the base material, and includes a film containing Si and N, and the film satisfies the following conditions.
  • ⁇ Film conditions> The amount of Si is in the range of 1.1 to 7.5 at%.
  • -The crystallite size is in the range of 10 to 30 nm.
  • -The residual stress of compression is 400 to 800 MPa.
  • the piston ring can enjoy the merit of adding Si that the hardness is increased when the Si amount of the film is 1.1 at% or more, while the crack in the film is 7.5 at% or less. Occurrence can be suppressed.
  • the hardness of the film is preferably 1000 HV0.1 to 1800 HV0.1. Although this hardness is softer than that of the conventional Cr—Si—N film, it is sufficiently hard as a film for a piston ring.
  • the ratio H / E of the film hardness H (GPa) measured by the nanoindenter to the Young's modulus E (GPa) of the film is preferably 0.04 to 0.07. When the ratio H / E is within the above range, the film can be appropriately elastically deformed, thereby reducing the Hertz stress caused by sliding and achieving excellent peel resistance.
  • Me is, for example, Cr. That is, when the film containing Si and N further contains Cr, the amount of Cr is preferably 40 at% or more from the viewpoint of suppressing the generation of cracks in the film. Further, from the viewpoint of suppressing peeling of the film due to cracks and their bonds, the crystal orientation of the film preferably has a structure coefficient of CrN (111) of 0.4 or more.
  • a piston ring provided with a film containing Si and N, which has sufficiently high levels of peel resistance, crack resistance and wear resistance, and a method for manufacturing the piston ring. NS.
  • FIG. 1 is a cross-sectional view schematically showing an embodiment of the piston ring of the present disclosure.
  • FIG. 2 is a schematic view showing the configuration of a slip fatigue tester.
  • FIG. 1 is a cross-sectional view schematically showing a piston ring according to the present embodiment.
  • the piston ring 10 shown in FIG. 1 is a pressure ring for an internal combustion engine (for example, an automobile engine).
  • the pressure ring is mounted, for example, in a ring groove formed on the side surface of the piston.
  • the pressure ring is a ring that is exposed to an environment where the heat load of the engine is particularly high.
  • the piston ring 10 is annular, for example, having an outer diameter of 40 to 300 mm.
  • the "ring” here does not necessarily mean a closed circle, and the piston ring 10 may have a joint portion. Further, the piston ring 10 may have a perfect circular shape or an elliptical shape in a plan view.
  • the piston ring 10 is substantially rectangular in the cross section shown in FIG. 1, and the sliding surface 10F may be rounded so as to bulge outward.
  • the piston ring 10 includes a base material 1 and a film 5 provided on the outer peripheral surface (surface corresponding to the sliding surface 10F) of the base material 1.
  • the base material 1 is made of a heat-resistant alloy. Specific examples of the alloy include spring steel and martensitic stainless steel.
  • the base material 1 may have a nitride layer formed on its surface.
  • the film 5 constitutes the sliding surface 10F.
  • the film 5 is made of a Me—Si—N-based material (Me indicates a metal element).
  • the thickness of the film 5 is, for example, 5 to 70 ⁇ m, preferably 10 to 50 ⁇ m. When the thickness of the film 5 is 5 ⁇ m or more, the durability of the piston ring 10 tends to be high, while when the thickness is 70 ⁇ m or less, high productivity of the film 5 can be ensured.
  • the metal element Me is, for example, Cr, Ti, Al, Zr, Nb, or the like.
  • the amount of Me in the Me—Si—N-based material is preferably 40 at% or more, more preferably 40 to 55 at%, and further preferably 45 to 52 at%. When the amount of Me in the Me—Si—N material is 40 at% or more, the characteristics of the metal element Me are sufficiently reflected in the film 5.
  • the Me—Si—N-based material may contain one kind of metal element, or may contain two or more kinds of metal elements. Of the above metal elements, Cr is preferable in that the atomic radius is close to that of Si that is dissolved in solid solution.
  • the amount of Si in the film 5 is 1.1 to 7.5 at%, preferably 1.5 to 7.0 at%, and more preferably 2.0 to 5.0 at%.
  • the film 5 having a Si content of 1.1 at% or more is composed of finely divided crystal grains and has excellent hardness.
  • an appropriate amount of amorphous phase is likely to be formed in the film 5. It is presumed that this amorphous phase contributes to the suppression of cracks.
  • the amount of Si in the film 5 can be adjusted by the amount of Si in the target used when the film 5 is formed by the physical vapor deposition method (PVD method).
  • the crystallite size of the film 5 is 10 to 30 nm, preferably 15 to 25 nm. When the crystallite size is 30 nm or less, even if the film 5 is worn, the unit of wear at one time becomes small and the wear resistance is improved.
  • the residual stress of compression of the film 5 is 400 to 800 MPa.
  • the stress difference from the base material 1 alloy or nitrided layer
  • the stress difference from the base material 1 can be reduced, thereby peeling at the interface between the base material 1 and the film 5.
  • cracks in the film 5 that are likely to occur due to the addition of Si can be suppressed.
  • the structure coefficient of each crystal plane satisfies the following conditions. By balancing the orientation of the crystals of the film 5, crack growth is inhibited, and peeling of the film 5 due to crack bonding can be effectively prevented.
  • the hardness of the film 5 is preferably 1000 HV0.1 to 1800 HV0.1, and more preferably 1100 HV0.1 to 1500 HV0.1.
  • the ratio H / E of the hardness H (GPa) of the film 5 and the Young's modulus E (GPa) of the film 5 obtained by the nanoindenter is preferably 0.04 to 0.07, and more preferably 0. It is 05 to 0.06.
  • the ratio H / E is within the above range, the film 5 can be appropriately elastically deformed, thereby reducing the Hertz stress caused by sliding and achieving excellent peel resistance.
  • the manufacturing method of this embodiment includes the following steps.
  • the step (a) is a step for cleaning the surface of the base material 1 prior to the formation of the film 5.
  • a cleaning treatment such as degreasing or shot blasting may be performed.
  • bombard cleaning may be performed in the chamber.
  • the formation of the film 5 in the step (b) can be carried out by a physical vapor deposition method.
  • the formation of the film 5 is carried out after the inside of the chamber is made into a nitrogen atmosphere.
  • Examples of the physical vapor deposition method include an ion plating method and a sputtering method. All of these physical vapor deposition methods are carried out in a vacuum chamber, and the nitrogen pressure in the vacuum chamber is set in the range of 2 to 6 Pa. Also, the bias voltage is set in the range of -5 to -18V.
  • the amount of Si in the film 5 can be adjusted by changing the amount of Si in the target.
  • the amount of Si in the film 5 may be adjusted by supplying a Si-containing gas into the chamber.
  • the hardness of the film 5 can be adjusted, and the crystal orientation and crystallite size can be adjusted by adjusting the amount of Si in the film 5.
  • These physical properties can also be adjusted by the temperature at which the film 5 is formed (deposition temperature).
  • the film formation temperature may be, for example, 550 ° C. or lower.
  • the residual stress and hardness of the film 5 may be adjusted by adjusting the nitrogen pressure and the bias voltage in the chamber.
  • ⁇ Set the nitrogen pressure in the chamber to a high level.
  • the pressure is, for example, 4.0 to 6.0 Pa.
  • the bias voltage is, for example, -5 to -10V.
  • a ring having the following composition was prepared as a base material for the piston ring.
  • ⁇ Fe 80.4% by mass
  • ⁇ C 0.85% by mass -Cr: 17.0% by mass
  • ⁇ Si 0.5% by mass -Mn: 0.5% by mass
  • Other elements Remaining
  • Piston rings according to Examples and Comparative Examples were produced as follows. That is, first, the base material was degreased and washed, and then installed in the chamber. The substrate was then bombard-cleaned in the chamber. Then, a film (thickness: about 20 ⁇ m) was formed on the surface of the substrate by the ion plating method under the conditions shown in Tables 1 and 2. The film formation temperature was 500 ° C. The arc current was 150 A.
  • Tables 1 and 2 show the characteristics of the piston ring coatings according to Examples and Comparative Examples. Each characteristic was measured by the following method.
  • Si amount The amount of Si in the film was measured using EPMA (device name: JXA-8100, manufactured by JEOL Ltd.), and the measurement conditions were an acceleration voltage of 15 kV, an irradiation current of 5.0 ⁇ 10-8 A, and a beam diameter of 10 ⁇ m. From the X-ray diffraction data, it was determined that Si in the films of Examples and Comparative Examples (excluding Comparative Example 4) was solid-solved.
  • I (hkl) is the X-ray diffraction intensity of the measured (hkl) plane
  • I 0 (hkl) is the standard X-ray diffraction intensity described in the JCPDS file.
  • the negative notation in Tables 1 and 2 means that it is the residual stress of compression.
  • Hardness The hardness of the film was obtained by performing a hardness test with a test load of 0.98 N based on the method specified in ISO6507 using a Vickers hardness tester (device name: HM-220, manufactured by Mitutoyo). ..
  • the hardness H of the film and the Young's modulus E of the film obtained by the nanoindenter were determined using an ultrafine indentation hardness tester (device name: ENT-1100a, manufactured by Elionix). That is, based on the test method specified in ISO14577, a hardness test was carried out using a diamond indenter having a regular triangular pyramid (Berkovich type) tip shape with a test load of 0.4 N, and the load applied to the indenter and the displacement of the indenter during the test. It was obtained from the "load-displacement curve" obtained from.
  • an ultrafine indentation hardness tester device name: ENT-1100a, manufactured by Elionix
  • ⁇ Slip fatigue test> As a wear acceleration test, a slip fatigue test was performed using a testing machine having the configuration shown in FIG.
  • the testing machine 50 shown in FIG. 2 includes a rotating drum 51, a mechanism for bringing a test piece S (piston ring cutting piece) into contact with the surface of the drum 51, and a mechanism for repeatedly applying a load to the test piece S. , A mechanism for supplying lubricating oil to the sliding portion is provided. As a result, the test piece can be worn in a relatively short time.
  • the test conditions were as follows.
  • Test load 20-50N, sine curve (50Hz) -Mating material (drum): SUJ2 heat-treated material (diameter 80 mm) ⁇ Dynamic speed: Forward / reverse reverse trapezoidal pattern operation ⁇ Lubricating oil: Base oil (once every 30 seconds, 0.1 cc dropped) ⁇ Drum surface temperature: 80 ° C ⁇ Test time: 1 cycle 2 to 3 minutes for 5 cycles
  • Abrasion resistance Abrasion amount when the wear amount of the conventional CrN film is 1.0
  • a piston ring provided with a film containing Si and N, which has sufficiently high levels of peel resistance, crack resistance and wear resistance, and a method for manufacturing the piston ring. NS.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Pistons, Piston Rings, And Cylinders (AREA)
  • Physical Vapour Deposition (AREA)
PCT/JP2021/002102 2020-01-27 2021-01-21 ピストンリング及びその製造方法 Ceased WO2021153425A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CN202180009792.7A CN115003936B (zh) 2020-01-27 2021-01-21 活塞环及其制造方法
US17/793,654 US12188564B2 (en) 2020-01-27 2021-01-21 Piston ring, and method for manufacturing same
EP21747026.9A EP4080033A4 (en) 2020-01-27 2021-01-21 PISTON RING AND METHOD FOR PRODUCING THEREOF
JP2021523533A JP7085692B2 (ja) 2020-01-27 2021-01-21 ピストンリング及びその製造方法
JP2022047479A JP2022087131A (ja) 2020-01-27 2022-03-23 ピストンリング及びその製造方法

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JP2020010754 2020-01-27
JP2020-010754 2020-01-27

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EP (1) EP4080033A4 (https=)
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WO (1) WO2021153425A1 (https=)

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WO2025074480A1 (ja) * 2023-10-02 2025-04-10 株式会社リケン 摺動部材およびピストンリング
KR20260047558A (ko) * 2024-09-30 2026-04-08 가부시끼가이샤 리켄 슬라이딩 부재의 제조 방법, 슬라이딩 부재 및 피스톤 링

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