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WO2009119269A1 - Procédé de production d'un composant à surface revêtue ayant une excellente adhérence à un film - Google Patents

Procédé de production d'un composant à surface revêtue ayant une excellente adhérence à un film Download PDF

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Publication number
WO2009119269A1
WO2009119269A1 PCT/JP2009/054075 JP2009054075W WO2009119269A1 WO 2009119269 A1 WO2009119269 A1 WO 2009119269A1 JP 2009054075 W JP2009054075 W JP 2009054075W WO 2009119269 A1 WO2009119269 A1 WO 2009119269A1
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WO
WIPO (PCT)
Prior art keywords
film
metal
carbon
base material
coated
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.)
Ceased
Application number
PCT/JP2009/054075
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English (en)
Japanese (ja)
Inventor
史明 本多
謙一 井上
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.)
Proterial Ltd
Original Assignee
Hitachi Metals Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hitachi Metals Ltd filed Critical Hitachi Metals Ltd
Priority to JP2010505491A priority Critical patent/JP5418917B2/ja
Publication of WO2009119269A1 publication Critical patent/WO2009119269A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • 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
    • C23C14/027—Graded interfaces
    • 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
    • C23C14/0605—Carbon
    • 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
    • F16J1/00—Pistons; Trunk pistons; Plungers
    • F16J1/02—Bearing surfaces
    • 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

Definitions

  • the present invention relates to a method for producing a surface-coated component having excellent film adhesion applied to sliding parts and molds.
  • diamond-like carbon which is excellent in sliding characteristics and wear resistance characteristics, is being used as a hard film to be surface-treated on sliding parts and molds from conventional CrN films and TiN films.
  • the film forming method can use a target material as an evaporation source and can obtain a film having a low surface roughness value. Therefore, there are many applications of a sputtering method that is easy to handle. And about this, in order to improve the adhesiveness of a membrane
  • the diamond-like carbon coated using the sputtering method has excellent sliding characteristics and wear resistance characteristics, and has improved adhesion by applying an argon gas bombardment process.
  • the present situation is that the adhesion is poor due to the high hardness. Therefore, it has been a big problem to provide adhesion equal to or better than that of a CrN film or a TiN film while having excellent film characteristics of diamond-like carbon.
  • the present invention has an object to provide a method for producing a surface-coated component that is superior to the present state in coating the hard physical vapor deposition film represented by diamond-like carbon, for example. To do.
  • the present invention has been studied in detail in order to produce a surface-coated component having better film adhesion than the present situation.
  • the physical vapor deposition film was coated, there were special and effective combination conditions for the bombarding treatment to the base material and the subsequent coating method of the intermediate film.
  • the adhesion of the hard coating is dramatically improved.
  • the present invention relates to a method of manufacturing a surface-coated component in which a surface of a base material is coated with a hard physical vapor deposition film, and the base material before the coating is subjected to metal ion bombardment treatment by an arc ion plating method.
  • a method for producing a surface-coated part excellent in film adhesion is characterized in that an intermediate metal film is coated by a sputtering method and then a physical vapor deposition film to be a surface layer is coated.
  • the physical vapor deposition film is preferably a hard film having a surface hardness of 1000 HV or more.
  • the sputtering method is preferably a non-equilibrium magnetron sputtering method, or further, the base material before the metal ion bombardment treatment is preferably subjected to an argon gas bombardment treatment.
  • a coating process by the sputtering method preferably non-equilibrium magnetron sputtering, is performed in a state where the base material after the process is maintained in the processing chamber. It is preferable to continuously perform the coating treatment by the method.
  • the metal subjected to the metal ion bombardment treatment is titanium, or that the intermediate metal film is titanium. It is more desirable to satisfy both of these requirements.
  • the physical vapor deposition film is a carbon film, and a mixed gradient of metal and carbon in which the metal content gradually decreases toward the carbon film side between the carbon film and the intermediate metal film. It is desirable to coat the film.
  • the carbon film is coated by a nonequilibrium magnetron sputtering method, or more preferably diamond-like carbon.
  • FIG. 2 is a transmission electron micrograph showing an example of the vicinity of the interface between the base material and the film in the present invention. It is the microscope picture which showed an example of the evaluation test result (state around Rockwell impression) of the film
  • the pretreatment for coating a hard physical vapor deposition film (hereinafter also simply referred to as physical vapor deposition film) is special and effective for the bombarding of the base material and the subsequent coating of the intermediate film. Since there is a combination condition, it is in the point that the film adhesion of the surface coating component can be dramatically improved by implementing it.
  • the base metal before coating the physical vapor deposition film that becomes the surface layer of the surface coating component, the base metal is subjected to a metal ion bombarding process using an arc ion plating method, and an intermediate metal film is formed thereon by a sputtering method. It is to coat.
  • the reason will be described together with preferable conditions.
  • the base material before the physical vapor deposition film is coated is subjected to metal ion bombardment by an arc ion plating method.
  • metal ion bombardment by an arc ion plating method.
  • a large amount of oxygen exists at the interface between the film and the base material, resulting in poor adhesion.
  • Oxygen present at this interface originates from the oxide film formed on the surface of the base material from the beginning, and is a residual element that has not been removed by the argon gas bombardment process.
  • the bias voltage applied to the base material is desirably a high negative pressure range of about ⁇ 400 to ⁇ 1000 V in order to obtain the above effect.
  • the metal species used for this metal ion bombardment is titanium. Since titanium has a high reactivity with oxygen, in addition to the above physical action, it is possible to further remove the oxide film from a chemical action. And before performing the metal ion bombardment of this invention, you may perform the conventional argon gas bombardment, and this combined use is preferable. When the argon gas bombardment process is performed, it is desirable that the bias voltage applied to the base material at that time is about ⁇ 100 to ⁇ 600V.
  • an intermediate metal film is coated by a sputtering method.
  • a sputtering method Conventionally, as a means of coating a physical vapor deposition film on a base material, by intentionally making the magnetic field of the sputtering source non-equilibrium, the plasma irradiation to the base material is strengthened, and a dense and highly adhesive film is formed.
  • a non-equilibrium magnetron sputtering method which is advantageous for formation is applied. Therefore, also in the present invention, it is preferable to apply the non-equilibrium magnetron sputtering method as described later for the formation of the physical vapor deposition film.
  • a feature of the present invention is that the base material after the metal ion bombardment is not immediately formed with this physical vapor deposition film, but further adhesion is achieved. An intermediate film is formed for the purpose.
  • the hard physical vapor deposition film applied to the surface layer of the base material is represented by, for example, a carbon film described later from a compound such as carbide, nitride, or sulfide, and the hardness thereof is approximately 1000 HV or more, Is a high hardness of 1500 HV or more and 2000 HV or more. Therefore, the adhesion strength is easily deteriorated due to the internal stress of the coating between the base material and the physical vapor deposition coating. Therefore, by sandwiching the intermediate metal film of the present invention between them, the metal film is lower in hardness than the physical vapor deposition film, so that the stress difference generated between the base material and the film is buffered. Has an effect. And about reducing the hardness of this intermediate
  • the hardness of the intermediate metal film is not necessarily required for the base material while considering the physical vapor deposition film. That is, this is because the adhesion between the base material and the intermediate metal film can be secured by performing the above-described metal ion bombardment on the base material before coating the intermediate film.
  • the intermediate metal film of the present invention is preferably composed of a single metal layer in view of the above-described stress buffering effect and ease of management of the film configuration.
  • titanium having an appropriate hardness of about 200 to 300 HV and a large oxygen scavenging action is preferable.
  • the adhesion between the base material and the intermediate metal film is further improved by applying the same kind of metal as the metal element used in the metal ion bombardment. This is because, for the present invention using the arc ion plating method for the metal ion bombardment process, a trace amount of the metal element may remain on the base material after the process.
  • the intermediate metal film is preferably coated by a nonequilibrium magnetron sputtering method.
  • molten particles droplets
  • the non-equilibrium magnetron sputtering method can eliminate the generation of molten grains, so that a smooth film can be obtained.
  • the series of coating processes is performed. Is characterized by applying a sputtering method and using an arc ion plating method only for metal ion bombardment.
  • the coating process by the sputtering method is continuously performed in a state where the processed base material is maintained in the process chamber.
  • a physical vapor deposition apparatus that performs a coating process by placing an object to be processed (base material) in a chamber, once the base material after the metal ion bombarding process is taken out of the processing chamber, an oxide film or Dirt is formed. Therefore, it is desirable that the metal ion bombardment process and the subsequent coating process by the sputtering method are continuously performed while the base material is maintained in the process chamber.
  • this physical vapor deposition apparatus has facilities, such as an evaporation source for arc ion plating and a sputtering target, necessary for a series of physical vapor deposition processes to be applied.
  • the physical vapor deposition film is a carbon film, and between the carbon film and the intermediate metal film, a mixed gradient of metal and carbon in which the metal content gradually decreases toward the carbon film side. Cover the film.
  • the type of physical vapor deposition film to be coated on the intermediate metal film is not limited.
  • the physical vapor deposition film is preferably a carbon film represented by diamond, graphite, or diamond-like carbon (DLC).
  • diamond-like carbon composed of a bond between both sp 2 and sp 3 carbons is a film having high hardness and excellent sliding properties, and therefore is preferably applied.
  • the above carbon film particularly DLC
  • the carbon film particularly DLC
  • the Bias voltage negative pressure
  • the Bias voltage when coating the carbon film of the present invention is preferably about ⁇ 40 to ⁇ 150V.
  • the bias voltage when the intermediate metal film or the mixed gradient film is coated before the carbon film is coated may follow the Bias voltage when the carbon film is coated.
  • the base material used for the surface covering component of the present invention may be of any material in order to obtain the above effects. However, in consideration of the fact that it can be applied to tools such as sliding parts and molds, it is desirable that the base material be a metal material with an alloy design such as steel typified by various tool steels.
  • the thickness of the physical vapor deposition film of the present invention is controlled to about 0.5 to 3 ⁇ m by the total film thickness from the intermediate metal film coated after the metal ion bombardment process. It is desirable in terms of both.
  • test piece (diameter 20 mm ⁇ thickness 5 mm) of JIS high-speed tool steel SKH51 adjusted to a hardness of 64 HRC was prepared as a base material for surface treatment. These test piece planes were mirror-polished and then subjected to alkaline ultrasonic cleaning.
  • Sample No. of the present invention 1-4 The prepared base material is placed in a non-equilibrium magnetron sputtering apparatus with a chamber volume of 1.4 m 3 (the insertion space for the processed product is 0.3 m 3 ), and a vacuum at a temperature of 773 K and a pressure of 1 ⁇ 10 ⁇ 3 Pa. After sufficient degassing in the atmosphere, bombarding with argon gas plasma at a pressure of 2.0 Pa at a temperature of 723 K was performed at a bias voltage of ⁇ 200 V to ⁇ 500 V for 5 minutes. Next, metal ion bombardment was performed by arc ion plating using titanium as the metal at a temperature of 723 K and a Bias voltage of ⁇ 500 V to ⁇ 800 V for 2 minutes.
  • Sample No. Table 1 summarizes the bias voltage conditions 1 to 7 during the bombardment process and the coating process.
  • TEM transmission electron microscope
  • the interface between the base material and the coating film was measured by using a field emission transmission microscope (FE-TEM: JEM-2010F type manufactured by JEOL Ltd.) with an acceleration voltage of 200 kV, 40 Observation was carried out under 10,000 times conditions. And about the interface which performed this TEM observation, the amount of oxygen analysis was performed by energy dispersive X-ray spectroscopy (EDS: Nolan's UTW type Si (Li) semiconductor detector) with a beam diameter of 1 nm. There were three measurement sites, a site located 10 nm from the interface on the film side (inside the intermediate titanium film), a base material-coating interface, and a base material located 10 nm from the interface on the base material side.
  • EDS energy dispersive X-ray spectroscopy
  • Long / indentation perimeter) ratio is less than 1/2
  • C is greater than or equal to 1/2 and less than 3/4
  • E is greater than or equal to 3/4 and less than 1 (entire circumference)
  • Sample No. Table 2 shows the amount of oxygen present in the vicinity of the interface and the evaluation results of adhesion of the coating films 1 to 7.
  • FIG. 1 is a TEM image showing the vicinity of the interface between the base material and the film.
  • the DLC film coated through the titanium and carbon gradient film is excellent in adhesion.
  • FIG. 1 is a photomicrograph showing the results of the adhesion evaluation test (state around Rockwell indentation).
  • FIG. 5 is a TEM image showing the vicinity of the interface of FIG. 5, and a layer having a thickness of about 5 nm containing oxygen can be confirmed to be white.
  • the sample No. The DLC film of 5 to 7 was peeled around the indentation as a result of the adhesion evaluation, although the intermediate titanium film and the gradient film of titanium and carbon were introduced, and sufficient adhesion was not obtained.
  • FIG. 5 is a photomicrograph showing the results of the adhesion evaluation test of No. 5 (state around the Rockwell indentation).
  • the present invention can be applied to sliding parts and molds. Specifically, it can also be applied to automotive parts such as valve lifters, needles or plungers.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Physical Vapour Deposition (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

Le procédé de production ci-décrit permet de produire un composant à surface revêtue ayant une excellente adhérence à un film dur. Le procédé de production comprend l'application d'un film dur en phase gazeuse par un procédé physique, de préférence, un film dur ayant une dureté superficielle égale ou supérieure à 1000 HV, sur une surface d'un matériau de base. Avant dépôt du film, le matériau de base est soumis à un traitement par bombardement d'ions métalliques par placage ionique à l'arc. Après quoi, un film métallique intermédiaire est appliqué par pulvérisation, et un film déposé en phase gazeuse par un procédé physique est ensuite appliqué à titre de couche superficielle. De préférence, le métal utilisé dans le traitement par bombardement d'ions métallique est le titane, et le film métallique intermédiaire est en titane. De préférence, le film déposé en phase vapeur par un procédé physique est un film en carbone, et un film à gradient mixte métal-carbone, la teneur en métal étant progressivement réduite au profit du film en carbone, est appliqué entre le film de carbone et le film métallique intermédiaire. De plus, le film en carbone est, de préférence, à base d'un carbone du type diamant.
PCT/JP2009/054075 2008-03-28 2009-03-04 Procédé de production d'un composant à surface revêtue ayant une excellente adhérence à un film Ceased WO2009119269A1 (fr)

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JP2010505491A JP5418917B2 (ja) 2008-03-28 2009-03-04 皮膜密着性に優れた表面被覆部品の製造方法

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JP2008085938 2008-03-28
JP2008-085938 2008-03-28

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012097821A (ja) * 2010-11-02 2012-05-24 Hitachi Ltd 摺動部品およびそれを用いた機械装置
GB2565320A (en) * 2017-08-10 2019-02-13 Yang Shicai Gradient method to deposit hard and lubricant coatings
WO2019167674A1 (fr) * 2018-02-27 2019-09-06 日立金属株式会社 Élément de revêtement et son procédé de fabrication
CN112135372A (zh) * 2020-09-08 2020-12-25 大连理工大学 一种具有结构色梯度的彩色碳纤维热管理器件及制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107338414A (zh) * 2016-05-03 2017-11-10 大连金泰表面工程科技有限公司 导电,抗腐蚀,耐磨损,高硬度类金刚石涂层的制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63286334A (ja) * 1987-05-19 1988-11-24 Idemitsu Petrochem Co Ltd 積層体およびその製造法
JP2003082458A (ja) * 2001-09-10 2003-03-19 Sumitomo Electric Ind Ltd 非晶質炭素被膜の形成装置及び形成方法
JP2007070667A (ja) * 2005-09-05 2007-03-22 Kobe Steel Ltd ダイヤモンドライクカーボン硬質多層膜成形体およびその製造方法
JP2007136597A (ja) * 2005-11-17 2007-06-07 Tungaloy Corp 被覆部材

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63286334A (ja) * 1987-05-19 1988-11-24 Idemitsu Petrochem Co Ltd 積層体およびその製造法
JP2003082458A (ja) * 2001-09-10 2003-03-19 Sumitomo Electric Ind Ltd 非晶質炭素被膜の形成装置及び形成方法
JP2007070667A (ja) * 2005-09-05 2007-03-22 Kobe Steel Ltd ダイヤモンドライクカーボン硬質多層膜成形体およびその製造方法
JP2007136597A (ja) * 2005-11-17 2007-06-07 Tungaloy Corp 被覆部材

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012097821A (ja) * 2010-11-02 2012-05-24 Hitachi Ltd 摺動部品およびそれを用いた機械装置
GB2565320A (en) * 2017-08-10 2019-02-13 Yang Shicai Gradient method to deposit hard and lubricant coatings
WO2019167674A1 (fr) * 2018-02-27 2019-09-06 日立金属株式会社 Élément de revêtement et son procédé de fabrication
JP6593667B1 (ja) * 2018-02-27 2019-10-23 日立金属株式会社 被覆部材およびその製造方法
CN111771011A (zh) * 2018-02-27 2020-10-13 日立金属株式会社 被覆构件及其制造方法
CN111771011B (zh) * 2018-02-27 2022-07-05 日立金属株式会社 被覆构件及其制造方法
US11976350B2 (en) 2018-02-27 2024-05-07 Proterial, Ltd. Covering member and method for manufacturing the same
CN112135372A (zh) * 2020-09-08 2020-12-25 大连理工大学 一种具有结构色梯度的彩色碳纤维热管理器件及制备方法

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Publication number Publication date
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JPWO2009119269A1 (ja) 2011-07-21

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