CN108203810B - 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法 - Google Patents

类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法 Download PDF

Info

Publication number
CN108203810B
CN108203810B CN201711382569.9A CN201711382569A CN108203810B CN 108203810 B CN108203810 B CN 108203810B CN 201711382569 A CN201711382569 A CN 201711382569A CN 108203810 B CN108203810 B CN 108203810B
Authority
CN
China
Prior art keywords
fullerene
target
graphene
boron nitride
controlled
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.)
Active
Application number
CN201711382569.9A
Other languages
English (en)
Other versions
CN108203810A (zh
Inventor
高凯雄
高斌基
张俊彦
张斌
王永富
强力
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.)
Lanzhou Institute of Chemical Physics LICP of CAS
Original Assignee
Lanzhou Institute of Chemical Physics LICP of CAS
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 Lanzhou Institute of Chemical Physics LICP of CAS filed Critical Lanzhou Institute of Chemical Physics LICP of CAS
Priority to CN201711382569.9A priority Critical patent/CN108203810B/zh
Priority to PCT/CN2018/077979 priority patent/WO2019119647A1/zh
Publication of CN108203810A publication Critical patent/CN108203810A/zh
Application granted granted Critical
Publication of CN108203810B publication Critical patent/CN108203810B/zh
Priority to US16/897,881 priority patent/US11225710B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/152—Fullerenes
    • C01B32/154—Preparation
    • 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
    • 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
    • C23C14/0036—Reactive sputtering
    • 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
    • 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
    • C23C14/0605—Carbon
    • 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
    • C23C14/0647—Boron nitride
    • 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
    • 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
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • C23C14/34—Sputtering
    • C23C14/3435—Applying energy to the substrate during sputtering
    • C23C14/345—Applying energy to the substrate during sputtering using substrate bias
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/042—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/044—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
    • 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
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • 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
    • 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
    • C10N2050/025—Multi-layer lubricant coatings in the form of films or sheets

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Nanotechnology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Physical Vapour Deposition (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

本发明公开了一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法，具体步骤为：1）依次在无水乙醇和丙酮中超声清洗基底15min‑30min；2）氩等离子体轰击清洗基底15min；3）利用高真空中频磁控溅射制备具有洋葱状结构的类富勒烯碳层A；4）利用高真空中频磁控溅射镀膜设备溅射单质硼靶制备类石墨烯氮化硼层B；5）重复步骤3）和步骤4），经过60‑80个周期获得按照ABAB……ABA的顺序叠加沉积而获得多层复合薄膜。本发明制备的多层复合超润滑薄膜将克服单一薄膜的缺点，发挥各自的优点，取长补短，从而获得高承载、耐磨损、耐高温和超润滑的高性能薄膜。

Description

类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法
技术领域
本发明属于润滑与防护领域，涉及类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法。
背景技术
目前，薄膜材料已经广泛地应用于润滑领域、计算机领域、云储存、传感器、精密运动机械、微电子学、航空宇航和核工业等各个行业中，其应用范围和作用还在不断地扩大。
薄膜材料应用于润滑领域已有多年。实践表明，摩擦与磨损大多数发生在材料表面和亚表面。因此，提高材料摩擦学性能的关键是如何提高材料的表面性能。通过在材料的表面形成薄膜，可以在不改变材料本身性质的同时有效地改变材料表面的摩擦学性能，从而使材料满足不同的使用要求。
然而，随着航空宇航、云储存、大数据、柔性可穿戴等新技术产业的迅速发展，不仅对极端苛刻工况（真空、高低温交变、高速、高负载等）条件下服役的润滑薄膜材料提出了更加严格的要求，而且由于装备的高可靠、高精度和长寿命方面的要求，对具有超低摩擦和多环境适应性的新型润滑薄膜材料也提出了越来越迫切的需求。
类富勒烯结构碳膜，因其具有低的摩擦系数、高硬度、良好的弹性恢复以及优良的耐磨性能，已作为一种先进的固体润滑材料而受到科学界和工业界的青睐。
氮化硼（h-BN），具有与石墨相似的层状结构，每一层由许多扁平的六角形单元构成，层间以范德华力相结合，层间具有极低的剪切力，具备成为超润滑材料的巨大潜质。在空气中非常稳定，能耐受2270K的高温，在3270K时升华。因此，六方氮化硼可以作为高温固体润滑材料而备受关注。
然而，薄膜材料的研制已经从单层、单一组分向复合化、梯度化和多层化发展。单一的薄膜已经无法满足苛刻的工况和众多设备对高可靠、高精度和长寿命方面的要求，迫切地需要我们制备出性能优异和多环境适应的可靠薄膜。多层复合薄膜将克服单一薄膜的缺点，发挥各自的优点，取长补短，而获得上述需求的高质量薄膜。
多层复合薄膜因其易于实现超润滑、低应力和耐磨损而备受关注。超润滑是指两接触面间摩擦力几乎为零甚至消失的现象，通常认为摩擦系数须小于0.01。因此，综合两种或多种薄膜各自的优异性能，发挥各自优点，使得多层复合薄膜获得超润滑性能成为了现实。
发明内容
本发明的目的在于提供类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法。
本发明主要综合了类富勒烯碳膜的高承载和类石墨烯氮化硼薄膜在高温条件下的低剪切力特点，从而获得高温超润滑复合薄膜。本发明获得了类富勒烯薄膜和类石墨烯氮化硼薄膜的多层结构，该结构有效地削弱了残余应力，显著提高了薄膜与基底间的结合力，解决了氮化硼薄膜在高密度粒子轰击下产生的缺陷。
类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法，其特征在于具体步骤为：
1）依次在无水乙醇和丙酮中超声清洗基底15min-30min；
2）氩（Ar）等离子体轰击清洗基底15min；
3）利用高真空中频磁控溅射制备具有洋葱状结构的类富勒烯碳层A；
4）利用高真空中频磁控溅射镀膜设备溅射单质硼靶制备类石墨烯氮化硼层B；
5）重复步骤3）和步骤4），经过60-80个周期获得按照ABAB……ABA的顺序叠加沉积而获得多层复合薄膜。
所述基底为金属或陶瓷。
所述类富勒烯碳层的厚度为6-12 nm，类石墨烯氮化硼层的厚度为2.1-3.5nm。
所述类富勒烯碳层由甲烷或乙炔经高真空中频磁控溅射制备，腔体内压力控制在10-15Pa，脉冲负偏压控制在800-1000V，占空比控制在60%-80%，溅射时间为10-50 min。
所述类石墨烯氮化硼层利用高真空中频磁控溅射镀膜设备在N2和Ar氛围中溅射单质硼靶，N2纯度大于99.99%，流量控制在55-95sccm，Ar纯度大于99.99%，流量控制在60-120sccm，腔体内压力控制在0.4-0.5Pa，脉冲负偏压控制在400-1000V，占空比控制在60%-80%，溅射时间为10-50 min。
所述磁控溅射所用靶为矩形靶、圆靶或旋转柱靶。
所述单质硼靶硼的纯净度大于99.9%，采用热压成型工艺获得，靶长60-90cm，靶宽10-20cm，靶高1-5cm。
本发明所述多层复合薄膜可以应用于高温条件下金属和陶瓷材质表面的耐磨损和降低摩擦系数，在高温有氧存在的条件下摩擦系数在0.004±0.002之间调整。
本发明所述类富勒烯碳层A和类石墨烯氮化硼层B逐层叠加沉积，获得性能优异的多层复合薄膜，硬度在20-36GPa之间变化。
和单层类富勒烯薄膜以及单层氮化硼薄膜相比较，本发明制备的薄膜具有高承载、耐高温、抗氧化和超润滑性能，摩擦系数低至0.004，磨损率降低70%，承受的高温提升至600-2000℃，寿命提高2-3倍。
附图说明
图1是本发明多层薄膜的断面示意图。
表1是摩擦磨损实验条件及结果汇总表。
Figure 976463DEST_PATH_IMAGE002
表1
具体实施方式
实施例1
1. 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备步骤如下所述：
（1）超声清洗基片：首先用无水乙醇和丙酮超声清洗304不锈钢片15min，用氮气吹干，将基片置于腔体中与靶相距80mm，开始抽真空；
（2）溅射清洗基片：当腔体中压力低于5×10-5Pa，通入氩气，氩气流量为120sccm，脉冲偏压-1000V，占空比70%，氩（Ar）等离子体轰击清洗基片15min，已去除基片表面的氧化物和其他杂质；
（3）类富勒烯碳膜的沉积：打开CH4气体，调节CH4流量为80sccm，调节Ar流量120sccm,保持腔体内压强为15Pa，偏压调节至-800V，溅射时间30 min；
（4）类石墨烯氮化硼的沉积：关闭CH4气体，打开N2，调节N2流量为80sccm，Ar流量为90sccm，保持腔体内压强为0.45Pa，打开单质硼靶挡板，硼靶通电，调节溅射靶电流为1A，脉冲偏压从-400V开始，每5 min偏压升高-100V，偏压升至-600V后保持10 min，溅射时间总共20 min；
（5）重复步骤（3）和（4），连续镀膜80个周期，总厚度1.04μm；
（6）上述所制备薄膜硬度25GPa，结合力60GPa,摩擦系数0.004。
2.采用BASALT-N2摩擦磨损试验机对本发明制备的类富勒烯碳/类石墨烯氮化硼多层超滑薄膜进行性能测试，测试条件为：球-盘往复摩擦模式，载荷20N，频率5Hz，行程5㎜，温度27℃，湿度38%，在不锈钢片上制备有本发明的薄膜，对偶球采用GCr15轴承钢，直径6 mm。结果显示，摩擦系数稳定在0.006，磨损率低至3.4×10-9 m³/Nm，表明本发明制备的薄膜具有超润滑和极低的磨损率。

Claims (7)

1.一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法，其特征在于具体步骤为：
1）依次在无水乙醇和丙酮中超声清洗基底15min-30min；
2）氩等离子体轰击清洗基底15min；
3）利用高真空中频磁控溅射制备具有洋葱状结构的类富勒烯碳层A；
4）利用高真空中频磁控溅射镀膜设备溅射单质硼靶制备类石墨烯氮化硼层B；
5）重复步骤3）和步骤4），经过60-80个周期获得按照ABAB……ABA的顺序叠加沉积而获得多层复合薄膜。
2.如权利要求1所述的制备方法，其特征在于所述基底为金属或陶瓷。
3.如权利要求1所述的制备方法，其特征在于所述类富勒烯碳层的厚度为6-12 nm，类石墨烯氮化硼层的厚度为2.1-3.5nm。
4.如权利要求1所述的制备方法，其特征在于所述类富勒烯碳层由甲烷或乙炔经高真空中频磁控溅射制备，腔体内压力控制在10-15Pa，脉冲负偏压控制在800-1000V，占空比控制在60%-80%。
5.如权利要求1所述的制备方法，其特征在于所述类石墨烯氮化硼层利用高真空中频磁控溅射镀膜设备在N2和Ar氛围中溅射单质硼靶，N2纯度大于99.99%，流量控制在55-95sccm，Ar纯度大于99.99%，流量控制在60-120sccm，腔体内压力控制在0.4-0.5Pa，脉冲负偏压控制在400-1000V，占空比控制在60%-80%。
6.如权利要求1所述的制备方法，其特征在于所述磁控溅射所用靶为矩形靶、圆靶或旋转柱靶。
7.如权利要求1所述的制备方法，其特征在于所述单质硼靶硼的纯净度大于99.9%，采用热压成型工艺获得，靶长60-90cm，靶宽10-20cm，靶高1-5cm。
CN201711382569.9A 2017-12-20 2017-12-20 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法 Active CN108203810B (zh)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201711382569.9A CN108203810B (zh) 2017-12-20 2017-12-20 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法
PCT/CN2018/077979 WO2019119647A1 (zh) 2017-12-20 2018-03-05 一种类富勒烯碳层/类石墨烯氮化硼多层复合超润滑薄膜的制备方法
US16/897,881 US11225710B2 (en) 2017-12-20 2020-06-10 Method for preparing super-lubricative multi-layer composite fullerene-like carbon layer/graphene-like boron nitride thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711382569.9A CN108203810B (zh) 2017-12-20 2017-12-20 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法

Publications (2)

Publication Number Publication Date
CN108203810A CN108203810A (zh) 2018-06-26
CN108203810B true CN108203810B (zh) 2020-05-26

Family

ID=62605884

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711382569.9A Active CN108203810B (zh) 2017-12-20 2017-12-20 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法

Country Status (3)

Country Link
US (1) US11225710B2 (zh)
CN (1) CN108203810B (zh)
WO (1) WO2019119647A1 (zh)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109750259A (zh) * 2019-02-27 2019-05-14 中国科学院兰州化学物理研究所 适用于水环境下超低摩擦磁控氮化硼润滑薄膜的制备方法
CN111607775A (zh) * 2019-05-09 2020-09-01 中国科学院半导体研究所 制备组分可调的二维h-BNC杂化薄膜的方法
CN112791225A (zh) * 2019-11-14 2021-05-14 美国发现集团有限公司 用于肿瘤治疗的纳米机器人及其制备方法
US11932539B2 (en) 2020-04-01 2024-03-19 Graphul Industries LLC Columnar-carbon and graphene-plate lattice composite
CN113140350B (zh) * 2021-03-29 2022-04-26 中国科学院长春光学精密机械与物理研究所 一种超反射镜及其设计方法和制备方法
CN115537727B (zh) * 2022-12-02 2023-03-28 深圳市汉嵙新材料技术有限公司 硅烯复合薄膜及其制备方法、电极及锂离子电池

Family Cites Families (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3417732A1 (de) * 1984-05-12 1986-07-10 Leybold-Heraeus GmbH, 5000 Köln Verfahren zum aufbringen von siliziumhaltigen schichten auf substraten durch katodenzerstaeubung und zerstaeubungskatode zur durchfuehrung des verfahrens
CH680369A5 (zh) * 1989-11-22 1992-08-14 Balzers Hochvakuum
US5392981A (en) * 1993-12-06 1995-02-28 Regents Of The University Of California Fabrication of boron sputter targets
US5759725A (en) * 1994-12-01 1998-06-02 Kabushiki Kaisha Toshiba Photoconductors and electrophotographic photoreceptors containing amorphous fullerenes
US5646474A (en) * 1995-03-27 1997-07-08 Wayne State University Boron nitride cold cathode
US5858538A (en) * 1996-01-08 1999-01-12 Director-General Of Agency Of Industrial Science & Technology Composite luminescent material
US5837331A (en) * 1996-03-13 1998-11-17 Motorola, Inc. Amorphous multi-layered structure and method of making the same
JP2002105623A (ja) * 2000-09-27 2002-04-10 Kobe Steel Ltd カーボンオニオン薄膜およびその製造方法
US8387993B2 (en) * 2005-08-01 2013-03-05 Aktiebolaget Skf Sealing device and method of producing the same
US20080001141A1 (en) * 2006-06-28 2008-01-03 Unidym, Inc. Doped Transparent and Conducting Nanostructure Networks
CN101469402B (zh) * 2007-12-25 2010-11-24 中国科学院兰州化学物理研究所 类富勒烯碳膜的制备方法
US7781061B2 (en) * 2007-12-31 2010-08-24 Alcatel-Lucent Usa Inc. Devices with graphene layers
CN101665942A (zh) * 2008-09-04 2010-03-10 中国科学院兰州化学物理研究所 超润滑复合碳薄膜材料的制备方法
US8835892B2 (en) * 2008-10-30 2014-09-16 Sandisk 3D Llc Electronic devices including carbon nano-tube films having boron nitride-based liners, and methods of forming the same
WO2011127258A1 (en) * 2010-04-07 2011-10-13 Massachusetts Institute Of Technology Fabrication of large-area hexagonal boron nitride thin films
CN102453913A (zh) * 2010-10-29 2012-05-16 中国科学院兰州化学物理研究所 类富勒烯碳基润滑薄膜材料的制备方法
JP2014509442A (ja) * 2011-03-22 2014-04-17 オーシャンズ キング ライティング サイエンス アンド テクノロジー シーオー．，エルティーディー 有機エレクトロルミネセンスデバイス、及び、その導電性基板
CN102994947B (zh) * 2011-09-17 2014-12-10 中国科学院兰州化学物理研究所 类金刚石复合二硫化钼纳米多层薄膜及其制备方法
CN103140067A (zh) * 2011-12-02 2013-06-05 深圳富泰宏精密工业有限公司 壳体及其制作方法
CN103160781B (zh) * 2011-12-16 2015-07-01 中国科学院兰州化学物理研究所 模具钢表面多层梯度纳米复合类金刚石薄膜的制备方法
CN103839821B (zh) * 2012-11-27 2016-08-31 中芯国际集成电路制造(上海)有限公司 晶体管及其制造方法
US9446965B2 (en) * 2013-02-19 2016-09-20 Nanotech Industrial Solutions, Inc. Applications for inorganic fullerene-like particles
US20150167148A1 (en) * 2013-12-17 2015-06-18 Brookhaven Science Associates, Llc Method for Synthesis of Uniform Bi-Layer and Few-Layer Hexagonal Boron Nitride Dielectric Films
CN104152849B (zh) * 2014-08-27 2016-08-31 中国科学院兰州化学物理研究所 合金工具钢柱塞表面批量化沉积类富勒烯碳薄膜的方法
CN105779950B (zh) * 2014-12-25 2018-10-12 中国科学院兰州化学物理研究所 低温气相沉积洋葱结构碳基超润滑薄膜的方法
CN105220120B (zh) * 2015-10-27 2017-06-23 中国科学院兰州化学物理研究所 一种多层复合类富勒烯薄膜在汽车发动机上产业化的方法
DE102016100725A1 (de) * 2016-01-18 2017-07-20 Phitea GmbH Verfahren und Anordnung zum Beschichten eines Substrats

Also Published As

Publication number Publication date
CN108203810A (zh) 2018-06-26
WO2019119647A1 (zh) 2019-06-27
US11225710B2 (en) 2022-01-18
US20200299828A1 (en) 2020-09-24

Similar Documents

Publication Publication Date Title
CN108203810B (zh) 类富勒烯碳/类石墨烯氮化硼多层超滑薄膜的制备方法
Watanabe et al. Tribological characteristics of WS2/MoS2 solid lubricating multilayer films
Erdemir et al. Tribology of diamond-like carbon films: recent progress and future prospects
CN107653438B (zh) 一种具有真空长效润滑性能碳薄膜的制备方法
TWI363742B (en) Diamond-like carbon film
CN105441870B (zh) 一种高硬度、低摩擦系数、低磨损率的固体自润滑涂层
Takeno et al. Deposition of DLC film with adhesive W-DLC layer on stainless steel and its tribological properties
CN101323945A (zh) 含应力缓和层的硬质薄膜及其制备方法
CN103225076A (zh) 一种耐磨石墨烯表面改性方法
CN109136924B (zh) 航天火工分离用石墨烯二硫化钼多层耐磨涂层及制备方法
Li et al. The role of tribo-pairs in modifying the tribological behavior of the MoS2/Ti composite coating
CN103866234A (zh) 多层多元素耐高温类金刚石纳米复合薄膜材料
CN105506566B (zh) 一种弹性硬质润滑纳米复合薄膜材料的制备方法
CN101463466A (zh) 金属掺杂的类金刚石表面离子液体润滑剂自组装润滑薄膜的制备方法
CN101921983B (zh) 一种w-s-c复合膜的制备方法
CN109722637A (zh) 润滑涂层及其制备方法
CN108396306A (zh) 一种低温沉积硬度可控的类金刚石复合薄膜的方法
CN102477540A (zh) 掺杂类金刚石与油脂复合润滑薄膜的制备方法
CN115074684B (zh) 一种含银高熵合金宽温域润滑薄膜材料及其制备方法
Liqiang et al. Preparation, structure and tribological properties of MoS 2 based composite films
CN104928639A (zh) 一种超强韧碳基表面防护涂层及其制备方法
Lei et al. Characterization and tribological behavior of TiAlN/TiAlCN multilayer coatings
CN105779950A (zh) 低温气相沉积洋葱结构碳基超润滑薄膜的方法
Liu et al. Tailoring the lubricative and electroconductive bifunction properties of NbSe2 film by controlling the sputtering plasma
CN111647852A (zh) 一种固体润滑薄膜及其制备方法和用途

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant