CN107034440B - 一种复合类金刚石碳膜及其制备方法 - Google Patents
一种复合类金刚石碳膜及其制备方法 Download PDFInfo
- Publication number
- CN107034440B CN107034440B CN201710302800.2A CN201710302800A CN107034440B CN 107034440 B CN107034440 B CN 107034440B CN 201710302800 A CN201710302800 A CN 201710302800A CN 107034440 B CN107034440 B CN 107034440B
- Authority
- CN
- China
- Prior art keywords
- dlc
- layers
- crc
- tic
- alloy
- 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
Links
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 15
- 239000010432 diamond Substances 0.000 title claims abstract description 15
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 26
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 26
- 102100021446 Rho GTPase-activating protein 7 Human genes 0.000 claims abstract description 25
- 101710116900 Rho GTPase-activating protein 7 Proteins 0.000 claims abstract description 25
- 101000647991 Homo sapiens StAR-related lipid transfer protein 13 Proteins 0.000 claims abstract description 23
- 102100025252 StAR-related lipid transfer protein 13 Human genes 0.000 claims abstract description 23
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910000599 Cr alloy Inorganic materials 0.000 claims abstract description 4
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 60
- 229910052786 argon Inorganic materials 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 29
- 238000000151 deposition Methods 0.000 claims description 16
- 230000008021 deposition Effects 0.000 claims description 16
- 238000010849 ion bombardment Methods 0.000 claims description 12
- 150000001721 carbon Chemical group 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000005496 tempering Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 229910001203 Alloy 20 Inorganic materials 0.000 claims 1
- 101100278842 Caenorhabditis elegans dlc-1 gene Proteins 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 5
- 238000005299 abrasion Methods 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010720 hydraulic oil Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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
- C23C14/22—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
- 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
- C23C14/025—Metallic sublayers
-
- 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
- C23C14/0635—Carbides
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
- C23C28/046—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 with at least one amorphous inorganic material layer, e.g. DLC, a-C:H, a-C:Me, the layer being doped or not
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公布了一种复合类金刚石碳膜及其制备方法,该结构自基体表面底层从内而外依次包括Cr、Ti或Cr和Ti合金打底层,CrC、TiC或CrC和TiC合金过渡层,以及DLC‑1层和DLC‑2层;其中,DLC‑1层和DLC‑2层分别由含有不同混合比例的sp3与sp2杂化碳原子构成;所述膜的DLC层由线性大面积离子源电离乙炔气体获得,适用于涂覆大面积低温处理工件表面;该涂层具有较高的膜‑基结合强度,同时表现出优良的减摩耐磨性能,尤其在应用于大型活塞表面处理后,有效改善了大型活塞在做高速往返运动过程的磨损情况,显著提高了活塞的使用寿命,减少故障率及降低了使用维护成本。
Description
技术领域
本发明涉及一种多层复合类金刚石碳膜及其制备方法,属于表面处理技术领域。
背景技术
类金刚石碳膜(Diamond-like Carbon,DLC),即DLC膜是一种由sp3杂化碳原子和sp2杂化碳原子共同组成的非晶态薄膜。由于结构介于金刚石和石墨之间,DLC膜兼具这两种材料的一些特性,如高硬度、高热导率、低介电常数、优异的减摩抗磨性、良好的光学透过性以及优异的化学惰性和生物相容性等,这使得DLC膜在机械、电子、光学、航空航天、生物医学、装饰外观等多个领域得到了广泛应用。
DLC膜良好的耐磨性、耐腐蚀性和低摩擦系数,可以满足对轴承、密封元器件等许多机械零件的表面强化与防护需求。然而,DLC膜存在的一些缺点也在很大程度上影响着它的应用,其中之一是DLC膜具有很高的内应力,由于内应力较高会导致其作为保护膜不能较好地与金属基体结合,因而限制了膜厚,尤其在大面积DLC膜涂覆时,表现尤为显著。
以液压破碎锤为例,活塞是液压破碎锤的关键部件,其在缸体内往复运动以维持液压破碎锤的正常工作。在实际工作过程中,由于不可避免地受液压油、加工精度及钎杆反弹等的影响,易出现因活塞拉伤而产生漏油的现象,尤其是较大规格的液压破碎锤,会导致液压破碎锤的冲击功下降,生产效率降低,甚至无法工作。液压破碎锤活塞失效形式主要表现为工作圆柱表面严重磨损、拉伤等,都是从表面开始的。如果能够克服大面积涂覆DLC膜产生的应力,在这种大型活塞表面形成附着力高的DLC膜,就可以在很大程度上延长活塞寿命,提高生产效率,减少使用维修成本。
发明内容
本发明要解决的技术问题是克服现有技术的不足,提供一种适用于涂覆大面积低温处理工件表面的复合类金刚石碳膜及其制备方法。
本发明所述的复合类金刚石碳膜,包括Cr、Ti或Cr和Ti合金打底层,CrC、TiC或CrC和TiC合金过渡层,以及DLC-1层和DLC-2层,主要技术特征在于,按原子数百分比计,所述DLC-1层含有sp3杂化的碳原子数占20~40%,所述DLC-2层含有sp3杂化的碳原子数占0~15%。其中,所述Cr、Ti或Cr和Ti合金层用于改善涂层与基体的结合情况,CrC、TiC或CrC和TiC合金过渡层结构可以为后续DLC涂层提供良好的沉膜环境,DLC-1层可以提供高的硬度和低的摩擦系数,而DLC-2可以起到很好的固体润滑作用,这种组合可以提供优良的摩擦学性能。与现有技术DLC膜相比较,本发明所述DLC膜层分DLC-1层和DLC-2层,按原子数百分比计,其中DLC-1层含有sp3杂化的碳原子数占20~40%,使得DLC膜具有较高的硬度,表现出耐摩擦抗磨损性能;DLC-2层含有sp3杂化的碳原子数占0~15%,因此sp2杂化碳原子数含量较大,从而使得DLC-2层碳膜表现出极高的固体润滑性,DLC膜表面润滑性高,能有效地减少基体表面摩擦系数。因此,DLC-1和DLC-2层的叠加能够实现比现有技术DLC膜更优异的减摩耐磨性能;此外,DLC-1和DLC-2层的叠加结构还有利于在制备过程中减少DLC膜层的内应力,其机理见后叙制备方法。
本发明所述复合类金刚石碳膜的进一步技术方案为:所述Cr、Ti或Cr和Ti合金打底层的厚度为300~800nm,CrC、TiC或CrC和TiC合金过渡层的厚度为200~500nm,DLC-1层的厚度为0.5~2μm,DLC-2层的厚度为200~500nm。DLC-1层含有sp3杂化的碳原子数占20~40%,相对硬度较高,DLC-2层含有sp3杂化的碳原子数仅占0~15%,这一层主要是含有sp2杂化的碳原子结构,具有良好的自润滑性能,可以有效降低摩擦系数,但其硬度较DLC-1层要低很多,所以具体实施过程中,可根据备件加工需求来调整各涂层的厚度,以满足工件硬度和耐磨性要求。
本发明所述复合类金刚石碳膜的制备方法为:所述的Cr、Ti或Cr和Ti合金层和CrC、TiC或CrC和TiC合金过渡层由中频磁控溅射获得,相较于多弧的方法,磁控溅射获得涂层表面更佳光滑;DLC-1层和DLC-2层由线性大面积离子源电离乙炔气体获得,本发明所采用的大面积线性离子源技术,利用高的场强,可以有效的电离乙炔气体,相较于磁控溅射碳靶技术,可以获得纯度更高、sp3杂化更多的类金刚石膜层。现有技术磁控溅射石墨靶,存在把靶上的一些污染源也溅射沉积到工件上的可能性,而大面积线性离子源技术可以避免上述污染源,获得纯度更高的DLC膜;同时,采用大面积线性离子源电离乙炔技术可以获得相对更多的sp3杂化碳原子,从而增强DLC膜的硬度。
本发明所述复合类金刚石碳膜的制备方法,具体包括以下步骤:
(1)将基体清洗干净放入真空转架上,打开线性离子源电离氩气,在负偏压的牵引下对基材表面进行轰击清洗;
(2)开启中频金属Cr或Ti靶,对基材进行金属离子轰击,再进行打底Cr、Ti或Cr和Ti合金层沉积,随后进行沉积CrC、TiC或CrC和TiC合金过渡层;
(3)打开大面积线性离子源进行DLC-1层和DLC-2层的沉积。
所述基体为160℃~220℃回火,硬度为HRC57~62的合金钢基材。
所述步骤(1)中,基材轰击的条件为:本底真空度为5×10-4~8×10-3Pa,基体温度为120~180℃,通入氩气控制气压在5×10-2~2×10-1Pa,线性离子源的电压为1200~2000V,负偏压为-300~-1000V,轰击10~30分钟。
所述步骤(2)中,氩离子轰击后,关闭线性离子源,打开中频磁控,电流设为2~10A,真空度增加到2×10-1~1Pa,负偏压保持在-400~-1000V,开启中频金属Cr或Ti靶对基材轰击1~10分钟;轰击完后,偏压降到-50~-200V,中频电流增加到6~15A,其他条件保持不变,开始沉积Cr、Ti或Cr和Ti合金层,沉积30~100分钟,厚度为300~800nm;打完底后,关闭氩气,通入20~50sccm乙炔,沉积CrC层20~60分钟,沉积厚度200~500nm。
所述步骤(3)中,温度保持在120~180℃,通入20~50sccm乙炔,真空炉内真空度维持在5×10-2~2×10-1Pa,线性离子源电压设为1200~1800V,偏压为-300~-800V,沉积60~100分钟,然后关闭乙炔气体,通入氩气,压强保持在5×10-2~2×10-1Pa,偏压为-500~-800V,用氩离子轰击表面5~20分钟,轰击完后,再关闭氩气,通入乙炔,继续沉积DLC-1层60~100分钟;DLC-1沉积完后,关闭乙炔气体,通入氩气,压强保持在5×10-2~2×10- 1Pa,偏压为-500~-800V,用氩离子轰击表面5~20分钟,随后将电压增加到1500~2000V,关闭氩气,通入5×10-2~2×10-1Pa的乙炔,沉积40~100分钟,沉积厚度200~500nm。
上述步骤(3)中,在DLC-1沉积期间和沉积DLC-2前的氩离子轰击,可以达到降低涂层内应力的效果,从而可以实现大面积表面涂覆多层复合类金刚石碳膜;由于涂层在形核成长的过程中,必然会引入拉应力,而氩离子轰击:一方面可以将结合不好的涂层轰掉,另一方面也会引入压应力,从而抵消涂层自身的拉应力,达到降低涂层内应力的效果。
本发明解决了现有技术的DLC膜应用于大面积涂覆时,存在内应力较高易从大面积低温处理工件基材表面剥离的问题,本发明制备方法形成的复合DLC膜相对现有技术DLC膜具有更优越的附着性和更低的摩擦系数,同时在很大程度上降低了膜的内应力,从而能够实现DLC膜的大面积涂覆。
附图说明
图1为本发明表示实施例中的基材及复合类金刚石碳膜的截面结构图。
1、基体 2、多层复合碳膜
21、Cr、Ti或Cr和Ti合金层 22、,CrC、TiC或CrC和TiC合金过渡层
23、DLC-1层 24、DLC-2层
具体实施方式
下面对本发明的实施例作详细说明,本实施例是在本发明技术方案前提下实施的,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述实施例。
以GCr15活塞表面处理为例:
1、首先用超声清洗线对GCr15活塞进行彻底地清洁处理,然后装卡在工件转架上;
2、通过泵组系统将真空室本底真空抽至5~8×10-3Pa,开始加热,设置加热温度150℃,并保温1~1.5小时。通入氩气,压强升至1.5×10-1Pa,打开线性离子源电源,对基材表面进行轰击清洗,电压设为1400~1500V,占空比50%,偏压为-400~-600V,占空比为40%,轰击10~20分钟;
3、氩离子轰击完后,关闭线性离子源,打开中频磁控,电流设为6~8A,真空度增加到5~6×10-1Pa,负偏压保持在-600V,占空比为40%,开启中频金属Cr靶对基材轰击2~3分钟;之后偏压降到-150V,占空比设为80%,中频电流增加到10A,沉积60分钟,获得厚度约为600nm的打底Cr层;
4、打底完成后,关闭氩气,通入30~40sccm乙炔,沉积CrC层40分钟,得到厚度大约为300nm的CrC层;
5、CrC层沉积结束后,关闭中频电源,温度保持在150℃,通入30~40sccm乙炔,真空度为1.0~1.5×10-1Pa,线性离子源电压设为1600V,占空比80%,偏压为-500V,占空比80%,沉积80分钟,然后关闭乙炔气体,通入30~40sccm氩气,压强保持在1.0~1.5×10-1Pa,偏压为-600~-700V,占空比40%,用氩离子轰击表面10分钟,轰击完后,再关闭氩气,通入30~40sccm乙炔,偏压降到-500V,占空比80%,继续沉积60分钟形成DLC-1层;
6、然后关闭乙炔气体,通入氩气,压强保持在1.0~1.5×10-1Pa,偏压为-600~-700V,占空比40%,用氩离子轰击表面10分钟,随后将电压增加到2000V,关闭氩气,通入5×10-2~2×10-1Pa的乙炔,偏压调到-500V,占空比80%,沉积40分钟形成DLC-2层。
总共沉积时间为280分钟,得到厚度为2~2.5μm的多层复合类金刚石碳膜。
该实施例通过采用本发明制备方法获得的复合DLC膜,在现有技术基础上不仅提高了膜基结合力,降低了DLC膜层的内应力,与现有技术相比具有更优越的附着性和更低的摩擦系数以及更好的耐磨性,从而提高了大型液压破碎锤活塞部件的使用寿命和工作稳定性,降低了使用维修成本。
Claims (7)
1.一种复合类金刚石碳膜,自基体表面底层从内而外依次包括Cr、Ti或Cr和Ti合金打底层,CrC、TiC或CrC和TiC合金过渡层,以及DLC-1层和DLC-2层,其特征在于:按原子数百分比计,所述DLC-1层含有sp3杂化的碳原子数占20~40%,所述DLC-2层含有sp3杂化的碳原子数占0~15%,所述复合类金刚石碳膜适用于破碎锤活塞表面涂层。
2.根据权利要求1所述的一种复合类金刚石碳膜,其特征在于:所述Cr、Ti或Cr和Ti合金打底层的厚度为300~800nm,CrC、TiC或CrC和TiC合金过渡层的厚度为200~500nm,DLC-1层的厚度为0.5~2μm,DLC-2层的厚度为200~500nm。
3.复合类金刚石碳膜的制备方法,其特征在于:所述Cr、Ti或Cr和Ti合金层以及CrC、TiC或CrC和TiC合金过渡层由中频磁控溅射获得,DLC-1层和DLC-2层由线性大面积离子源电离乙炔气体获得。
4.根据权利要求3所述的制备方法,其特征在于:首先将清洗后基体放入真空转架上,通入氩气,用线性离子源对基材表面进行轰击清洗。基材轰击的条件为:本底真空度为5×10-4~8×10-3Pa,基体温度为120~180℃,通入氩气控制气压在5×10-2~2×10-1Pa,线性离子源的电压为1200~2000V,负偏压为-300~-1000V,轰击10~30分钟。
5.根据权利要求4所述的制备方法,其特征在于:开启中频金属Cr或Ti靶,对基材进行金属离子轰击,再进行打底Cr、Ti或Cr和Ti合金层沉积,随后进行沉积CrC、TiC或CrC和TiC合金过渡层。具体操作方法为:对基材表面进行轰击清洗后,关闭线性离子源,打开中频磁控,电流设为2~10A,真空度增加到2×10-1~1Pa,负偏压保持在-400~-1000V,开启中频金属Cr或Ti靶对基材轰击1~10分钟;轰击完后,偏压降到-50~-200V,中频电流增加到6~15A,其他条件保持不变,开始沉积Cr、Ti或Cr和Ti合金层,沉积30~100分钟,厚度为300~800nm;打底层完成后,关闭氩气,通入20~50sccm乙炔,沉积CrC、TiC或CrC和TiC合金20~60分钟,沉积厚度为200~500nm。
6.根据权利要求5所述的制备方法,其特征在于:打开线性大面积离子源进行DLC-1层和DLC-2层的沉积。具体操作方法为:温度保持在120~180℃,通入20~50sccm乙炔,真空炉内真空度维持在5×10-2~2×10-1Pa,线性离子源电压设为1200~1800V,偏压为-300~-800V,沉积60~100分钟,然后关闭乙炔气体,通入氩气,压强保持在5×10-2~2×10-1Pa,偏压为-500~-800V,用氩离子轰击表面5~20分钟,轰击完后,再关闭氩气,通入乙炔,继续沉积DLC-1层60~100分钟;DLC-1层沉积完成后,关闭乙炔气体,通入氩气,压强保持在5×10-2~2×10-1Pa,偏压为-500~-800V,用氩离子轰击表面5~20分钟,随后将电压增加到1500~2000V,关闭氩气,通入5×10-2~2×10-1Pa的乙炔,沉积40~100分钟,沉积厚度200~500nm,完成DLC-2层的沉积。
7.根据权利要求3所述的制备方法,其特征在于:适用于基体为160℃~220℃回火,硬度为HRC57~62的合金钢基材。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710302800.2A CN107034440B (zh) | 2017-05-03 | 2017-05-03 | 一种复合类金刚石碳膜及其制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710302800.2A CN107034440B (zh) | 2017-05-03 | 2017-05-03 | 一种复合类金刚石碳膜及其制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107034440A CN107034440A (zh) | 2017-08-11 |
CN107034440B true CN107034440B (zh) | 2019-09-17 |
Family
ID=59537378
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710302800.2A Active CN107034440B (zh) | 2017-05-03 | 2017-05-03 | 一种复合类金刚石碳膜及其制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107034440B (zh) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109913798B (zh) * | 2017-12-13 | 2022-12-23 | 维达力实业(深圳)有限公司 | 表面硬化的石墨模具及其表面硬化的方法 |
CN108396306A (zh) * | 2018-01-12 | 2018-08-14 | 华南理工大学 | 一种低温沉积硬度可控的类金刚石复合薄膜的方法 |
CN109402577B (zh) * | 2018-12-27 | 2021-06-22 | 广东省新材料研究所 | 一种超硬碳基薄膜及其制备方法 |
CN109594042B (zh) * | 2019-01-29 | 2020-10-20 | 苏州涂冠镀膜科技有限公司 | 用于注塑模具的防粘附硬质涂层及其制备方法 |
CN110438465B (zh) * | 2019-08-14 | 2021-04-20 | 中国科学院宁波材料技术与工程研究所 | 金属基体表面抗磨蚀防护涂层及其制备方法与应用 |
CN111139430B (zh) * | 2020-01-17 | 2020-12-11 | 兰州理工大学 | 一种织构化类金刚石碳基薄膜及其制备方法 |
CN111908935B (zh) * | 2020-01-19 | 2022-12-09 | 湖南碳康生物科技有限公司 | 一种碳基复合材料接骨螺钉及其制备方法 |
CN111945119B (zh) * | 2020-09-10 | 2022-05-06 | 东莞市华升真空镀膜科技有限公司 | 碳基薄膜、碳基薄膜的制备方法、刀具及应用 |
CN112458399A (zh) * | 2020-11-24 | 2021-03-09 | 创隆实业(深圳)有限公司 | 一种TiB2/DLC涂层的制备方法 |
CN113278915B (zh) * | 2021-07-22 | 2022-01-18 | 艾瑞森表面技术(苏州)股份有限公司 | 一种具有多孔结构磨合层的dlc复合薄膜及其制备工艺 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102286723A (zh) * | 2011-07-21 | 2011-12-21 | 中国第一汽车股份有限公司 | 一种应用于汽车高合金钢运动摩擦副表面耐磨涂层 |
CN104213076A (zh) * | 2014-08-27 | 2014-12-17 | 慕恩慈沃迪 | Pvd与hipims制备超硬dlc涂层方法及设备 |
CN104630708A (zh) * | 2015-03-06 | 2015-05-20 | 重庆大学 | 一种类金刚石厚膜及其制备方法及一种工件 |
CN106232873A (zh) * | 2014-08-27 | 2016-12-14 | 宝马股份公司 | 用于金属构件的涂层、 用于涂布金属构件的方法、用于内燃机的活塞和机动车辆 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6475573B1 (en) * | 1999-05-03 | 2002-11-05 | Guardian Industries Corp. | Method of depositing DLC inclusive coating on substrate |
TW200741020A (en) * | 2006-04-28 | 2007-11-01 | Tatung Co Ltd | Diamond-like carbon(DLC) film and manufacturing method thereof |
-
2017
- 2017-05-03 CN CN201710302800.2A patent/CN107034440B/zh active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102286723A (zh) * | 2011-07-21 | 2011-12-21 | 中国第一汽车股份有限公司 | 一种应用于汽车高合金钢运动摩擦副表面耐磨涂层 |
CN104213076A (zh) * | 2014-08-27 | 2014-12-17 | 慕恩慈沃迪 | Pvd与hipims制备超硬dlc涂层方法及设备 |
CN106232873A (zh) * | 2014-08-27 | 2016-12-14 | 宝马股份公司 | 用于金属构件的涂层、 用于涂布金属构件的方法、用于内燃机的活塞和机动车辆 |
CN104630708A (zh) * | 2015-03-06 | 2015-05-20 | 重庆大学 | 一种类金刚石厚膜及其制备方法及一种工件 |
Non-Patent Citations (2)
Title |
---|
"离子束大面积、高性能DLC薄膜材料的研究";代伟等;《第八届全国表面工程学术会议暨第三届青年表面工程学术论坛》;20100425;第96-100页 |
"类金刚石涂层与铝合金间的摩擦磨损行为研究";邓耀锋等;《材料研究与应用》;20140315;第8卷(第1期);第10-14页 |
Also Published As
Publication number | Publication date |
---|---|
CN107034440A (zh) | 2017-08-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107034440B (zh) | 一种复合类金刚石碳膜及其制备方法 | |
RU2520245C2 (ru) | Скользящий элемент, в частности поршневое кольцо, имеющий покрытие, и способ получения скользящего элемента | |
CN103334106B (zh) | 一种钛及钛合金球阀密封副和摩擦副的表面硬化处理方法 | |
CN105239039B (zh) | 一种多层纳米复合涂层冲压模具及其制备方法 | |
CN103212729B (zh) | 一种具有CrAlTiN超晶格涂层的数控刀具及其制备方法 | |
CN106884149A (zh) | 水环境耐磨涂层、其制备方法及应用 | |
CN107587133B (zh) | 一种钨探针复合类金刚石涂层及其制备方法 | |
JP7382124B2 (ja) | 改良されたコーティングプロセス | |
CN108411258A (zh) | 一种超厚无氢类金刚石薄膜及其制备方法 | |
CN111500982A (zh) | 一种四面体非晶碳复合涂层及其制备方法 | |
CN102994947A (zh) | 类金刚石复合二硫化钼纳米多层薄膜及其制备方法 | |
CN110423989A (zh) | 一种低残余应力的硬质类金刚石薄膜的制备方法 | |
CN111378927A (zh) | 一种敷设在弹性基底上的硬质薄膜结构及制备方法 | |
CN108977775A (zh) | 一种TiAlSiN涂层刀具制备工艺 | |
CN105039908B (zh) | 具有绝缘性能的类金刚石涂层及制备方法 | |
CN107699859B (zh) | 轴瓦用全金属自润滑减摩涂层及其制备方法 | |
JP2001064005A (ja) | 被覆摺動部材およびその製造方法 | |
Chen et al. | Microstructure and tribological properties of CrAlTiN coating deposited via multi-arc ion plating | |
CN108265291A (zh) | 一种软质基体表面的碳基涂层及其制备方法 | |
CN102673043A (zh) | 一种纺织钢领用高硬度、低摩擦系数耐磨涂层及其沉积方法 | |
CN106676470B (zh) | 一种AlTiON热作模具钢复合梯度涂层及其制备方法 | |
CN109722637A (zh) | 润滑涂层及其制备方法 | |
CN108118305A (zh) | 一种强韧一体化类富勒烯碳氮多层复合薄膜及其制备方法 | |
Yang et al. | Characterization of microstructure and surface properties of GLC film deposited in plasma nitriding system | |
JP5126867B2 (ja) | 炭素膜の製造方法 |
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 | ||
CP03 | Change of name, title or address |
Address after: 243000 Danyang Industrial Park, Bowang District, Ma'anshan City, Anhui Province Patentee after: Ma'anshan Kamet Hydraulic Machinery Co.,Ltd. Address before: 243000 Bowang Danyang Industrial Park, Ma'anshan City, Anhui Province Patentee before: MAANSHAN KAMAITE HYDRAULIC MACHINERY MANUFACTURING Co.,Ltd. |
|
CP03 | Change of name, title or address |