CN113403579A - 一种强韧化CrTiNiSiN纳米复合涂层制备方法 - Google Patents
一种强韧化CrTiNiSiN纳米复合涂层制备方法 Download PDFInfo
- Publication number
- CN113403579A CN113403579A CN202110692487.4A CN202110692487A CN113403579A CN 113403579 A CN113403579 A CN 113403579A CN 202110692487 A CN202110692487 A CN 202110692487A CN 113403579 A CN113403579 A CN 113403579A
- Authority
- CN
- China
- Prior art keywords
- target
- crtinisin
- preparation
- coating
- depositing
- 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.)
- Pending
Links
- 238000000576 coating method Methods 0.000 title claims abstract description 87
- 239000011248 coating agent Substances 0.000 title claims abstract description 83
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000000151 deposition Methods 0.000 claims abstract description 56
- 230000008021 deposition Effects 0.000 claims abstract description 36
- 238000005498 polishing Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 230000007704 transition Effects 0.000 claims abstract description 15
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 14
- -1 argon ions Chemical class 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 10
- 238000005728 strengthening Methods 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 229910003460 diamond Inorganic materials 0.000 claims description 6
- 239000010432 diamond Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010410 layer Substances 0.000 abstract description 9
- 239000011229 interlayer Substances 0.000 abstract description 8
- 238000007373 indentation Methods 0.000 description 8
- 238000001000 micrograph Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 229910017878 a-Si3N4 Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C23C14/06—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
- 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
- C23C14/3464—Sputtering using more than one target
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physical Vapour Deposition (AREA)
Abstract
本发明公开了一种强韧化CrTiNiSiN纳米复合涂层制备方法,包括以下步骤:1)对基材进行镜面抛光和超声清洗;2)将Ti靶和Cr靶分别安装在直流靶上,Si靶和CrNi靶安装在射频靶上,将基材装夹在样品台上,关闭密封盖,改变沉积腔真空度,运用氩离子轰击基材表面进行清洗除污;3)沉积过渡Cr层;4)沉积CrN涂层;5)沉积CrTiNiSiN涂层。实现层间相的稳定过渡,有效提高层间界面质量和结合力;断面形成硬度逐渐增加的梯度,有效提高复合涂层整体的抗载能力;通过优化制备工艺,在实现增韧的前提下有效保证硬度值。
Description
技术领域
本发明涉及薄膜制备领域,具体为一种强韧化CrTiNiSiN纳米复合涂层制备方法。
背景技术
根据Archard磨损模型V=K(PL)/H,材料的磨损体积(V)与其硬度(H)成反比,因此合成超硬质(H>40GPa)涂层就成为科研工作者始终追求的目标。然而,传统均质涂层在提高硬度的同时,会大幅降低其韧性,出现强度和韧性“倒置关系”。即涂层硬度越高、脆性就越大、其韧性也就越小,导致其抵抗裂纹扩展的能力也就越小。涂层韧性差的问题再应用中逐步凸显,如在摩擦磨损、冲蚀防护等应用中,当硬质涂层表面产生了裂纹,其耐磨损性能取决于其韧性。CrTiSiN涂层硬度较高,可以达到超硬硬度,但其高硬度导致韧性较差,当作为刀具涂层或者关键零件保护涂层时,在周期性冲击载荷下容易出现裂纹失效。
涂层增韧常用的方法有组织结构增韧、残余压应力增韧、结构设计增韧、韧性相增韧等,但每种增韧方法具有一定的不足。对于韧性相增韧,软金属Ni是最常用的掺杂相,其原因主要是Ni具有良好的抗氧化特性,元素Ni很难与元素Ti、Cr、Zr、N结合形成化合物,多以自由态的形式存在于过渡金属氮化物薄膜中,从而保持其良好的韧性特征;但软相金属Ni的引入,随着含量的增加会导致硬度和抗磨性大幅降低,因此需要控制好Ni含量。
对于结构增韧,常把软金属(Ni、Cu等)和硬质涂层构成多层结构,这种多层结构能有效提高涂层的韧性。然而,Ni和Cu不能和过渡金属氮化物形成化合相,因此,层间界面质量及结合力较差,容易发生层间剥离而失效。鉴于单一增韧方法的局限性,多种增韧方法协同作用已成为硬质涂层增韧发展的趋势。
发明内容
本发明的目的在于提供一种强韧化CrTiNiSiN纳米复合涂层制备方法,实现层间相的稳定过渡,有效提高层间界面质量和结合力;断面形成硬度逐渐增加的梯度,有效提高复合涂层整体的抗载能力;通过优化制备工艺,在实现增韧的前提下有效保证硬度值。
为达到上述目的,根据本发明的一个方面,本发明提供如下技术方案:
一种强韧化CrTiNiSiN纳米复合涂层制备方法,包括以下步骤:
1)对基材进行镜面抛光和超声清洗;
2)将Ti靶和Cr靶分别安装在直流靶上,Si靶和CrNi靶安装在射频靶上,将基材装夹在样品台上,关闭密封盖,改变沉积腔真空度,运用氩离子轰击基材表面进行清洗除污;
3)沉积过渡Cr层;
4)沉积CrN涂层;
5)沉积CrTiNiSiN涂层。
本发明进一步设置为:所述步骤1)对基材进行镜面抛光和超声清洗,具体为,基材在金相抛光机上进行镜面抛光,先用w20金刚石粉配合粗抛帆布进行粗抛,然后用w2.5金刚石粉配合精抛绒布进行精抛,基材精抛清洗干净后,在酒精溶液中进行超声清洗20~30分钟。
本发明进一步设置为:所述步骤2)中,沉积腔真空度抽至2.5×10-3~3.0×10- 3Pa,氩离子的流量20sccm,基材偏压为-500V。
本发明进一步设置为:所述步骤2)中,Ti靶和Cr靶的靶材纯度为99.9%,Si靶和CrNi靶的靶材纯度为99.99%,且CrNi靶为Cr占20%,Ni占80%的合金靶材。
本发明进一步设置为:所述步骤3)沉积过渡Cr层,具体为,沉积腔工作气体压强保持0.10~0.15Pa,制备温度在180~250℃之间,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr靶电流4A,沉积过渡Cr层10分钟。
本发明进一步设置为:所述步骤4)沉积CrN涂层,具体为,沉积腔工作气体压强保持0.10~0.15Pa,制备温度在180~250℃之间,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr靶电流4A,N2流量为8sccm,沉积30分钟。
本发明进一步设置为:所述步骤5)沉积CrTiNiSiN涂层,具体为,沉积腔工作气体压强保持0.10~0.15Pa,制备温度在180~250℃之间,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr和Ti靶电流均为4A,Si靶功率1000W,CrNi靶功率400~1200W,制备CrTiNiSiN复合薄膜,沉积时间为180分钟。
本发明进一步设置为:所述基材为硬质合金样片基材。
本发明进一步设置为:所述过渡Cr层厚度为100nm,CrN涂层厚度为400nm,CrTiNiSiN涂层厚度为2.5μm。
与现有技术相比,本发明具有的有益之处是:涂层采用Cr-CrN-CrTiNiSiN多层结构,层间界面均存在CrNx相,实现层间相的稳定过渡,有效提高层间界面质量和结合力;Cr/CrN/CrTiNiSiN复合涂层断面形成硬度逐渐增加的梯度,能有效提高复合涂层整体的抗载能力;通过优化制备工艺,控制软相金属Ni的掺杂量和涂层内其它元素成分含量,生成(Cr,Ti)N结晶相镶嵌于a-Si3N4非晶基质中、非晶相Ni以固溶体形式存在于(Cr,Ti)N晶粒间,固溶强化效应和纳米复合结构nc-(Cr,Ti)N/a-Si3N4的形成,实现增韧的前提下有效保证硬度值。
附图说明
图1为实施例1制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的断面形貌扫描电镜图;
图2为实施例1制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的纳米压痕形貌;
图3为实施例2制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的断面形貌扫描电镜图;
图4为实施例2制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的纳米压痕形貌;
图5为实施例3制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的断面形貌扫描电镜图;
图6为实施例3制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的纳米压痕形貌;
图7为Cr/CrN/CrTiNiSiN多层纳米复合涂层示意图;
具体实施方式
下面结合说明书附图,对本发明作进一步的说明。
如图7所示,为制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层示意图。
实施例1:
本发明提供了一种强韧化CrTiNiSiN纳米复合涂层制备方法,包括以下步骤:
1)对基材进行镜面抛光和超声清洗;
对硬质合金样片基材进行镜面抛光和超声清洗,硬质合金样片基材在金相抛光机上进行镜面抛光,先用w20金刚石粉配合粗抛帆布进行粗抛,然后用w2.5金刚石粉配合精抛绒布进行精抛,基材精抛清洗干净后,在酒精溶液中进行超声清洗20分钟。
2)将靶材纯度为99.9%的Ti靶和Cr靶分别安装在直流靶上,靶材纯度为99.99%的Si靶和CrNi靶安装在射频靶上,所述CrNi靶为Cr占20%,Ni占80%的合金靶材,将基材装夹在样品台上,关闭密封盖,改变沉积腔真空度,运用氩离子轰击基材表面进行清洗除污;其中沉积腔真空度抽至2.5×10-3Pa,氩离子的流量20sccm,基材偏压为-500V。
3)沉积过渡Cr层;
沉积腔工作气体压强保持0.10Pa,薄膜沉积过程中没有开启加热源,制备温度在180℃,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr靶电流4A,沉积过渡Cr层10分钟。
4)沉积CrN涂层;
沉积腔工作气体压强保持0.10Pa,薄膜沉积过程中没有开启加热源,制备温度在180℃,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr靶电流4A,N2流量为8sccm,沉积30分钟。
5)沉积CrTiNiSiN涂层;
沉积腔工作气体压强保持0.10Pa,薄膜沉积过程中没有开启加热源,制备温度在180℃,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr和Ti靶电流均为4A,Si靶功率1000W,CrNi靶功率400W,制备CrTiNiSiN复合薄膜,沉积时间为180分钟。
实施例1制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层断面形貌扫描电镜图如图1所示。
实施例1制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层,Cr含量为63.1at.%,Ti含量为9.1at.%,Ni含量为0.9at.%,Si含量为0.7at.%,N含量为26.2at.%;Cr/CrN/CrTiNiSiN多层纳米复合涂层的纳米硬度为48.5GPa,弹性模量为512.5GPa;涂层使用纳米压痕大载荷压入深度1μm后,运用扫描电子显微镜测试压痕形貌在压痕尖端未发现放射性裂纹,只是在压痕边缘出现堆积裂纹,如图2所示。
实施例2:
采用与实施例1相同的材料和方法,其与实施例1中的区别在于,步骤1)对基材进行镜面抛光和超声清洗中,超声清洗25分钟;步骤2)中,沉积腔真空度抽至2.7×10-3Pa;步骤3)沉积过渡Cr层中,沉积腔工作气体压强保持0.12Pa,制备温度在200℃;步骤4)沉积CrN涂层中,沉积腔工作气体压强保持0.12Pa,制备温度在200℃;步骤5)沉积CrTiNiSiN涂层中沉积腔工作气体压强保持0.12Pa,制备温度在200℃,CrNi靶功率为800W。
实施例2制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层的断面形貌扫描电镜图如图3所示。
实施例2制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层,Cr含量为60.7at.%,Ti含量为8.6at.%,Ni含量为9.7at.%,Si含量为1.4at.%,N含量为19.5at.%;Cr/CrN/CrTiNiSiN多层纳米复合涂层的纳米硬度为43.6GPa,弹性模量为464.5GPa,具有超硬硬度;涂层使用纳米压痕大载荷压入深度1μm后,运用扫描电子显微镜测试压痕形貌,未发现裂纹,如图4所示,表明涂层具有较好的韧性。
因涂层具有超硬硬度和良好的韧性,获得硬韧兼备涂层,因此适合应用于耐磨涂层的保护层或者刀具涂层。
实施例3:
采用与实施例1相同的材料和方法,其与实施例1中的区别在于,步骤1)对基材进行镜面抛光和超声清洗中,超声清洗30分钟;步骤2)中,沉积腔真空度抽至3.0×10-3Pa;步骤3)沉积过渡Cr层中,沉积腔工作气体压强保持0.15Pa,制备温度在250℃;步骤4)沉积CrN涂层中,沉积腔工作气体压强保持0.15Pa,制备温度在250℃;步骤5)沉积CrTiNiSiN涂层中沉积腔工作气体压强保持0.15Pa,制备温度在250℃,CrNi靶功率为1200W。
实施例3制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层断面形貌扫描电镜图如图5所示。
实施例3制备的Cr/CrN/CrTiNiSiN多层纳米复合涂层,Cr含量为57.1at.%,Ti含量为7.8at.%,Ni含量为16.0at.%,Si含量为2.0at.%,N含量为17.1at.%;Cr/CrN/CrTiNiSiN多层纳米复合涂层的纳米硬度为38.3GPa,弹性模量为412.8GPa;涂层使用纳米压痕大载荷压入深度1μm后,运用扫描电子显微镜测试压痕形貌,未发现裂纹,如图6所示。
以上显示和描述了本发明的基本原理、主要特征及优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (9)
1.一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于,包括以下步骤:
1)对基材进行镜面抛光和超声清洗;
2)将Ti靶和Cr靶分别安装在直流靶上,Si靶和CrNi靶安装在射频靶上,将基材装夹在样品台上,关闭密封盖,改变沉积腔真空度,运用氩离子轰击基材表面进行清洗除污;
3)沉积过渡Cr层;
4)沉积CrN涂层;
5)沉积CrTiNiSiN涂层。
2.根据权利要求1所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述步骤1)对基材进行镜面抛光和超声清洗,具体为,基材在金相抛光机上进行镜面抛光,先用w20金刚石粉配合粗抛帆布进行粗抛,然后用w2.5金刚石粉配合精抛绒布进行精抛,基材精抛清洗干净后,在酒精溶液中进行超声清洗20~30分钟。
3.根据权利要求1所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述步骤2)中,沉积腔真空度抽至2.5×10-3~3.0×10-3Pa,氩离子的流量20sccm,基材偏压为-500V。
4.根据权利要求1所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述步骤2)中,Ti靶和Cr靶的靶材纯度为99.9%,Si靶和CrNi靶的靶材纯度为99.99%,且CrNi靶为Cr占20%,Ni占80%的合金靶材。
5.根据权利要求1所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述步骤3)沉积过渡Cr层,具体为,沉积腔工作气体压强保持0.10~0.15Pa,制备温度在180~250℃之间,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr靶电流4A,沉积过渡Cr层10分钟。
6.根据权利要求5所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述步骤4)沉积CrN涂层,具体为,沉积腔工作气体压强保持0.10~0.15Pa,制备温度在180~250℃之间,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr靶电流4A,N2流量为8sccm,沉积30分钟。
7.根据权利要求6所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述步骤5)沉积CrTiNiSiN涂层,具体为,沉积腔工作气体压强保持0.10~0.15Pa,制备温度在180~250℃之间,基材旋转速度每分钟5转,Ar气流量20sccm,基材偏压-60V,Cr和Ti靶电流均为4A,Si靶功率1000W,CrNi靶功率400~1200W,制备CrTiNiSiN复合薄膜,沉积时间为180分钟。
8.根据权利要求1所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述基材为硬质合金样片基材。
9.根据权利要求1所述的一种强韧化CrTiNiSiN纳米复合涂层制备方法,其特征在于:所述过渡Cr层厚度为100nm,CrN涂层厚度为400nm,CrTiNiSiN涂层厚度为2.5μm。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110692487.4A CN113403579A (zh) | 2021-06-22 | 2021-06-22 | 一种强韧化CrTiNiSiN纳米复合涂层制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110692487.4A CN113403579A (zh) | 2021-06-22 | 2021-06-22 | 一种强韧化CrTiNiSiN纳米复合涂层制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113403579A true CN113403579A (zh) | 2021-09-17 |
Family
ID=77682263
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110692487.4A Pending CN113403579A (zh) | 2021-06-22 | 2021-06-22 | 一种强韧化CrTiNiSiN纳米复合涂层制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113403579A (zh) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010089184A (ja) * | 2008-10-06 | 2010-04-22 | Dijet Ind Co Ltd | 被覆切削工具基材 |
CN103029366A (zh) * | 2012-12-06 | 2013-04-10 | 浙江工业大学 | 一种含有NiCrN三元涂层的制品及制备方法 |
JP2013233602A (ja) * | 2012-05-08 | 2013-11-21 | Sumitomo Electric Hardmetal Corp | 表面被覆切削工具 |
CN107459370A (zh) * | 2017-08-15 | 2017-12-12 | 上海双石钛金有限公司 | 一种陶瓷基多彩镀层及其制备方法 |
CN111118385A (zh) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | 一种防腐蚀合金抽油杆及其制造方法 |
CN111172503A (zh) * | 2019-12-26 | 2020-05-19 | 西安交通大学 | 一种锆合金包壳表面多层复合涂层及其制备方法 |
-
2021
- 2021-06-22 CN CN202110692487.4A patent/CN113403579A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010089184A (ja) * | 2008-10-06 | 2010-04-22 | Dijet Ind Co Ltd | 被覆切削工具基材 |
JP2013233602A (ja) * | 2012-05-08 | 2013-11-21 | Sumitomo Electric Hardmetal Corp | 表面被覆切削工具 |
CN103029366A (zh) * | 2012-12-06 | 2013-04-10 | 浙江工业大学 | 一种含有NiCrN三元涂层的制品及制备方法 |
CN107459370A (zh) * | 2017-08-15 | 2017-12-12 | 上海双石钛金有限公司 | 一种陶瓷基多彩镀层及其制备方法 |
CN111118385A (zh) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | 一种防腐蚀合金抽油杆及其制造方法 |
CN111172503A (zh) * | 2019-12-26 | 2020-05-19 | 西安交通大学 | 一种锆合金包壳表面多层复合涂层及其制备方法 |
Non-Patent Citations (1)
Title |
---|
蔡志海等: "Ti含量对(Cr,Ti)N复合涂层组织结构与性能的影响", 《装甲兵工程学院学报》 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109338300B (zh) | 一种高熵合金氮化物涂层的高硬度材料及其制备方法 | |
CN100577860C (zh) | 一种低应力氮化铬多层硬质薄膜的制备方法 | |
CN105887012B (zh) | 一种Zr-B-N纳米复合涂层制备工艺 | |
WO2017156996A1 (zh) | 一种钛合金切削用复合功能刀具涂层及其制备方法 | |
EP1736565A1 (en) | Composite coatings for finishing of hardened steels | |
CN104928638A (zh) | 一种AlCrSiN基多层纳米复合刀具涂层及其制备方法 | |
CN108517487B (zh) | 一种高硬度和高耐磨的TiAlN/W2N多层涂层及其制备方法 | |
CN109097743B (zh) | 一种超硬W-Cr-Al-Ti-N纳米梯度多层膜及其制备方法 | |
CN106086886A (zh) | 一种自润滑二硼化钛/类金刚石涂层及其制备方法和应用 | |
CN107916402A (zh) | 一种AlCrTiSiCN涂层结构及其制备方法 | |
Cao et al. | Microstructure, mechanical and tribological properties of multilayer TiAl/TiAlN coatings on Al alloys by FCVA technology | |
CN111647851B (zh) | 兼具高硬度和高韧性Zr-B-N纳米复合涂层及其制备方法 | |
CN107190233A (zh) | 一种具有超高硬度的Si掺杂纳米复合涂层的制备工艺 | |
CN114196914B (zh) | 一种碳化物高熵陶瓷材料、碳化物陶瓷层及其制备方法和应用 | |
TWI293991B (en) | Sputtering target and method of manufacturing same | |
CN113403579A (zh) | 一种强韧化CrTiNiSiN纳米复合涂层制备方法 | |
JP2015157975A (ja) | 硬質皮膜およびその形成方法 | |
JP7360202B2 (ja) | ダイヤモンドコーティング窒化ケイ素セラミック全体ツールの製造方法 | |
CN110484881A (zh) | 一种致密二硼化钛涂层及其制备方法和应用 | |
JP2012511437A (ja) | 高い寸法精度が必要とされている切削工具インサートの製造方法 | |
US20090226715A1 (en) | Coated article and method of making the same | |
CN113652638A (zh) | 一种超高硬质刀具涂层及其制备方法 | |
Peng et al. | Characterization and adhesion strength of diamond films deposited on silicon nitride inserts by dc plasma jet chemical vapour deposition | |
CN111471973A (zh) | 一种还原性气氛中制备Zr-B-N纳米复合涂层的工艺 | |
CN113403578A (zh) | 一种超硬质多层纳米复合涂层制备方法 |
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 | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210917 |