CN114032505A - 耐腐蚀防护涂层材料及其制备方法 - Google Patents

耐腐蚀防护涂层材料及其制备方法 Download PDF

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CN114032505A
CN114032505A CN202111301199.8A CN202111301199A CN114032505A CN 114032505 A CN114032505 A CN 114032505A CN 202111301199 A CN202111301199 A CN 202111301199A CN 114032505 A CN114032505 A CN 114032505A
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关晓艳
岳都元
栾奕
贾志忠
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Yantai Jialong Nano Industry Co ltd
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    • 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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • 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
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Abstract

本发明涉及表面工程领域，尤其涉及一种耐腐蚀防护涂层材料及其制备方法，耐腐蚀防护涂层材料包括基材和耐腐蚀防护涂层，所述耐腐蚀防护涂层包含金属过渡层Zr以及ZrN与CrZrN交替沉积的多层结构，所述耐腐蚀防护涂层制备方法依次包含：(1)金属Zr过渡层的沉积；(2)ZrN层的沉积；(3)CrZrN层的沉积；(4)ZrN层和CrZrN层的交替循环沉积。本发明提供的耐腐蚀涂层具有非常优异的耐腐蚀性能和良好的致密度和良好的膜基结合力。本发明技术可应用于化工生产、资源开发以及海洋工程等领域，提高零部件及装备在腐蚀性工况下的运行稳定性及服役寿命。

Description

耐腐蚀防护涂层材料及其制备方法
技术领域
本发明涉及表面工程领域，尤其涉及一种耐腐蚀防护涂层材料及其制备方法。
背景技术
CrN涂层因具有较高的硬度、良好的化学稳定性、优异的耐磨损性能和耐腐蚀性能而常被用作防护涂层。然而，CrN涂层通常呈柱状晶结构。柱状晶之间往往存在贯穿性孔隙或缺陷，是Cl-离子等腐蚀性介质的主要扩散通道，从而严重限制了涂层在腐蚀性介质中的应用。多元复合和多层结构设计常被用来细化晶粒和提高涂层的耐腐蚀性能。Shan等人(Corrosion and wear behaviors of PVD CrN and CrSiN coatings in seawater，Trans.Nonferrous Met.Soc.China 26(2016)175-184.)采用多弧离子镀技术制备的CrSiN涂层在海水环境下的耐腐蚀性能明显优于CrN性能。Khamseh等人(A study of theoxidation behavior of CrN and CrZrNceramic thin films prepared in a magnetronsputtering system,Ceramics International,42(2016)9988-9994.)采用磁控溅射制备的CrZrN薄膜具有更高的硬度和更好的抗氧化性能。Guan等人(Microstructures andproperties of Zr/CrN multilayer coatings fabricated by multi-arc ion plating，tribology international 106(2017)78-87)制备的Zr/CrN多层涂层在海水环境下的腐蚀电流密度可达10-8A/cm2，阻抗值约为105Ωcm2。Münz等人(Industrial scalemanufactured superlattice hard PVD coatings,Surface Engineering 17(2013)15)制备的CrN/NbN多层涂层在NaCl溶液中的腐蚀电流密度低至10-8A/cm2。Wang等人(Corrosionmechanism investigation of TiAlN/CrN superlattice coating by multi-arc ionplating in 3.5wt％NaCl solution 391(2020)125660)制备的TiAlN/CrN超晶格涂层在3.5wt％NaCl溶液中有较好的耐腐蚀性能，极化阻抗值达到1.2*105Ωcm2。综上，多元复合和多层结构设计可以提高涂层的致密度，降低孔隙从而改善CrN涂层的耐腐蚀等性能。
对CrN基多层体系研究报道的较多，然而，关于CrZrN/ZrN多层体系的研究鲜有报道，对CrZrN/ZrN多层涂层体系材料的制备方法也未有涉及。
发明内容
本发明技术可应用于化工生产、资源开发以及海洋工程等领域，提供一种耐腐蚀的表面防护材料和技术。
本发明提供了一种耐腐蚀防护涂层材料及制备方法，该方法处理得到的涂层呈多晶结构，涂层硬度高，附着性好，且在3.5％NaCl溶液中呈现出优良的耐腐蚀性能。
所述耐腐蚀防护涂层材料，包括基材和耐腐蚀防护涂层，所述耐腐蚀防护涂层包含金属过渡层Zr以及ZrN与CrZrN交替沉积的多层结构。
进一步的，在沉积过程中，采用高偏压氩等离子体进行基底刻蚀，偏压为800～1100V，氩气流量为300～600sccm。
进一步的，所述耐腐蚀防护涂层首先在所述金属基底上沉积一层Zr金属过渡层。
进一步的，所述耐腐蚀涂层以金属Zr为过渡层，然后交替沉积ZrN层和CrZrN层。
本发明还提供了上述耐腐蚀防护涂层材料的制备方法，工作腔体中真空度低于3.0×10-3Pa、工件转速2.0～6.0rmp，采用多弧离子镀技术，依次包括以下步骤:
a)将基材超声波清洗并用普通氮气吹干后固定在样品架上，之后放入真空室，靶材与基材的距离为10～15cm。加热腔室温度至400℃，抽真空至真空度低于3×10-4Pa时，通入氩气并用高偏压800～1100V等离子体轰击清洗样品表面10～30min。
b)调节氩气流量为300～600sccm，基底偏压为-20～-70V，铬靶电流为50～70A，溅射纯锆靶材，沉积Zr过渡层10～30min；
c)关闭氩气阀，同时打开氮气阀并调节其流量为300～800sccm，偏压为-20～-70V，锆靶电流为50～70A，沉积ZrN层1～10min；
d)保持其他参数不变，打开铬靶电源并调节其电流为50～70A，沉积CrZrN层1～10min。
循环步骤c)和d)，得到预期涂层厚度的CrZrN/ZrN多层涂层。
与现有技术相比，本发明的有益效果是：
本发明的制备的CrZrN/ZrN多层涂层致密且与基底结合良好，具有较高的硬度等机械性能。在3.5％NaCl溶液中，涂层的交流阻抗值达到108Ωcm2，呈现出良好的耐腐蚀性能。这主要是因为过渡层Zr、CrZrN和ZrN交替沉积的多层结构体系提高了涂层的致密度，Zr过渡层提高了涂层与基底的结合强度，抑制和减少了涂层内部的贯穿性缺陷，从而有效抑制了腐蚀性介质在涂层内部的贯穿和渗透。CrZrN/ZrN多层涂层致密的结构和较少的缺陷使涂层呈现出较高的耐腐蚀性能。
具体实施方式
实施例1：
a)将基材依次在丙酮和无水乙醇中超声波清洗并用普通氮气吹干后固定在样品架上，之后放入真空室，靶材与基材的距离为10cm。加热腔室温度至400℃，当真空度低于3×10-4Pa时，工件转速2.0rmp，通入氩气并用高偏压1000V等离子体轰击清洗样品表面10min。
b)调节氩气流量为300sccm，基底偏压为-20V，锆靶电流为70A，溅射纯锆靶材，沉积Zr过渡层10min；
c)关闭氩气阀，同时打开氮气阀并调节其流量为300sccm，偏压为-20V，锆靶电流为50A，沉积ZrN层1min；
d)保持以上参数不变，打开铬靶并调节电流为70A，沉积CrZrN层10min。
循环步骤c)和d)9次，得到厚度约为5μm的CrZrN/ZrN多层涂层。
测试分析表明涂层与基底结合良好，涂层呈多晶结构，涂层在3.5％NaCl溶液中的腐蚀电位为-0.20V，腐蚀电流密度低至10-7A/cm2，交流阻抗值达到107Ωcm2；较相同参数下制备的单层CrZrN涂层的(腐蚀电流密度低至10-6A/cm2，交流阻抗值约106Ωcm2)耐腐蚀性能有所提高。
实施例2：
a)将基材依次在丙酮和无水乙醇中超声波清洗并用普通氮气吹干后固定在样品架上，之后放入真空室，靶材与基材的距离为10cm。加热腔室温度至400℃，当真空度低于3×10-4Pa时，工件转速6.0rmp，通入氩气并用高偏压800V等离子体轰击清洗样品表面30min。
b)调节氩气流量为600sccm，基底偏压为-70V，锆靶电流为50A，溅射纯锆靶材，沉积Zr过渡层30min；
c)关闭氩气阀，同时打开氮气阀并调节其流量为600sccm，偏压为-70V，锆靶电流为70A，沉积ZrN层10min；
d)保持以上参数不变，打开铬靶并调节电流为50A，沉积CrZrN层1min。
循环步骤c)和d)7次，得到厚度约为6μm的CrZrN/ZrN多层涂层。
测试分析表明涂层与基底结合良好，涂层呈多晶结构，涂层在3.5％NaCl溶液中的腐蚀电位为-0.20V，腐蚀电流密度低至10-7A/cm2，交流阻抗值达到108Ωcm2；较相同参数下制备的单层CrZrN涂层的(腐蚀电流密度低至10-6A/cm2，交流阻抗值约106Ωcm2)耐腐蚀性能有所提高。

Claims (5)

1.一种耐腐蚀防护涂层材料，其特征在于，所述耐腐蚀防护涂层包含金属过渡层Zr以及ZrN与CrZrN交替沉积的多层结构。
2.根据权利要求1所述的耐腐蚀防护涂层材料,其特征在于，在沉积过程中，采用高偏压氩等离子体进行基底刻蚀，偏压为800～1100V，氩气流量为300～600sccm。
3.根据权利要求1所述的耐腐蚀防护涂层材料，其特征在于，所述耐腐蚀防护涂层在所述金属基底上首先沉积一层Zr金属过渡层。
4.根据权利要求3所述的耐腐蚀防护涂层材料，其特征在于，所述耐腐蚀涂层以金属Zr为过渡层，然后交替沉积ZrN层和CrZrN层。
5.一种如权利要求1所述的耐腐蚀防护涂层材料的制备方法,其特征在于,设备腔体中真空度低于3.0×10-3Pa、工件转速2.0～6.0rmp，采用多弧离子镀技术，依次包括以下步骤:
①沉积金属过渡层Zr：Zr靶电流为50～70A，氩气流量为300～600sccm，偏压为-20～-70V，沉积10～30min；
②沉积ZrN层：Zr靶电流为50～70A，氮气流量为300～800sccm，偏压为-20～-70V，沉积1～10min；
③沉积CrZrN层：开启Cr靶电流为50～70A，Zr靶电流为50～70A，氮气流量为300～800sccm，偏压为-20～-70V，沉积1～10min；
交替循环步骤②和③，从而获得ZrN/CrZrN多层涂层。
CN202111301199.8A 2021-11-04 2021-11-04 耐腐蚀防护涂层材料及其制备方法 Pending CN114032505A (zh)

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CN114807850A (zh) * 2022-04-30 2022-07-29 西安交通大学 一种应用于热锻模具表面的氮化物硬质薄膜及其制备方法
CN114990481A (zh) * 2022-06-10 2022-09-02 吉林大学 一种智能组装根状毛细扩散通道的自适应纳米多层膜及其制备方法和应用
CN115216726A (zh) * 2022-08-24 2022-10-21 烟台佳隆纳米产业有限公司 高性能薄膜材料及其制备方法

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