CN112779493A - 一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法 - Google Patents

一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法 Download PDF

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CN112779493A
CN112779493A CN202010847279.2A CN202010847279A CN112779493A CN 112779493 A CN112779493 A CN 112779493A CN 202010847279 A CN202010847279 A CN 202010847279A CN 112779493 A CN112779493 A CN 112779493A
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杜建
董骐
田俊瑞
胡中军
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Beijing Danpu Surface Technology Co ltd
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    • 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
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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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    • 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
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    • 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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    • 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
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    • 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
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Abstract

本发明公开了一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，本发明采用气体离子源刻蚀清洗技术(Gas Ion Source Etching,GISETCH)和高功率脉冲磁控溅射技术(High Power Impulse MagnetronSputtering，HIPIMS)，在凹版印刷板表面镀制高质量的Cr+CrN涂层，用于取代原有的水电镀工艺。通过球坑测试、粗糙度测试、划痕试验、硬度测试、表面形貌观察等分析涂层各方面的性能后发现，GISETCH和HIPIMS技术制备的Cr+CrN涂层膜基结合力更强，其表面晶粒更细小，缺陷少，断面组织致密，经过实际印刷测试，耐印率超过水电镀水平。

Description

一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制 备方法
技术领域
本发明属于功能涂层技术领域，具体涉及一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法。
背景技术
凹版印刷以按原稿图文刻制的凹坑载墨，线条的粗细及油墨的浓淡层次在刻版时可以任意控制，不易被模仿和伪造，应用越来越广泛。传统凹版印刷版涂层采用电镀铜或铬等金属层来增加寿命。该电镀工艺污染严重，涂层表面不均匀。近年来利用物理气相沉积PVD技术制备涂层应用广泛，目前较成熟的微直流磁控溅射技术及电弧离子镀技术，但普通磁控溅射技术膜基之间结合力较差，涂层易剥落失效，电弧离子镀技术有高金属离化率和强膜基结合力的优点，但是在沉积过程中容易产生的大量宏观颗粒堆积，造成涂层表面粗糙，且涂层的内应力高，耐印率低。因此，开发一种高可性能凹版印刷版涂层制备工艺很有必要。
发明内容
本发明采用气体离子源刻蚀清洗技术(Gas Ion Source Etching,GISETCH)和高功率脉冲磁控溅射技术(High Power Impulse MagnetronSputtering，HIPIMS)，在凹版印刷板表面镀制高质量的Cr+CrN涂层，用于取代原有的水电镀工艺，膜基结合力更强，其表面晶粒更细小，缺陷少，断面组织致密，经过实际印刷测试，耐印率超过水电镀水平。
为实现上述目的，本发明提供如下技术方案：采用镍板为基底，将镍板表面清洗干燥，然后固定在镀膜机转架上，镀膜机抽真空后，设定一定的温度和偏压，通入一定量的氩气和氢气，通过气体离子源刻蚀清洗技术(Gas Ion Source Etching,GISETCH)，Ar原子和H原子在高电压下电离出Ar离子和H离子，Ar离子和H离子在偏压的作用下轰击和活化镍板，完成对镍板表面刻蚀清洗，然后在镀膜工艺下完成Cr+CrN复合涂层的制备。
作为本发明的一种优选技术方案，所述的基底为镍板，镍板装卡前用丙酮溶液和工业用无水乙醇试剂超声清洗15～20min，并在干燥箱内烘干。CrN涂层制备采用纯度超过99.9％的高纯Cr靶。
作为本发明的一种优选技术方案，所述的镀膜机有效镀膜空间为φ1100mm×1100mm，真空室内配备HIPIMS高能脉冲磁控电源。
作为本发明的一种优选技术方案，所述的气体离子源刻蚀清洗技术，包括转架转速设定为1-2r/min，开始沉积前抽真空至3.0*10-3Pa以下，沉积温度为150～180℃；真空室内通入纯Ar至腔体气压达到0.5pa，偏压调整为-400V，在偏压条件下利用Ar离子轰击镍板60-90min，完成镍板表面清洗。
作为本发明的一种优选技术方案，所述的镀膜工艺，具体为：先镀一层Cr作为打底层，然后以再镀制CrN层。打底层沉积时间控制为30～40min；沉积CrN层时通入氮气，氮气流量设定为30～40sccm，Highpulse靶溅射功率为10kW，基体偏压为-70～-90V。多层结构涂层采用以一层Cr以及一层CrN相互叠加的方式沉积，每一层沉积时间控制为8～10 min。
与现有技术相比，本发明的有益效果是：本发明采用气体离子源刻蚀清洗技术(Gas Ion Source Etching,GISETCH)和高功率脉冲磁控溅射技术(High Power ImpulseMagnetronSputtering，HIPIMS)，在凹版印刷板表面镀制高质量的Cr+CrN涂层，用于取代原有的水电镀工艺。Cr+CrN膜层更加致密，膜层光亮度和致密性比其他的磁控溅射技术更好。通过球坑测试、粗糙度测试、划痕试验、硬度测试、表面形貌观察等分析发现， GISETCH和HIPIMS技术制备的Cr+CrN涂层膜基结合力更强，其表面晶粒更细小，缺陷少，断面组织致密，经过实际印刷测试，耐印率远超过水电镀水平。
附图说明
图1为CrN涂层球磨仪球坑图；
图2为CrN涂层制备对比图；
图3为CrN涂层划痕轨迹图与划痕参数曲线图；
图4为其他工艺CrN涂层划痕轨迹图与划痕参数曲线图；
图5为沉积态CrN涂层表面微观组织照片；
图6为其他工艺沉积态CrN涂层表面微观组织照片
图7为沉积态CrN涂层断面微观组织照片；
具体实施方式
一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，其特征在于，具体步骤如下：采用镍板为基底，将镍板表面清洗干燥，然后固定在镀膜机转架上，镀膜机抽真空后，设定一定的温度和偏压，通入一定量的氩气和氢气，通过气体离子源刻蚀清洗技术(Gas Ion Source Etching,GISETCH)，Ar原子和H原子在高电压下电离出Ar离子和H离子，Ar离子和H离子在偏压的作用下轰击和活化镍板，完成对镍板表面刻蚀清洗，然后在镀膜工艺下完成Cr+CrN复合涂层的制备。
作为本发明的一种优选技术方案，所述的基底为镍板，镍板装卡前用丙酮溶液和工业用无水乙醇试剂超声清洗15～20min，并在干燥箱内烘干。CrN涂层制备采用纯度超过99.9％的高纯Cr靶。
作为本发明的一种优选技术方案，所述的镀膜机有效镀膜空间为φ1100mm×1100mm，真空室内配备HIPIMS高能脉冲磁控电源。
作为本发明的一种优选技术方案，所述的气体离子源刻蚀清洗技术，包括转架转速设定为1-2r/min，开始沉积前抽真空至3.0*10-3Pa以下，沉积温度为150～180℃；真空室内通入纯Ar至腔体气压达到0.5pa，偏压调整为-400V，在偏压条件下利用Ar离子轰击镍板60～90min，完成镍板表面清洗。
作为本发明的一种优选技术方案，所述的镀膜工艺，具体为：先镀一层Cr作为打底层，然后以再镀制CrN层。打底层沉积时间控制为30～40min；沉积CrN层时通入氮气，氮气流量设定为30～400sccm，Highpulse靶溅射功率为10kW，基体偏压为-70～-90V。多层结构涂层采用以一层Cr以及一层CrN相互叠加的方式沉积，每一层沉积时间控制为8～10 min。
作为本发明的一种优选技术方案，所述的镀膜工艺，具体为：先镀一层Cr作为打底层，然后以再镀制CrN层。打底层沉积时间控制为30～40min；沉积CrN层时通入氮气，氮气流量设定为30～40sccm，Highpulse靶溅射功率为10kW，基体偏压为-70～-90V。多层结构涂层采用以一层Cr以及一层CrN相互叠加的方式沉积，每一层沉积时间控制为8～10 min。
实施例1
图1采用球坑仪摩擦涂层，摩擦后在显微镜下观察涂层的多层涂层形貌。可以看出各层层次分明，环装结构基本为同心圆环，与图2的涂层制备方法相比，该工艺可制备涂层的层数多，层厚度均匀，过度层结合较好。
图3分别是ARC CrN、(H+B)CrN、图中基线上下波动的曲线为声发射信号曲线，基线上方的趋势线为摩擦系数曲线。摩擦系数曲线的突变区间表明金刚石压头从涂层划破到基体。如图在曲线上标定ARC CrN临界载荷33.5N，(H+B)CrN临界载荷72.2N，采用该方法沉积得到的涂层具有更好的膜基结合力。而图3中划痕边缘光滑平整，涂层与基体的结合更加紧密。图4的其他工艺对比图中划痕边缘出现细碎的涂层脱落块，涂层结合不好，脆硬易碎。
图5分别为扫描电镜下观察到的表面微观形貌。图6对比图中电弧离子镀沉涂层的表面存在大液滴，并带有针孔缺陷，本工艺条件下涂层的表面光滑，组织排列地十分紧密，虽然有少量针孔出现，但整体较均匀。断面图观察到多层涂层花样一层一层分布十分明显。
图7涂层断面(本工艺)可以看到有细碎的柱状晶被紧紧压在一起，组织更加细小。
上述实施例均为本发明较佳实例，凡是依据本发明的技术实质对以上实施所做的任何简单修饰、等同变化与修饰、均落入本发明的保护范围内。

Claims (5)

1.一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，其特征在于，具体步骤如下：采用镍板为基底，将镍板表面清洗干燥，然后固定在镀膜机转架上，镀膜机抽真空后，设定一定的温度和偏压，通入一定量的氩气和氢气，通过气体离子源刻蚀清洗技术(Gas Ion Source Etching,GISETCH)，Ar原子和H原子在高电压下电离出Ar离子和H离子，Ar离子和H离子在偏压的作用下轰击和活化镍板，完成对镍板表面刻蚀清洗，然后在镀膜工艺下完成Cr+CrN复合涂层的制备。
2.根据权利要求1所述的一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，其特征在于：所述的基底为镍板，镍板装卡前用丙酮溶液和工业用无水乙醇试剂超声清洗15～20min，并在干燥箱内烘干。Cr+CrN涂层制备采用纯度超过99.9％的高纯Cr
靶。
3.根据权利要求1所述的一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，其特征在于：所述的镀膜机有效镀膜空间为φ1100mm×1100mm，真空室内配备HIPIMS高能脉冲磁控电源。
4.根据权利要求1所述的一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，其特征在于：所述的气体离子源刻蚀清洗技术，包括转架转速设定为1-2r/min，开始沉积前抽真空至3.0*10-3Pa以下，沉积温度为150～180℃；真空室内通入纯Ar至腔体气压达到0.5pa，偏压调整为-400V，在偏压条件下利用Ar离子轰击镍板60-90min，完成镍板表面清洗。
5.根据权利要求1所述的一种基于GIS和HIPIMS技术的用于凹版印刷板表面CrN涂层制备方法，其特征在于：所述的镀膜工艺，具体为：先镀一层Cr作为打底层，然后以再镀制CrN层。打底层沉积时间控制为30～40min；沉积CrN层时通入氮气，氮气流量设定为30～40sccm，Highpulse靶溅射功率为10kW，基体偏压为-70～-90V。多层结构涂层采用以一层Cr以及一层CrN相互叠加的方式沉积，每一层沉积时间控制为8～10min。
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