CN108543687A - 一种高延展性周期变量合金保护膜及形成方法 - Google Patents

一种高延展性周期变量合金保护膜及形成方法 Download PDF

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CN108543687A
CN108543687A CN201810232390.3A CN201810232390A CN108543687A CN 108543687 A CN108543687 A CN 108543687A CN 201810232390 A CN201810232390 A CN 201810232390A CN 108543687 A CN108543687 A CN 108543687A
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coating
periodic variable
protecting film
powder
alloy protecting
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王再德
马焕明
张胜超
李帅
魏庆旺
李传明
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CITIC Dicastal Co Ltd
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CITIC Dicastal Co Ltd
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Priority to US16/223,320 priority patent/US11072853B2/en
Priority to EP19162979.9A priority patent/EP3542911A1/en
Priority to MA046407A priority patent/MA46407A/fr
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Abstract

本发明公开了一种高延展性周期变量合金保护膜，依次包括：金属或非金属基底、高光有机树脂涂膜、高延展性周期变量合金膜和透明树脂膜。本发明同时提供了一种高延展性周期变量合金保护膜的形成方法。本发明能提高镀膜和表面透明涂层结合力和结合力耐久性问题；形成金属铬光亮的颜色外观，涂层系统具备良好的耐腐蚀性能。

Description

一种高延展性周期变量合金保护膜及形成方法
技术领域
本发明涉及周期合金保护膜表面处理领域，具体地涉及一种高真空直流磁控溅镀周期变量合金保护膜及形成该合金保护膜的方法。
背景技术
目前，物理汽相淀积法（PVD）进行的表面处理方式主要包括蒸镀、等离子多弧溅射、高真空直流磁控溅射。其中高真空直流磁控溅射可以利用到汽车零部件制造业，包括汽车车标、汽车轮毂盖帽、汽车轮毂等零部件表面处理及装饰。其特点是使零部件表面达到金属白亮镜面光泽装饰效果，美观大方，而且涂层性能可以达到汽车厂标准，与传统喷涂底粉+色漆+透明漆相比，涂层性能相当，外观可以达到电镀效果。
高真空直流磁控溅射是在真空室，把工作气体电离，电离后的离子在电场和磁场混合场作用下高速撞击到金属靶上，靶材上的金属原子或离子飞溅出来，再沉积溅射到工件表面上的方法。此方法可以得到光亮镜面的金属外观新效果，绿色环保、前景广阔。单一金属或单一合金的高真空直流磁控溅射膜必须要达到主机厂涂层耐腐蚀标准，需要选择惰性金属或合金，耐腐蚀性强。溅射膜与上下结合有机涂层达到良好的集合，再进行涂层固化时候热胀冷缩，镀膜的延展性要满足要求，否则会出现龟裂，外观不能满足要求。
发明内容
因此，本发明的目的是提供一种高延展性周期变量合金保护膜及形成该合金保护膜的方法。
一种高延展性周期变量合金保护膜，依次包括：金属或非金属基底、高光有机树脂涂膜、高延展性周期变量合金膜和透明树脂膜。所述的高光有机树脂涂膜可以是环氧树脂涂层、丙烯酸树脂涂层、纯聚酯涂层、聚丁二烯涂层；所述的高延展性周期变量合金保护膜在高真空环境下直流磁控溅射形成，溅射靶材的材料是由NiCr合金层和纯Cr组成；透明树脂膜是纯丙烯酸树脂涂层。
所述的高延展性周期变量合金保护膜由Ni、Cr两种金属元素组成，Ni金属成分80%-0；Cr金属成分20%-100%，循环渐变，其中每种金属元素含量随镀膜的厚度不同，所含百分比不同，本发明的高延展性周期变量合金保护膜从表层到底部周期性变化的合金膜。
所述的高光有机树脂涂膜的厚度是100～300μm。
所述的Ni、Cr高延展性周期变量合金保护膜为0.100～0.800μm。
所述的丙烯酸层的厚度是80-150μm。
本发明还公开了一种形成高延展性周期变量合金保护膜方法，包括步骤为：
（1）、铝合金或其他金属表面进行预处理，所述的预处理步骤包括水洗+碱洗+水洗+酸洗+纯水洗+钝化+纯水洗+封闭+纯水洗+烘干。
（2）、在金属表面上喷底粉并且进行固化，所述的底粉是环氧树脂粉末或纯聚酯粉末涂料。
（3）、在步骤（2）的表面上进行精细打磨，抛光。
（4）、在步骤（3）的表面上进行清洗，所述的步骤包括水洗+碱洗+水洗+酸洗+纯水洗+纯水洗+烘干。
（5）、在步骤（4）的表面上喷高光、高流平树脂粉末涂料或者溶剂型液体漆；并且进行固化，所述的底漆是环氧树脂粉末、聚酯粉末涂料或聚丁二烯液体涂料。
（6）、在步骤（5）的表面上进行高真空直流磁控溅镀，所述的溅镀包括NiCr合金靶材和纯Cr金属靶材同时开启，自传、公转同时进行，达到周期变量合金保护膜。
（7）、在步骤（6）的表面上喷透明粉并且进行固化，所述的透明粉是丙烯酸树脂或者聚酯粉末涂料。
在步骤（2）中，底层喷粉厚度是100～300μm，轮毂表面固化温度是190℃，固化时间是20min。
在步骤（3）中，所述的精细打磨步骤是使用800/1000目的砂纸进行打磨，打磨表面缺陷和不平，并且不能露出金属基体。
在步骤（5）中，高光有机涂层厚度是80～120μm，轮辐表面固化温度是220℃，固化时间是20min。
在步骤（6）中，镀膜工件温度为80～150℃，气体流量为40～80cc/min，镀膜直流电流为20～30A，直流电压≤800v；真空度为2～8*10-3Pa，双靶材镀膜时间为15～40s，所述的工作气体为99.999%氩气，镀膜环境湿度为≤50%。
在步骤（7）中，透明粉厚度是80～150μm，轮毂表面固化温度是175℃，固化时间是20min。
本发明的高延展性周期变量合金保护膜和方法的优点在于：（1）改善沉积金属层的应力残留，解决溅镀合金稳定性，提高镀膜延展性，避免镀膜快速加热、快速冷却时龟裂问题；（2）提高金属镀膜与底层高光树脂材料结合力问题；（3）提高镀膜和表面透明涂层结合力和结合力耐久性问题；（4）形成金属铬光亮的颜色外观，起到了装饰作用；（5）涂层系统具备良好的耐腐蚀性能。原PVD铬镀层由于金属单一，金属物理性质脆性高，与有机涂层结合后聚冷聚热产生龟裂，影响与有机涂层之间的结合力。采用这种新的周期变量合金工艺后，基本上解决了以上问题。本发明的技术方案还可以应用于其他用途，比如笔记本外壳、汽车内饰件、卫浴管件等。
具体实施方式
除非另外地说明，本发明的实施例中采用两种靶材，一种是NiCr合金中Ni的质量百分比为60%-80%，Cr的质量百分比为20%-80%；另一种是纯Cr，Cr金属纯度为99.99%。PVD设备为高真空磁控溅射镀膜机。
溅镀基材采用A356.2铝合金；底粉为纯聚酯粉末涂料；高光粉末涂料为纯环氧树脂涂料；透明涂层为纯丙烯酸透明粉末涂料；
涂层按照美国通用汽车轮毂涂装性能标准进行检查，检查项目包括：百格附着力、CASS、FLIFORM、NASS、贴带试验、耐高湿度试验、耐砾石冲击、耐热冲击试验、耐油试验、耐清洗剂试验、耐老化等。
形成延展性周期变量合金保护膜的方法，所述方法包括：
（1）提供铝合金或其他金属表面进行预处理；预处理包括：水洗+碱洗+水洗+酸洗+纯水洗+钝化+纯水洗+封闭+纯水洗+烘干。
（2）在步骤（1）的金属表面上喷底粉并且进行固化，所述的底粉是环氧树脂粉末或纯聚酯粉末涂料。
（3）在步骤（2）的表面上进行精细打磨，抛光。
（4）在步骤（3）的表面上进行清洗，所述的清洗步骤包括水洗+碱洗+水洗+酸洗+纯水洗+纯水洗+烘干。
（5）在步骤（4）的表面上喷涂高光、高流平树脂粉末涂料或者溶剂型液体漆；并且进行固化，所述的底漆是环氧树脂粉末、聚酯粉末涂料或聚丁二烯液体涂料。
（6）在步骤（5）的表面上进行高真空直流磁控溅镀，所述的溅镀包括NiCr合金靶材和纯Cr金属靶材同时开启，自传、公转同时进行，达到周期变量合金保护膜。
（7）在步骤（6）的表面上喷透明粉并且进行固化，所述的透明粉是丙烯酸树脂或者聚酯粉末涂料。
在步骤（2）中，喷粉厚度是100-300μm，固化温度工件表面达到180℃，固化时间是20min。
在步骤（3）中，所述的精细打磨步骤是使用800/1000目的砂纸进行打磨抛光。
在步骤（5）中，底漆厚度是80-120μm，固化温度工件表面达到是215℃，固化时间是20min。
在步骤（6）中，镀膜工件温度为80～150℃，气体流量为40～80cc/min，镀膜直流电流为20～30A，直流电源电压≤800v；真空度为2～8*10-3Pa，双靶材镀膜时间为15～80s，所述的工作气体为99.999%氩气，镀膜环境湿度为≤50%。
在步骤（7）中，透明粉厚度是80～150μm，固化温度工件表面是180℃，固化时间是17min。
对比例1：使用本领域一般采用的方法来制备PVD保护层。采用靶材为纯Cr单靶。采用的工艺方法和涂层结构与本发明的制备方法相同。
对比例2：使用本领域一般采用的方法来制备PVD保护层。采用靶材为NiCr合金单靶。采用的工艺方法和涂层结构与本发明的制备方法相同。
采用实施例1与比例1、2金属表面延展性周期高真空磁控溅镀层进行了以下的检测和对比，见下表：
组 实施例1 对比例1 对比例2
表面龟裂 无 密集龟裂 有龟裂
百格法附着力 100%无脱落 93%无脱落 92%无脱落
贴带试验 100%无脱落 95%无脱落 92%无脱落
CASS 2.0㎜ 3.1㎜ 6.1㎜
FLIFORM 3.3㎜ 4.1㎜ 4.8㎜
NASS 1.8㎜ 2.2㎜ 5.2㎜
耐水试验 无变化，附着力100%无脱落 无变化，附着力85%无脱落 无变化，附着力67%无脱落
耐砾石冲击 优于8级 8级 8级
耐热冲击 无脱落 10%脱落 13%脱落
耐油试验 无变化 无变化 无变化
耐清洗剂 无变化 无变化 无变化
耐老化 无变化，附着力100%无脱落 无变化，附着力91%无脱落 无变化，附着力90%无脱落
由此可见，本发明的方法中，镀膜温度、氩气流量、镀膜电流、真空度、NiCr合金靶材和纯Cr镀膜时间为关键参数。通过优化以上的工艺，得到了性能良好的PVD镀膜。本发明中，实施例的技术方案通过摸索以上的条件得到了最佳的条件。在该最佳的条件下涂层检测实验结果最好。

Claims (8)

1.一种高延展性周期变量合金保护膜，其特征在于：依次包括：有机粉末涂层、高光有机涂层、延展性周期变量合金保护膜和透明粉涂层；所述的底粉层是环氧树脂或纯聚酯粉末涂料涂层；所述的高光有机涂层是是环氧树脂粉末涂层、聚酯粉末涂层、聚丁二烯有机涂层；所述的延展性周期变量合金保护膜由两个靶材同时开启溅射，在高真空环境下直流磁控溅射形成，溅射靶材的材料是由Ni-Cr合金层和纯Cr组成；所述的透明粉层是丙烯酸粉末涂层或聚酯透明粉末涂层。
2.根据权利要求1所述的一种高延展性周期变量合金保护膜，其特征在于：所述保护膜的Ni百分含量变化范围0-85%；Cr金属含量变化为15%-100%。
3.根据权利要求1所述的所述的一种高延展性周期变量合金保护膜，其特征在于：所述的底粉层的厚度是100～300μm；所述的底漆层的厚度是80～120μm；所述的丙烯酸层的厚度是80-150μm；所述的NiCr合金层和Cr金属层的厚度均为0.1～0.8μm。
4.一种形成高延展性周期变量合金保护膜的方法，其特征在于：所述的方法包括步骤：（1）提供铝合金或其他金属表面进行预处理；所述的预处理步骤包括水洗+碱洗+水洗+酸洗+纯水洗+钝化+纯水洗+封闭+纯水洗+烘干；
（2）在步骤（1）的金属表面上喷底粉并且进行固化，所述的底粉是环氧树脂粉末或纯聚酯粉末涂料；
（3）在步骤（2）的表面上进行精细打磨，抛光；
（4）在步骤（3）的表面上进行清洗，所述的预处理步骤包括水洗+碱洗+水洗+酸洗+纯水洗+纯水洗+烘干；
（5）在步骤（4）的表面上喷高光、高流平树脂粉末涂料或者溶剂型液体漆，并且进行固化，所述的底漆是环氧树脂粉末、聚酯粉末涂料或聚丁二烯液体涂料；
（6）在步骤（5）的表面上进行高真空直流磁控溅镀，所述的溅镀靶材材料包括NiCr合金靶材和纯Cr金属靶同时开启，自传、公转同步进行，达到周期变量合金保护膜；
（7）在步骤（6）的表面上喷透明粉并且进行固化，所述的透明粉是丙烯酸树脂或者聚酯粉末涂料；
在步骤（6）中，镀膜工件温度为80～140℃，气体流量为40～80cc/min，镀膜直流电流为20～30A，直流电源电压≤800v；真空度为2～8*10-3Pa，双靶材镀膜时间为15～80s，所述的工作气体为99.999%氩气，镀膜环境湿度为≤50%。
5.根据权利要求4所述的一种形成高延展性周期变量合金保护膜的方法，其特征在于：在步骤（2）中，喷粉厚度是100-300μm，固化温度工件表面达到180℃，固化时间是20min。
6.根据权利要求4所述的一种形成高延展性周期变量合金保护膜的方法，其特征在于：在步骤（3）中，所述的精细打磨步骤是使用800/1000目的砂纸进行打磨抛光。
7.根据权利要求4所述的一种形成高延展性周期变量合金保护膜的方法，其特征在于：在步骤（5）中，底漆厚度是80-120μm，固化温度工件表面达到是215℃，固化时间是20min。
8.根据权利要求4所述的一种形成高延展性周期变量合金保护膜的方法，其特征在于：在步骤（7）中，透明粉厚度是80～150μm，固化温度工件表面是180℃，固化时间是17min。
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Application publication date: 20180918