CN109487214A - 一种镁合金表面镀膜方法及由其制备的抗腐蚀镁合金 - Google Patents

一种镁合金表面镀膜方法及由其制备的抗腐蚀镁合金 Download PDF

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CN109487214A
CN109487214A CN201811570475.9A CN201811570475A CN109487214A CN 109487214 A CN109487214 A CN 109487214A CN 201811570475 A CN201811570475 A CN 201811570475A CN 109487214 A CN109487214 A CN 109487214A
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magnesium
film
alloy
magnesium alloy
corrosion
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蒋贵霞
贾建国
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Kunshan Yingli Yue Electronics Co Ltd
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Abstract

本发明公开了一种镁合金表面镀膜方法以及由该方法制备的抗腐蚀镁合金。所述方法包括以下步骤：对镁合金基材进行前处理；在经过前处理的镁合金基材表面上溅射沉积金属薄膜；在沉积金属薄膜的镁合金基材表面上溅射沉积Si3N4薄膜。所述金属为选自Nb、Cr、Ta中的任一种。本发明的方法能够对镁合金提供有效的保护，提高了镁合金的抗腐蚀性能。

Description

一种镁合金表面镀膜方法及由其制备的抗腐蚀镁合金
技术领域
本发明涉及一种镁合金表面镀膜方法以及由该方法制备的抗腐蚀镁合金，属于金属表面处理技术领域。
背景技术
镁合金是最轻的金属结构材料，被誉为新一代绿色工程材料，但由于其抗腐蚀性能较差，使其应用受到很大限制。目前，提高镁合金抗腐蚀性能的最行之有效的方法之一是采用适当的表面处理技术在镁合金表面形成一层防护性的膜层。镁合金防护的表面处理技术主要有化学转化膜、气相沉积、电化学镀、阳极氧化及微弧氧化等。其中化学转化膜、电化学镀、阳极氧化及微弧氧化等方法工艺复杂，膜基结合不好，还存在着能耗高、环境污染问题。在气相沉积中，磁控溅射镀膜是一种比较重要的物理气相沉积镀膜技术，具有沉积温度低、工艺简薄膜质量好、对环境友好等优点，已成为薄膜工业化应用的主要方法。尽管国内外已有了一些利用气相沉积对镁合金进行表面改性的方法以提高镁合金的耐腐蚀和耐磨性能，但仍然存在膜基结合不好、表面有空隙、裂纹等缺陷，抗腐蚀效果仍然不够理想。
发明内容
本发明的目的在于提供一种镁合金表面镀膜方法，其能够使镁合金具有优良的抗腐蚀性能。
本发明的另一目的在于提供一种抗腐蚀镁合金，其具有优良的抗腐蚀性能。
为达到上述目的，本发明提供了一种镁合金表面镀膜方法，所述方法包括以下步骤：
对镁合金基材进行前处理；
在经过前处理的镁合金基材表面上溅射沉积金属薄膜；
在沉积金属薄膜的镁合金基材表面上溅射沉积Si3N4薄膜。
进一步，所述金属为选自Nb、Cr、Ta中的任一种。
进一步，所述金属薄膜的厚度为1µm。
进一步，所述Si3N4薄膜的厚度为2µm。
进一步，所述镁合金表面镀膜方法还包括：在沉积金属薄膜前使用离子源清除镁合金基材表面的气体吸附物。
进一步，所述镁合金表面镀膜方法还包括：沉积Si3N4薄膜时保持溅射室腔体温度为100℃，镁合金基材温度为250℃。
本发明还提供了一种抗腐蚀镁合金，包括镁合金基材、沉积在镁合金基材上的金属薄膜以及沉积在金属薄膜上的Si3N4薄膜。
进一步，所述金属为选自Nb、Cr、Ta中的任一种。
进一步，所述金属薄膜的厚度为1µm。
进一步，所述金属薄膜的厚度为2µm。
与现有技术相比，本发明所达到的有益技术效果为：本发明提供的镁合金表面镀膜方法沉积的Si3N4薄膜表面光滑、致密，作为外层保护层能够有效地降低镁合金的腐蚀速率，同时在镁合金表面先溅射沉积金属过渡层，该金属过渡层能够增加Si3N4薄膜与镁合金间的附着力，使得膜基结合较好，从而使镁合金具有优良的抗腐蚀性能；另外，Nb、Ta、Cr金属过渡层本身还能够发生钝化形成钝化膜，进一步提高了镁合金的抗腐蚀性能。
具体实施方式
下面结合具体实施例对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
一、薄膜制备
本发明实施例选用AZ31镁合金作为沉积基材，设备使用K08030刀具改性多弧与磁控溅射镀膜系统（中国科学院沈阳科学仪器研制中心），溅射靶材分别采用99.99%硅和金属Nb、Ta 、Cr，溅射气体分别为Ar气和N2气。
实施例1：
将镁合金基材表面反复进行打磨和抛光处理至表面粗糙度在0.5µm以下，置于无水乙醇中超声波清洗10min，然后置于丙酮中超声波清洗15min，烘干；
将烘干后的镁合金基材固定在溅射室的样品转台上，启动真空系统抽真空直至本底真空为6×10-4Pa，同时辅助加热以除去水汽；
通入Ar气，调节气体流量使得溅射室内气压为0.3Pa，启动霍尔离子源，用Ar+轰击镁合金基材表面，除去基材表面的气体吸附物，提高沉积薄膜在基材上的附着力；
气体吸附物清除结束后，调节Ar气通入量使得溅射室内气压为1Pa，溅射功率为150W；
开启电源，直流溅射Nb靶材，控制溅射时间使得Nb薄膜的膜厚达到1µm左右后，关闭电源；
通入N2气，控制Ar和N2的总流量为50sccm（N2流量约占总流量的10%），溅射室内气压为1Pa，基材偏压为0V，溅射功率为250W；
加热溅射室腔体至温度为100℃，并加热镁合金基材至温度为250℃，保持恒温；
开启电源，射频溅射Si靶材，控制溅射时间使得沉积的Si3N4薄膜的膜厚达到2µm左右；
沉积结束后，关闭电源、氮气阀门，在Ar气流中冷却，当溅射室温度降至室温后，关闭真空系统，获得镀有Nb/Si3N4复合薄膜的镁合金基材。
实施例2：
将镁合金基材表面反复进行打磨和抛光处理至表面粗糙度在0.5µm以下，置于无水乙醇中超声波清洗10min，然后置于丙酮中超声波清洗15min，烘干；
将烘干后的镁合金基材固定在溅射室的样品转台上，启动真空系统抽真空直至本底真空为6×10-4Pa，同时辅助加热以除去水汽；
通入Ar气，调节气体流量使得溅射室内气压为0.3Pa，启动霍尔离子源，用Ar+轰击镁合金基材表面，除去基材表面的气体吸附物，提高沉积薄膜在基材上的附着力；
气体吸附物清除结束后，调节Ar气通入量使得溅射室内气压为1Pa，溅射功率为150W；
开启电源，直流溅射Cr靶材，控制溅射时间使得Cr薄膜的膜厚达到1µm左右后，关闭电源；
通入N2气，控制Ar和N2的总流量为60sccm（N2流量约占总流量的15%）、溅射室内气压为1Pa，基材偏压为0V，溅射功率为250W；
加热溅射室腔体至温度为100℃，并加热镁合金基材至温度为250℃，保持恒温；
开启电源，射频溅射Si靶材，控制溅射时间使得沉积的Si3N4薄膜的膜厚达到2µm左右；
沉积结束后，关闭电源、氮气阀门，在Ar气流中冷却，当沉积室温度降至室温后，关闭真空系统，获得镀有Cr/Si3N4复合薄膜的镁合金基材。
实施例3：
将镁合金基材表面反复进行打磨和抛光处理至表面粗糙度在0.5µm以下，置于无水乙醇中超声波清洗10min，然后置于丙酮中超声波清洗15min，烘干；
将烘干后的镁合金基材固定在溅射室的样品转台上，启动真空系统抽真空直至本底真空为6×10-4Pa，同时辅助加热以除去水汽；
通入Ar气，调节气体流量使得溅射室内气压为0.3Pa，启动霍尔离子源，用Ar+轰击镁合金基材表面，除去基材表面的气体吸附物，提高沉积薄膜在基材上的附着力；
气体吸附物清除结束后，调节Ar气通入量使得溅射室内气压为1Pa，溅射功率为150W；
开启电源，直流溅射Ta靶材，控制溅射时间使得Ta薄膜的膜厚达到1µm左右后，关闭电源；
通入N2气，控制Ar和N2的总流量为60sccm（N2流量约占总流量的15%）、溅射室内气压为1Pa，基材偏压为0V，溅射功率为250W；
加热溅射室腔体至温度为100℃，并加热镁合金基材至温度为250℃，保持恒温；
开启电源，射频溅射Si靶材，控制溅射时间使得沉积的Si3N4薄膜的膜厚达到2µm左右；
沉积结束后，关闭电源及氮气阀门，在Ar气流中冷却，沉积室温度降至室温后，关闭真空系统，获得镀有Ta/Si3N4复合薄膜的镁合金基材。
二、中性盐雾试验
1. 将空白镁合金、镀有Nb/Si3N4的镁合金基材置于盐雾试验箱一周，结果表明，空白镁合金被严重腐蚀，腐蚀面积高于50%，而镀有Nb/ Si3N4的镁合金基材基本完好，腐蚀面积约在5%左右。
2. 将空白镁合金、镀有Cr/Si3N4的镁合金基材置于盐雾试验箱一周，结果表明，空白镁合金被严重腐蚀，腐蚀面积高于50%，而镀有Nb/ Si3N4的镁合金基材基本完好，腐蚀面积约在6%左右。
3. 将空白镁合金、镀有Ta/Si3N4的镁合金基材置于盐雾试验箱100h，结果表明，空白镁合金被严重腐蚀，腐蚀面积高于50%，而镀有Nb/ Si3N4的镁合金基材基本完好，腐蚀面积约在5%左右。
以上结果表明：在镁合金上沉积Nb/ Si3N4、Cr/ Si3N4和Ta/ Si3N4复合薄膜能够对镁合金提供有效的保护，提升了镁合金的耐腐蚀性能。
以上已以较佳实施例公布了本发明，然其并非用以限制本发明，凡采取等同替换或等效变换的方案所获得的技术方案，均落在本发明的保护范围内。

Claims (10)

1.一种镁合金表面镀膜方法，其特征在于，所述方法包括以下步骤：
对镁合金基材进行前处理；
在经过前处理的镁合金基材表面上溅射沉积金属薄膜；
在沉积金属薄膜的镁合金基材表面上溅射沉积Si3N4薄膜。
2.根据权利要求1所述的镁合金表面镀膜方法，其特征在于，所述金属为选自Nb、Cr、Ta中的任一种。
3.根据权利要求1所述的镁合金表面镀膜方法，其特征在于，所述金属薄膜的厚度为1µm。
4.根据权利要求1所述的镁合金表面镀膜方法，其特征在于，所述Si3N4薄膜的厚度为2µm。
5.根据权利要求1所述的镁合金表面镀膜方法，其特征在于，所述方法还包括：在沉积金属薄膜前使用离子源清除镁合金基材表面的气体吸附物。
6.根据权利要求1所述的镁合金表面镀膜方法，其特征在于，所述方法还包括：沉积Si3N4薄膜时保持溅射室腔体温度为100℃，镁合金基材温度为250℃。
7.一种抗腐蚀镁合金，其特征在于，包括镁合金基材、沉积在镁合金基材上的金属薄膜以及沉积在金属薄膜上的Si3N4薄膜。
8.根据权利要求7所述的抗腐蚀镁合金，其特征在于，所述金属为选自Nb、Cr、Ta中的任一种。
9.根据权利要求7所述的抗腐蚀镁合金，其特征在于，所述金属薄膜的厚度为1µm。
10.根据权利要求7所述的抗腐蚀镁合金，其特征在于，所述金属薄膜的厚度为2µm。
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