CN107829074B - 一种非晶合金反光镜及其制备方法 - Google Patents

一种非晶合金反光镜及其制备方法 Download PDF

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CN107829074B
CN107829074B CN201711048989.3A CN201711048989A CN107829074B CN 107829074 B CN107829074 B CN 107829074B CN 201711048989 A CN201711048989 A CN 201711048989A CN 107829074 B CN107829074 B CN 107829074B
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覃广生
许积文
薛云飞
王本鹏
付华萌
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Guilin University of Electronic Technology
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Abstract

本发明公开了一种非晶合金反光镜及其制备方法，所述反光镜包括基板、涂覆在基板上的Zr‑Ti‑Cu‑Ni‑Al‑Ag‑Re非晶涂层以及基板与非晶涂层之间的过渡层。所述非晶合金反光镜的制备方法主要包括：（1）以Ti、Ni、Cr或Al为靶材，在基板上制备过渡层；（2）以所述涂层材料为靶材，在过渡层上溅射非晶合金反光涂层。本发明公开的反光涂层材料不仅具有高的反射率，而且硬度高、耐磨、耐腐蚀、抗氧化、抗硫化，用其制造反光镜，表面无需保护层，制造成本也低于纯银及银合金反光镜，适合于各种场合尤其适合在沙漠、高寒等恶劣环境下使用。

Description

一种非晶合金反光镜及其制备方法
技术领域
本发明涉及反光涂层材料技术领域，具体涉及一种非晶合金反光镜及其制备方法。
背景技术
利用银的高反射率，可以通过真空镀膜或者化学还原反应制造银反光镜。虽然银反光镜具有较高的反射率，但银反射层存在价格贵，硬度低，抗氧化、硫化能力及耐腐蚀能力不强。通过在银反射层表面涂覆保护层来提高银层的物理、化学性能，是一种有效的改善方式，如中国专利CN102419459B采用的聚氨酯保护层以及中国专利CN101776778B采用的SiOx保护层。
发明内容
本发明提供一种非晶态反光涂层材料，用以取代传统的银及银合金，解决现有技术中存在的缺陷。本发明同时还提供了一种非晶合金反光镜及其制备方法。本发明提供的反光涂层材料不仅具有高的反射率，而且硬度高、耐磨、耐腐蚀、抗氧化、抗硫化，用其制造非晶态合金反光镜，表面无需保护层，制造成本也低于纯银及银合金反光镜，适合于各种场合尤其适合在沙漠、高寒等恶劣环境下使用。
本发明提供的非晶反光涂层材料，是一种Zr基非晶合金体系，其组成为Zr-Ti-Cu-Ni-Al-Ag-RE，按原子百分比计：48-58％的Zr，0-2％的Ti,27-34％的Cu，3-8％的Ni，6-12％的Al，0.05-2％的Ag，0.1-2％的RE；RE表示稀土元素，为Y、Er、Sc或其组合，实际中将按照公知的相应公式折算重量配比。将上述材料应用现有工艺涂覆在不锈钢、玻璃、陶瓷、亚克力(PMMA)、聚酰亚胺(PET)或聚碳酸酯(PC)基板上，即可制得非晶态合金反光镜。在基板和反光涂层之间设置一层以Ti、Ni、Cr或Al为靶材，采用磁控溅射或蒸发方式制备的过渡层，能取得更好的技术效果。
具体实施方式
非晶态合金反光镜的制造方法，包括如下步骤：
(1)制备Zr-Ti-Cu-Ni-Al-Ag-RE合金非晶靶材，其中各元素原子百分比：48-58％的Zr，0-2％的Ti,27-34％的Cu，3-8％的Ni，6-12％的Al，0.05-2％的Ag，0.1-2％的RE；稀土元素RE可以是Y、Er、Sc或其组合。
(2)采用超声方式清洗基板，并进行紫外臭氧表面处理；基板材料可以是不锈钢、玻璃、陶瓷、亚克力(PMMA)、聚酰亚胺(PET)或聚碳酸酯(PC)。
(3)以金属Ti、Ni、Cr或Al为靶材，采用磁控溅射或蒸发方式在基板上制备过渡层，过渡层厚度可以为10-28nm，基板温度可以为25-800℃。
(4)以步骤1制得的Zr-Ti-Cu-Ni-Al-Ag-RE非晶合金为靶材，采用磁控溅射或蒸发方式在过渡层上制备非晶层反光涂层，反光涂层的厚度可以为400nm到5000nm，基板温度可以为25-400℃。
下面给出的是具体的实施例。
实施例1：
采用丙酮、酒精、纯水超声清洗玻璃基板，采用直径60mm的Ti靶材在玻璃基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Y非晶合金靶材(其中的原子百分比：58％Zr，27％Cu，3％Ni，11.85％Al，0.05％Ag，0.1％Y)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为80W、氩气压强为0.6Pa、基板温度为室温，过渡层和非晶层的厚度分别约为10nm和400nm。反光镜的硬度为12GPa，反射率为0.86，耐刮擦次数为30次，盐雾测试(盐雾浓度为5％，温度为35℃，湿度为60％)大于500h。
实施例2：
采用丙酮、酒精、纯水超声清洗不锈钢基板，采用直径60mm的Ni靶材在不锈钢基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Er非晶合金靶材(其中的原子百分比：58％Zr，27％Cu，3％Ni，11.85％Al，0.05％Ag，0.1％Er)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为80W、氩气压强为0.6Pa、基板温度为室温，过渡层和非晶层的厚度分别约为20nm和1000nm。反光镜的硬度为14GPa，反射率为0.89，耐刮擦次数为82次，盐雾测试大于800h。
实施例3：
采用丙酮、酒精、纯水超声清洗抛光氧化铝基板，采用直径60mm的Cr靶材在氧化铝基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Sc非晶合金靶材(其中的原子百分比：58％Zr，27％Cu，3％Ni，11.85％Al，0.05％Ag，0.1％Sc)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为80W、氩气压强为0.6Pa、基板温度为室温，过渡层和非晶层的厚度分别约为28nm和5000nm。反光镜的硬度为15GPa，反射率为0.91，耐刮擦次数160次，盐雾测试大于1200h。
实施例4：
采用丙酮、酒精、纯水超声清洗抛光亚克力基板，采用直径60mm的Al靶材在亚克力基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Y-Er非晶合金靶材(其中的原子百分比：58％Zr，27％Cu，3％Ni，11.85％Al，0.05％Ag，0.05％Y，0.05％Er)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为80W、氩气压强为0.6Pa、基板温度为室温，过渡层和非晶层的厚度分别约为10nm和400nm。反光镜的硬度为10GPa，反射率为0.86，耐刮擦次数为31次，盐雾测试大于500h。
实施例5：
采用丙酮、酒精、纯水超声清洗抛光玻璃基板，采用直径60mm的Cr靶材在玻璃基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Y-Sc非晶合金靶材(其中的原子百分比：58％Zr，27％Cu，3％Ni，11.85％Al，0.05％Ag，0.05％Y，0.05％Sc)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为80W、氩气压强为0.02Pa、基板温度为室温，过渡层和非晶层的厚度分别约为10nm和400nm。反光镜的硬度为13GPa，反射率为0.88，耐刮擦次数为42次，盐雾测试大于500h。
实施例6：
采用丙酮、酒精、纯水超声清洗抛光玻璃基板，采用直径60mm的Cr靶材在玻璃基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Er-Sc非晶合金靶材(其中的原子百分比：58％Zr，27％Cu，3％Ni，11.85％Al，0.05％Ag，0.05％Er，0.05％Sc)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为80W、氩气压强为0.02Pa、基板温度400℃，过渡层和非晶层的厚度分别约为10nm和400nm。反光镜的硬度为13GPa，反射率为0.89，耐刮擦次数为45次，盐雾测试大于500h。
实施例7：
采用丙酮、酒精、纯水超声清洗抛光玻璃基板，采用直径60mm的Ti靶材在玻璃基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Er非晶合金靶材(其中的原子百分比：48％Zr，34％Cu，8％Ni，8％Al，1％Ag，1％Er)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为100W、氩气压强为0.5Pa、基板温度为300℃，过渡层和非晶层的厚度分别约为12nm和500nm。反光镜的硬度为12GPa，反射率为0.87，耐刮擦次数为50次，盐雾测试大于800h。
实施例8：
采用丙酮、酒精、纯水超声清洗抛光陶瓷基板，采用直径60mm的Ti靶材在陶瓷基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Y非晶合金靶材(其中的原子百分比：48％Zr，34％Cu，8％Ni，6％Al，2％Ag，2％Y)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为100W、氩气压强为0.5Pa、基板温度为300℃，过渡层和非晶层的厚度分别约为12nm和500nm。反光镜的硬度为15GPa，反射率为0.89，耐刮擦次数为110次，盐雾测试大于800h。
实施例9：
采用丙酮、酒精、纯水超声清洗抛光聚碳酸酯基板，采用直径60mm的Ni靶材在聚碳酸酯基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Sc非晶合金靶材(其中的原子百分比：48％Zr，34％Cu，8％Ni，6％Al，2％Ag，2％Sc)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为100W、氩气压强为0.5Pa、基板温度为400℃，过渡层和非晶层的厚度分别约为12nm和500nm。反光镜的硬度为13GPa，反射率为0.86，耐刮擦次数为45次，盐雾测试大于800h。
实施例10：
采用丙酮、酒精、纯水超声清洗抛光聚酰亚胺基板，采用直径60mm的Ti靶材在聚酰亚胺基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Cu-Ni-Al-Ag-Y非晶合金靶材(其中的原子百分比：50％Zr，30％Cu，6％Ni，12％Al，1％Ag，1％Y)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为100W、氩气压强为0.5Pa、基板温度为200℃，过渡层和非晶层的厚度分别约为13nm和500nm。反光镜的硬度为12GPa，反射率为0.86，耐刮擦次数为36次，盐雾测试大于800h。
实施例11：
采用丙酮、酒精、纯水超声清洗抛光聚酰亚胺基板，分别采用直径60mm的Ti和Cr靶材在聚酰亚胺基板上进行直流磁控溅射镀膜得到过渡层，然后采用Zr-Ti-Cu-Ni-Al-Ag-Y非晶合金靶材(其中的原子百分比：50％Zr，2％Ti，34.9％Cu，5％Ni，7.5％Al，0.1％Ag,0.5％Y)在过渡层上进行直流磁控溅射镀膜得到非晶反光涂层，溅射功率为100W、氩气压强为0.5Pa、基板温度为200℃，过渡层和非晶层的厚度分别约为13nm和5000nm。反光镜的硬度为13GPa，反射率为0.86，耐刮擦次数为78次，盐雾测试大于1300h。

Claims (2)

1.一种非晶合金反光镜，其特征在于：所述非晶合金反光镜包括基板、涂覆在基板上的过渡层以及涂覆在过渡层上的非晶合金反光涂层；
所述非晶合金反光涂层的材料是Zr基非晶合金；
所述过渡层以Ni或Al为靶材，采用磁控溅射方式在基板上制得；
所述Zr基非晶合金为Zr-Ti-Cu-Ni-Al-Ag-RE，按原子百分比计：48-58％的Zr，0-2％的Ti，27-34％的Cu，3-6％的Ni，6-12％的Al，0.05-2％的Ag，0.1-2％的RE；RE表示稀土元素，为Y、Er、Sc或其组合；
其中所述非晶合金反光涂层的厚度为1000nm到5000nm；
其中所述过渡层厚度为10-13nm；
所述非晶合金反光镜的制备方法包括如下步骤：采用超声方式清洗基板，并进行紫外臭氧表面处理；基板材料是不锈钢、玻璃、陶瓷、PMMA亚克力、PET聚酰亚胺或PC聚碳酸酯；以Ni或Al为靶材，采用磁控溅射方式在基板上制备过渡层，基板温度为25-800℃；以所述的非晶合金反光涂层材料为靶材，采用磁控溅射方式在过渡层上制备非晶合金反光涂层，基板的温度控制在200-400℃之间。
2.一种非晶合金反光镜的制备方法，所述方法至少包括如下步骤：采用超声方式清洗基板，并进行紫外臭氧表面处理；基板材料是不锈钢、玻璃、陶瓷、PMMA亚克力、PET聚酰亚胺或PC聚碳酸酯；以Ni或Al为靶材，采用磁控溅射方式在基板上制备过渡层，基板温度为25-800℃；以权利要求1所述的非晶合金反光涂层材料为靶材，采用磁控溅射方式在过渡层上制备非晶合金反光涂层，基板的温度控制在200-400℃之间。
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