CN105779943A - 一种物理气相沉积氟硅烷制备疏水膜的方法 - Google Patents

一种物理气相沉积氟硅烷制备疏水膜的方法 Download PDF

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CN105779943A
CN105779943A CN201610292659.8A CN201610292659A CN105779943A CN 105779943 A CN105779943 A CN 105779943A CN 201610292659 A CN201610292659 A CN 201610292659A CN 105779943 A CN105779943 A CN 105779943A
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silicon
hydrophobic membrane
silicon fluoride
fluoroalkyl silane
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黄贤明
张先超
孙昇凌
李明仁
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Xiamen Runner Industrial Corp
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Abstract

本发明公开一种物理气相沉积氟硅烷制备疏水膜的方法，一，等离子体辉光处理：将基材放入PVD真空设备中，进行抽真空，当真空度达到10‑2Pa时，对基材实施等离子辉光处理；二，中频磁控溅射透明氧化硅膜，溅射靶材为纯硅靶；三，真空蒸镀氟硅烷疏水膜：采用真空蒸镀技术，在溅射二氧化硅膜过程的第三分钟开始进行蒸发氟硅烷：预热清洗氟硅烷镀材10‑30秒，电压2‑3V；预蒸发20‑50秒，电压3‑4V；蒸发100‑200秒，电压4‑6V，在二氧化硅膜层表面沉积一层氟硅烷，并与二氧化硅形成硅烷交联反应，得到透明的氟硅烷疏水膜层。本发明可以形成结合力较好的镀膜，且成膜无需高温烘烤，生产成本较低。

Description

一种物理气相沉积氟硅烷制备疏水膜的方法
技术领域
本发明涉及表面处理技术领域，尤其是指一种物理气相沉积氟硅烷制备疏水膜的方法。
背景技术
疏水性表面具有防污，防水，防腐蚀等作用。现有技术中，制备疏水表面的方法主要有两种：一，改变材料表面结构形貌，制备针状表面；二，驱使材料表面具有较低的表面能。
常规的氟硅烷疏水膜制备方法之一是通过浸涂后烘烤的方法制备，该方法的缺点是工艺流程较长，需要消耗较多的氟硅烷原材料，烘烤温度较高，而一般塑胶材料无法耐高温，造成成本较高和影响使用。
常规的氟硅烷疏水膜制备方法之二是使用物理气相沉积(PVD)或化学气相沉积(CVD)的方法制备。物理气相沉积制备疏水涂层的缺点是氟硅烷在沉积过程中没有发生化学反应，所以涂层的结合力不好，耐磨性较差及使用寿命较短。化学气相沉积制备反应气体容易造成氟硅烷的裂解，而影响疏水效果，并且沉积速度较慢成本较高。
有鉴于此，本发明提出一种克服所述缺陷的物理气相沉积氟硅烷制备疏水膜的方法，本案由此产生。
发明内容
本发明的目的在于提供一种物理气相沉积氟硅烷制备疏水膜的方法，以形成结合力较好的镀膜，且成膜无需高温烘烤，生产成本较低。
为达成上述目的，本发明的解决方案为：
一种物理气相沉积氟硅烷制备疏水膜的方法，包括以下步骤：
一，等离子体辉光处理：将基材放入PVD真空设备中，进行抽真空，当真空度达到10-2Pa时，对基材实施等离子辉光处理，离子源电流0.5-0.8A，氩气流速100-200SCCM，时间为2-5min；
二，中频磁控溅射透明氧化硅膜：中频电源功率300-1000W，负偏压100-200V，氩气流速30-80SCCM，氧气流速50-100SCCM，溅射时间为4-7min，溅射靶材为纯硅靶；
三，真空蒸镀氟硅烷疏水膜：采用真空蒸镀技术，在溅射二氧化硅膜过程的第三分钟开始进行蒸发氟硅烷：预热清洗氟硅烷镀材10-30秒，电压2-3V；预蒸发20-50秒，电压3-4V；蒸发100-200秒，电压4-6V，在二氧化硅膜层表面沉积一层氟硅烷，并与二氧化硅形成硅烷交联反应，得到透明的氟硅烷疏水膜层。
进一步，在等离子体辉光处理步骤之前，还包括基材清洗步骤。
采用上述方案后，本发明在溅射形成二氧化硅膜后开始蒸发氟硅烷，同时继续溅射形成二氧化硅膜，使得在二氧化硅膜层表面沉积一层氟硅烷，并与二氧化硅形成硅烷交联反应，发生化学反应而得到透明的氟硅烷疏水膜层，进而使得镀膜的结合力较好，成膜无需高温烘烤，生产成本较低。
因此，与现有技术相比，其具有以下优点：在物理沉积过程中氧离子和硅离子能与氟硅烷形成硅烷交联反应，形成镀膜结合力好；成膜后无需高温烘烤，可以用于不耐高温的塑胶材料表面处理；工艺连续，工艺过程短，原材料利用率高，成本低；可以在金属，陶瓷或有机物等各种材料表面制备疏水膜，不受材料限制。
具体实施方式
以下结合具体实施例对本发明做详细描述。
一种物理气相沉积氟硅烷制备疏水膜的方法，包括以下步骤：
一，清洗基材。
二，等离子体辉光处理：将基材放入PVD真空设备中，进行抽真空，当真空度达到10-2Pa时，对基材实施等离子辉光处理，离子源电流0.5-0.8A，氩气流速100-200SCCM，时间为2-5min，达到清洁及活化基材表面之目的。
三，中频磁控溅射透明氧化硅膜：中频电源功率300-1000W，负偏压100-200V，氩气流速30-80SCCM，氧气流速50-100SCCM，溅射时间为4-7min，溅射靶材为纯硅靶。
四，真空蒸镀氟硅烷疏水膜：采用真空蒸镀技术，在溅射二氧化硅膜过程的第三分钟开始进行蒸发氟硅烷：预热清洗氟硅烷镀材10-30秒，电压2-3V，清除氟硅烷中的小分子溶剂；预蒸发20-50秒，电压3-4V，加热蒸发使氟硅烷发生水解反应；蒸发100-200秒，电压4-6V，在二氧化硅膜层表面沉积一层氟硅烷，并与二氧化硅形成硅烷交联反应，得到透明的氟硅烷疏水膜层。
氟硅烷与二氧化硅形成硅烷交联反应如下：
R表示全氟侧基
对使用本发明方法镀好的疏水膜产品进行功能测试，疏水，疏油效果优越，耐摩擦性能优越，并且使产品具有良好的抗腐蚀性。油接触角达到70°以上；水接触角达到110°以上。耐腐蚀测试，铜加速盐雾测试CASS(防腐蚀测试ASTM B368-09)可通过24h测试；酸性盐雾测试AASS(盐雾测试ASTM G85-9)可通过96h测试。
以上所述仅为本发明的优选实施例，并非对本案设计的限制，凡依本案的设计关键所做的等同变化，均落入本案的保护范围。

Claims (2)

1.一种物理气相沉积氟硅烷制备疏水膜的方法，其特征在于，包括以下步骤：
一，等离子体辉光处理：将基材放入PVD真空设备中，进行抽真空，当真空度达到10-2Pa时，对基材实施等离子辉光处理，离子源电流0.5-0.8A，氩气流速100-200SCCM，时间为2-5min；
二，中频磁控溅射透明氧化硅膜：中频电源功率300-1000W，负偏压100-200V，氩气流速30-80SCCM，氧气流速50-100SCCM，溅射时间为4-7min，溅射靶材为纯硅靶；
三，真空蒸镀氟硅烷疏水膜：采用真空蒸镀技术，在溅射二氧化硅膜过程的第三分钟开始进行蒸发氟硅烷：预热清洗氟硅烷镀材10-30秒，电压2-3V；预蒸发20-50秒，电压3-4V；蒸发100-200秒，电压4-6V，在二氧化硅膜层表面沉积一层氟硅烷，并与二氧化硅形成硅烷交联反应，得到透明的氟硅烷疏水膜层。
2.如权利要求1所述的一种物理气相沉积氟硅烷制备疏水膜的方法，其特征在于，在等离子体辉光处理步骤之前，还包括基材清洗步骤。
CN201610292659.8A 2016-05-05 2016-05-05 一种物理气相沉积氟硅烷制备疏水膜的方法 Pending CN105779943A (zh)

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CN107460448A (zh) * 2017-08-04 2017-12-12 中国科学院宁波材料技术与工程研究所 一种基体表面的修饰涂层及其制备方法
CN108395284A (zh) * 2018-02-01 2018-08-14 九牧厨卫股份有限公司 一种防污涂层及其应用以及含有其的陶瓷产品
CN112903991A (zh) * 2021-01-28 2021-06-04 中国地质大学（武汉） 一种具有疏水涂层的纳米孔道膜及其制备方法和应用
CN113376717A (zh) * 2021-07-01 2021-09-10 江苏航运职业技术学院 一种眼镜镜片纳米防雾膜及其制备方法
CN114457309A (zh) * 2022-02-11 2022-05-10 九牧厨卫股份有限公司 一种五金易洁表面处理的方法

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CN114457309A (zh) * 2022-02-11 2022-05-10 九牧厨卫股份有限公司 一种五金易洁表面处理的方法

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