CN103882392A - 一种防指纹薄膜的制备方法及防指纹薄膜 - Google Patents

一种防指纹薄膜的制备方法及防指纹薄膜 Download PDF

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CN103882392A
CN103882392A CN201210559311.2A CN201210559311A CN103882392A CN 103882392 A CN103882392 A CN 103882392A CN 201210559311 A CN201210559311 A CN 201210559311A CN 103882392 A CN103882392 A CN 103882392A
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preparation
fingerprint
magnetron sputtering
magnesium fluoride
film
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周维
孙永亮
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BYD Co Ltd
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Priority to PCT/CN2013/089127 priority patent/WO2014094565A1/en
Priority to EP13866340.6A priority patent/EP2935644A4/en
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Abstract

本发明提供了一种防指纹薄膜的制备方法，在反应气氛中采用磁控溅射在基材表面形成防指纹薄膜；所述磁控溅射采用的靶材为聚四氟乙烯和氟化镁的混合物，所述反应气氛为保护气体和反应气体的混合物，所述反应气体为CF4或SiF4。本发明还提供了采用该制备方法制备得到的防指纹薄膜。本发明提供的防指纹薄膜的制备方法，采用磁控溅射的方法在触摸屏表面一次成型制备一层兼具有低表面和低折射率的氟化镁掺杂聚四氟乙烯薄膜，工艺简单；得到的防指纹薄膜，在保持结合力、耐磨性和耐腐蚀性较好的前提下具有低反射率和防手印的效果。

Description

一种防指纹薄膜的制备方法及防指纹薄膜
技术领域
本发明属于薄膜材料制备领域，尤其涉及一种防指纹薄膜的制备方法及由该制备方法制备得到的防指纹薄膜。 
背景技术
触摸屏作为一种最新的输入技术，是目前最简单、方便、自然的一种人机交互方式。它赋予了多媒体以崭新的面貌，是极富吸引力的全新多媒体交互设备。随着电子工业的发展，触摸屏的应用越来越广泛，从最初的小屏幕手机、MP3，到现在大尺寸屏幕的电脑、ATM、医疗、工业控制设备及显示器和电视机。特别是近两年， iPhone手机和ipad电脑的推出带动了触摸屏技术的发展，这一技术也正逐渐应用到其他的便携电子产品上。触摸屏在带来方便、舒适和快捷的同时，因使用过程中手指经常触碰屏幕表面留下指纹印和油污，不易清洗，时间一长就会影响屏幕的正常使用。 
手机及其它触摸屏产品在阳光下使用过程中，看不清屏幕，导致阅读、编辑短信困难，严重的会无法拨打号码，目前通常采用提高屏幕亮度的方法来改善，但该方法效果不大，且会大大降低电池使用时间，对日常手机使用造成严重困扰。因此寻求一种制备阳光下清晰、同时兼具防指纹效果的薄膜的方法已成为当务之急。 
发明内容
本发明解决了现有技术中存在的触摸屏在使用过程中表面易粘留指纹印和油污、且在阳光下无法使用的技术问题，提供了一种防指纹薄膜的制备方法以及由该制备方法制备得到的防指纹薄膜。 
具体地，本发明的技术方案为： 
一种防指纹薄膜的制备方法，在反应气氛中采用磁控溅射在基材表面形成防指纹薄膜；所述磁控溅射采用的靶材为聚四氟乙烯和氟化镁的混合物，所述反应气氛为保护气体和反应气体的混合物，所述反应气体为CF4或SiF4。
一种防指纹薄膜，所述防指纹薄膜由本发明提供的制备方法制备得到。 
本发明提供的防指纹薄膜的制备方法，采用磁控溅射的方法在触摸屏表面一次成型制备一层兼具有低表面和低折射率的氟化镁掺杂聚四氟乙烯薄膜（即本发明提供的防指纹薄膜），工艺简单。采用本发明提供的制备方法制备得到的防指纹薄膜，一方面能使屏幕表面具有较大的油接触角和低附着性，达到屏幕表面不易脏污和易清洁的效果；另一方面其低折射率可以使阳光反光率从10%降低到1%以下，提高阳光下触摸屏屏幕的清晰度；此外，本发明所制备的防指薄膜具有良好的耐摩擦性能。    
具体实施方式
本发明提供了一种防指纹薄膜的制备方法，在反应气氛中采用磁控溅射在基材表面形成防指纹薄膜；所述磁控溅射采用的靶材为聚四氟乙烯和氟化镁的混合物，所述反应气氛为保护气体和反应气体的混合物，所述反应气体为CF4或SiF4。 
本发明提供的防指纹薄膜的制备方法，采用磁控溅射的方法在触摸屏表面一次成型制备一层兼具有低表面和低折射率的氟化镁掺杂聚四氟乙烯薄膜（即本发明提供的防指纹薄膜），工艺简单。采用本发明提供的制备方法制备得到的防指纹薄膜，一方面能使屏幕表面具有较大的油接触角和低附着性，达到屏幕表面不易脏污和易清洁的效果；另一方面其低折射率可以使阳光反光率从10%降低到1%以下，提高阳光下触摸屏屏幕的清晰度；此外，本发明所制备的防指薄膜具有良好的耐摩擦性能。 
具体地，本发明中，所述靶材中聚四氟乙烯与氟化镁的摩尔比为1：（0.05~1）。优选情况下，所述靶材中聚四氟乙烯与氟化镁的摩尔比为1：（0.1~0.5）。 
本发明中，所述靶材可通过本领域技术人员制备得到，其制备方法为：将聚四氟乙烯颗粒与氟化镁颗粒按比例混合均匀，拌油熟化后装胚出胚，经烧结并车削成型，得到所述靶材。上述拌油、熟化和烧结的方法为本领域技术人员所公知，例如所述拌油的方法可以将聚四氟乙烯颗粒、氟化镁颗粒与5wt%的石墨混合均匀；所述熟化方法可以为在250℃静置30min；所述烧结方法可以为330-380℃烧结30min。 
本发明中，所述反应气氛为保护气体与反应气体的混合物，其中反应气体中的原子或分子会与靶材中的原子共同在衬底表面沉积，形成所述防指纹薄膜。所述反应气氛中，保护气体为N2或惰性气体。惰性气体即为元素周期表中零族元素对应的气体。所述反应气体为CF4或SiF4，其可提高沉积的薄膜中F的含量，从而得到高性能的薄膜。 
优选情况下，所述反应气氛中保护气体与反应气体的体积流量比为1：（0.1~1）。 
本发明中，保护气体和反应气体均采用纯度大于99.99%的气体，防止在薄膜中引入其它杂质元素。所述保护气体的体积流量为200-500 sccm，反应气体的体积流量为大于0至200sccm。 
本发明采用的磁控溅射可以为各种方式的磁控溅射，例如可以采用射频磁控溅射。且可以采用现有的磁控溅射设备完成，例如本发明采用的是13.56MHz、3KW的射频电源作为工作电源的磁控溅射镀膜机（北京北仪真空JP-900A）完成。 
具体地，所述磁控溅射的方法为：将真空室抽真空至5.0×10-3 Pa以下，充入反应气氛，直至气压为0.3-2Pa，优选为0.5-1     Pa，调整偏压为50-500V，占空比为15%-90%，以300-3000W的功率溅射5-25min。优选情况下，所述磁控溅射在恒定的功率下进行。更优选情况下，溅射功率为900-1500W。磁控溅射的条件更优选为：偏压为50-250V，占空比为40-60%，溅射时间为8-15min。 
在进行所述磁控溅射之前，还包括对基材进行超声波清洗处理。所述超声波清洗的方法为本领域常用的，例如在20kHz的超声中水洗10-25min。这样可以提高制得的防指纹薄膜在基材表面的附着力和透光率。 
优选情况下，在进行磁控溅射之前还包括对基材进行离子轰击处理，以提高基材表面的活性，从而提高磁控溅射膜层与基材的结合力。所述对基材进行离子轰击处理的步骤为本领域技术人员所公知，例如可以对基材表面进行氩离子轰击处理。所述氩离子轰击处理的方法为：将基材放置在工件架上，将真空室抽真空至1.0×10-2 - 8.0×10-2 Pa，充入氩气，至气压为0.1-5Pa，优选为0.5-3.0Pa，然后在偏压为200-1000V、占空比为20-70%的条件下轰击5-20min。优选情况下，偏压为400-800V，占空比为35-55%，轰击处理时间为8-15min。 
本发明还提供了一种防指纹薄膜，所述防指纹薄膜由本发明提供的制备方法制备得到。本发明所制备的防指纹薄膜，在保持结合力、耐磨性和耐腐蚀性较好的前提下还具有低反射率和防手印的效果。 
优选情况下，所述防指纹薄膜的厚度为10-30nm，可保证其具有优异的透光率和防指纹效果。更优选情况下，所述防指纹薄膜的厚度为15-30nm。 
为了使本发明所解决的技术问题、技术方案及有益效果更加清楚明白，以下结合具体实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。 
实施例1 
将聚偏氟乙烯颗粒和氟化镁颗粒混合（聚偏氟乙烯与氟化镁的摩尔比为1：0.1），然后拌油、熟化，再经过装胚、出胚，并进行烧结成胚，经车削后得到本实施例的靶材A1。   
将玻璃基底在20kHz的超声仪器中水洗20min，将清洗后的玻璃基材放入磁控溅射仪的真空炉内，关闭炉门，开启真空泵进行抽真空，抽真空至1.2×10-2Pa，通入氩气至真空度为1.5Pa，在偏压为600V、占空比为50%，对玻璃基底进行氩离子轰击处理，时间为8min。   
然后将靶材A1放入真空室内，关闭炉门抽真空至真空度为5.0×10-3Pa，通入Ar和CF4，Ar的体积流量为400sccm，CF4的体积流量为200sccm，调节Ar和CF4的体积比例为1：0.5，使真空度为1.0Pa，开启射频电源，靶电源功率为1000W，偏压200V，占空比为50%，时间为10min。冷却3min后出炉，得到厚度为20nm的表面具有防指纹薄膜B1的样品B10。
实施例2 
将聚偏氟乙烯颗粒和氟化镁颗粒混合（聚偏氟乙烯与氟化镁的摩尔比为1：0.5），然后拌油、熟化，再经过装胚、出胚，并进行烧结成胚，经车削后得到本实施例的靶材A2。   
将玻璃基底在20kHz的超声仪器中水洗20min，将清洗后的玻璃基材放入磁控溅射仪的真空炉内，关闭炉门，开启真空泵进行抽真空，抽真空至1.2×10-2Pa，通入氩气至真空度为1.5Pa，在偏压为600V、占空比为50%，对玻璃基底进行氩离子轰击处理，时间为8min。   
然后将靶材A2放入真空室内，关闭炉门抽真空至真空度为4.5×10-3Pa，通入Ar和SiF4，Ar的体积流量为333sccm，SiF4的体积流量为267sccm，调节Ar和SiF4的体积比例为1：0.8，使真空度为1.0Pa，开启射频电源，靶电源功率为2000W，偏压300V，占空比为50%，时间为15min。冷却3min后出炉，得到厚度为30nm的表面具有防指纹薄膜B2的样品B20。
实施例3 
将聚偏氟乙烯颗粒和氟化镁颗粒混合（聚偏氟乙烯与氟化镁的摩尔比为1：0.05），然后拌油、熟化，再经过装胚、出胚，并进行烧结成胚，经车削后得到本实施例的靶材A3。   
将玻璃基底在20kHz的超声仪器中水洗20min，将清洗后的玻璃基材放入磁控溅射仪的真空炉内，关闭炉门，开启真空泵进行抽真空，抽真空至1.2×10-2Pa，通入氩气至真空度为1.5Pa，在偏压为600V、占空比为50%，对玻璃基底进行氩离子轰击处理，时间为8min。   
然后将靶材A3放入真空室内，关闭炉门抽真空至真空度为5.0×10-3Pa，通入Ar和CF4，Ar的体积流量为300sccm，CF4的体积流量为300sccm，调节Ar和CF4的体积比例为1：1，使真空度为1.0Pa，开启射频电源，靶电源功率为1000W，偏压200V，占空比为50%，时间为10min。冷却3min后出炉，得到厚度为10nm的表面具有防指纹薄膜B3的样品B30。
实施例4 
将聚偏氟乙烯颗粒和氟化镁颗粒混合（聚偏氟乙烯与氟化镁的摩尔比为1：1），然后拌油、熟化，再经过装胚、出胚，并进行烧结成胚，经车削后得到本实施例的靶材A4。   
将玻璃基底在20kHz的超声仪器中水洗20min，将清洗后的玻璃基材放入磁控溅射仪的真空炉内，关闭炉门，开启真空泵进行抽真空，抽真空至1.2×10-2Pa，通入氩气至真空度为1.5Pa，在偏压为600V、占空比为50%，对玻璃基底进行氩离子轰击处理，时间为8min。   
然后将靶材A4放入真空室内，关闭炉门抽真空至真空度为5.0×10-3Pa，通入Ar和CF4，Ar的体积流量为550sccm，CF4的体积流量为55sccm，调节Ar和CF4的体积比例为1：0.1，使真空度为1.0Pa，开启射频电源，靶电源功率为1000W，偏压200V，占空比为50%，时间为10min。冷却3min后出炉，得到厚度为10nm的表面具有防指纹薄膜B4的样品B40。
对比例1 
制备方法与实施例1相同，不同的是，采用聚四氟乙烯靶材取代实施例1中的靶材A1，得到本对比例的具有防指纹薄膜DB1的样品DB10。
对比例2 
在玻璃基材上采用真空镀膜法依次镀制厚度为10nm二氧化硅膜、厚度为10nm的三氧化二铝膜、厚度为10nm的二氧化锆膜、厚度为10nm的氟化镁膜和厚度为10nm的聚四氟乙烯膜，得到本对比例的具有防指纹薄膜DB2的样品DB20。
性能测试 
对上述制备得到的样品B10-B40和DB10-DB20进行如下性能测试。
1、反射率测试 
采用LCD-5200光电特性测试仪，扫描380-780nm波段，按照GBT 2680-1994公开的太阳光各波段分布特性，计算各样品以及玻璃表面针对可见光的反射率。
2、接触角测试 
以接触角测量仪（德国Dataphysics公司生产的型号为OCA20；主要技术指标为：接触角测量范围：0-180°，测量精度：±0.1°）测定十六烷在样品表面的接触角，采用即滴即测的方式测试。
3、耐摩擦测试 
采用耐磨擦测试机（型号为HD-206），接触面为0000#钢丝绒，接触面积2cm×2cm，负重500g，行程35mm，摩擦速度为50循环/分。测试1000次后再进行接触角测试。
测试结果如表1所示。   
表1
Figure 2012105593112100002DEST_PATH_IMAGE001
。
从上表1的测试结果可以看出，通过本发明提供的制备方法制备得到的防指纹薄膜具有非常高的接触角，说明其具有优异的防指纹、油污的效果，而且耐摩擦效果好，反射率低，即采用该防指纹薄膜的样品即使在阳光下仍非常清晰。 
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。 

Claims (12)

1. 一种防指纹薄膜的制备方法，在反应气氛中采用磁控溅射在基材表面形成防指纹薄膜；其特征在于，所述磁控溅射采用的靶材为聚四氟乙烯和氟化镁的混合物，所述反应气氛为保护气体和反应气体的混合物，所述反应气体为CF4或SiF4。
2.根据权利要求1所述的制备方法，其特征在于，所述靶材中聚四氟乙烯与氟化镁的摩尔比为1：（0.05~1）。
3.根据权利要求2所述的制备方法，其特征在于，所述靶材中聚四氟乙烯与氟化镁的摩尔比为1：（0.1~0.5）。
4.根据权利要求1-3任一项所述的制备方法，其特征在于，制备所述靶材的方法为：将聚四氟乙烯颗粒与氟化镁颗粒按比例混合均匀，拌油熟化后装胚出胚，经烧结并车削成型，得到所述靶材。
5.根据权利要求1所述的制备方法，其特征在于，所述保护气体为N2或惰性气体。
6.根据权利要求1或5所述的制备方法，其特征在于，所述反应气氛中保护气体与反应气体的体积流量比为1：（0.1~1）。
7.根据权利要求1或5所述的制备方法，其特征在于，所述保护气体的体积流量为200-500 sccm，反应气体的体积流量为大于0至200sccm。
8.根据权利要求1所述的制备方法，其特征在于，所述磁控溅射的方法为：将真空室抽真空至5.0×10-3 Pa以下，充入反应气氛，直至气压为0.3-2Pa，调整偏压为50-500V，占空比为15%-90%，以300-3000W的功率溅射5-25min。
9.根据权利要求1所述的制备方法，其特征在于，在进行所述磁控溅射之前，还包括对基材进行超声波清洗和离子轰击处理的步骤。
10.根据权利要求1所述的制备方法，其特征在于，所述离子轰击处理为氩离子轰击处理，步骤为：将真空室抽真空至1.0×10-2 - 8.0×10-2 Pa，充入氩气，至气压为0.1-5Pa，然后在偏压为200-1000V、占空比为20-70%的条件下轰击5-20min。
11. 一种防指纹薄膜，其特征在于：所述防指纹薄膜由权利要求1-10任一项所述的制备方法制备得到。
12.根据权利要求11所述的防指纹薄膜，其特征在于，在基材表面形成的防指纹薄膜的厚度为10-30nm。
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