CN1237200C - 等离子体活化蒸发法沉积二氧化硅 - Google Patents

等离子体活化蒸发法沉积二氧化硅 Download PDF

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CN1237200C
CN1237200C CNB981151191A CN98115119A CN1237200C CN 1237200 C CN1237200 C CN 1237200C CN B981151191 A CNB981151191 A CN B981151191A CN 98115119 A CN98115119 A CN 98115119A CN 1237200 C CN1237200 C CN 1237200C
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C·D·亚科范格洛
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Abstract

使用等离子体活化反应性沉积法在不同基片上沉积氧化硅抗刮伤的涂层。本方法包括将硅或硅的氧化物蒸发到氩气和一氧化二氮等离子体中，等离子体朝着待涂复的表面。

Description

等离子体活化蒸发法 沉积二氧化硅
技术领域
本发明涉及在各种表面上，特别是塑料表面，沉积稳定的粘附的抗磨损薄膜或涂层，也涉及具有这样涂层的制品。
背景技术
工程树脂是工业上可以得到的众所周知的材料，这些材料具有多种物理和化学性能，它们得到了广泛的应用。例如，聚碳酸酯，由于它们具有极好的抗断裂作用，所以它们在许多产品中代替了玻璃，例如汽车前灯和交通指示灯的镜片，窗安全遮护板以及建筑窗用玻璃等等。可是，聚碳酸酯所显示的主要缺点是它们抗刮伤能力很低，而且对紫外光诱导降解作用也敏感。
硅薄膜沉积的几种技术已广泛使用，例如化学蒸汽沉积(CVD)、物理蒸汽沉积(PVD)、电子束取向生长沉积和等离子体增强化学蒸汽沉积(PECVD)、以及等离子体聚合(pp)。方法的选择常常受要涂覆的基片特别是基片的热稳定性的支配，基片的这种热稳定性限制了可能作用于基片的温度。对于各种各样的应用而言，例如光学玻璃、建筑窗、汽车窗用玻璃等等，沉积的主要目的就是将硬的耐磨的硅膜沉积在塑料上。生产这样产品的关键就是开发高速度低价格的方法，这种方法能够使高质量的氧化物薄膜沉积在表面上，特别是塑料表面上。物理蒸汽沉积技术例如喷涂可以形成优质的涂层，但是在低速下进行，从成本上讲并不有效。高温化学蒸汽沉积技术在超过基片温度极限的温度下可以在高速下进行，但是温度则超过基片的极限温度。
等离子体活化反应性蒸发(ARE)法已发现是一种适合于在低温基片上例如塑料上进行沉积，也适合于在高温材料上例如陶瓷和玻璃上进行沉积的方法。此方法是在一氧化氮、有机硅和氩等离子体存在时，使用电子束高速蒸发二氧化硅或硅，以便在不超过塑料的温度耐受能力的条件下进行成核并沉积出致密的薄膜。在非氧化物元素蒸发的场合下，附加的氧气入口可以用来提供氧气，而在蒸发氧化物时则可以用作补充氧。
发明内容
本发明提供在基片上沉积硅、碳和氧的硬的稳定的粘附的和抗磨损涂层的方法，此基片例如聚碳酸酯表面或预先用任何沉积硬涂层的常规方法例如浸涂法或滚压法涂覆过聚硅氧烷硬涂层的聚碳酸酯表面。在真空室中，在蒸发二氧化硅上方放置的塑料表面上，使用标准电子束蒸发二氧化硅。多重中空(multiple hollow)阴极等离子体源放在基片的正下方，以便使蒸发材料和基片表面暴露于等离子体中。在等离子体源的正下方引入一氧化二氮气流，以使气体通过等离子体而到达被涂覆的表面。出乎意料地发现一氧化二氮的存在改善了涂层的稳定性和改变了涂层中的应力。有机硅也是在等离子体源的正下方引入的，以便使它通过等离子体源。发现有机硅的存在改进了涂层的柔软性(对微断裂的应变％测量的)和涂层的泰伯尔(Taber)抗磨损性。
具体而言，本发明提供一种用抗磨损金属氧化物层涂覆塑料基片的方法，该方法包括：将塑料基片放入真空室中；在真空室内使形成氧化物的金属或金属氧化物进行电子束蒸发，将形成氧化物的金属通入已经引入一氧化二氮的氩气等离子体中；使塑料基片暴露于等离子体内，从而使抗磨损层沉积在基片的暴露表面上。
特别是，本发明提供一种用抗磨损金属氧化物层或二氧化硅层涂覆塑料基片的方法，该方法包括：将塑料基片放入真空室中；在真空室内使形成氧化物的金属或二氧化硅进行电子束蒸发，将形成氧化物的金属或二氧化硅通入已经引入一氧化二氮的氩气等离子体中；使塑料基片暴露于等离子体内，从而使抗磨损层沉积在基片的暴露表面上，其中形成氧化物的金属是硅、钛或铝。
有机硅改性的具有改进柔软性的氧化物层或薄膜，可抗开裂、抗剥离和抗磨损，这些薄膜可以利用一种方法在基片表面上进行沉积，这种方法是在等离子体存在下，将物理的和化学的蒸汽沉积技术结合起来。少量的至少一种合适的有机单体可改进薄膜的性能。向反应室供给反应性气体和单体，同时供应蒸发形成氧化物的元素，例如象钛、铝或硅这样的元素金属或金属氧化物例如二氧化硅，以使这些成分在与要沉积的薄膜的基片表面接触之前通过高密度的等离子体。使反应性气体、氧化物前体和单体在接触到表面之前通过等离子体可以改进薄层的结构和它的性能。
含硅反应性单体包括硅烷、二硅烷或有机硅化合物，例如四甲基二硅氧烷(TMDSO)，六甲基二硅氧烷(HMDSO)，原硅酸四乙酯，六甲基二硅烷，八甲基环四硅氧烷(D4)，和四甲基环四硅氧烷。
附图说明
图1表示了本发明的优选实施方案，在此方案中，基片1是塑料板，此塑料板置于可动台板2的顶部。此塑料板位于台板窗的正上方，以使它可在冷却盖3的窗的上方平移。它暴露于等离子体、气体和蒸发物之中。利用电子束枪5冲击表面，使二氧化硅从转鼓4中蒸发出来，当转鼓转动时，电子束沿着转鼓长度平移。和常规操作一样，电子束发生磁力偏转。多重中空阴极等离子体源6位于平移板的正下方，并进行磁力聚焦(未示出)，为使电子束沿着板的宽度以均匀等离子体密度散布。反应性气体例如一氧化二氮、有机硅和/或氧通过位于窗两侧和等离子体下方的两个气体进口总管7和8而送入反应室，因此气体通过等离子体源，并与蒸发物反应。典型情况下，为了从反应室除去残留的水分，反应室用泵抽以达到设定的压力。然后通过向多重中空阴极和氧化剂进料供应氩气而增加压力。在调节二氧化硅蒸发速度和获得稳定的等离子体密度后，打开冷却板内遮盖窗口的活门。为了根据蒸发速度获得所需要的厚度，来设定含有待涂覆的塑料板的台板2的移动速度。
在18厘米×36厘米×3毫米的有和没有硅硬涂层的聚碳酸酯板上进行沉积。将一氧化二氮和氧气流的速度从0调节到4升/分，使两支进气总管具有相等的气流速度。有机硅的流速从0调节到4克/分。多重中空阴极等离子体从0调节到200安培。视气流速度而定，沉积期间的压力范围由0.1-0.7Pa。调节沉积时间，以获得2-4微米范围的靶厚。
图2表示3本发明的另一个实施方案。基片1是一种塑料薄膜，它从输出盘2经由冷却鼓3传送到接受盘4。二氧化硅从一系列配置在冷却鼓3底部的耐热蒸发皿5中蒸发出来。使用基片前面的一对磁控管7来产生高密度的等离子体。在等离子区下部配置有供引入一氧化二氮和其它的反应性气体或等离子体气体而用的喷管8，9，10和11。喷管对着待涂覆的表面。
具体实施方式
18厘米×36厘米×3毫米的聚碳酸酯板按下列方式用二氧化硅进行涂覆。一氧化二氮以2升/分的速度经两条进料管线的每条管线给料，总流量4升/分。反应室在沉积前泵抽至0.21Pa，然后在沉积期间上升到0.7Pa。使用0.32安的电子束流蒸发硅，0.32安的电子束流将给出约250纳米/秒的沉积速度。为得到4微米的沉积厚度、塑料板通过可动台板上的蒸发源，移动速度约1厘米/秒。设定多重中空阴极电流为200安。和标准的深紫色氩的等离子体相比较，这种等离子体的颜色是很浅的。涂层很清晰，能很好地附着于聚碳酸酯板的基片上。几星期后的目测检查在外观、附着力、剥离或与空气的明显反应方面未发现有变化。
例6、7按类似的方式进行，如表1所示，只是流速和等离子体流有改变。在低等离子体或没有等离子体的情况下，获得了良好的结果，这显示出本发明的主要长处。本发明的附加长处在于控制一氧化二氮的进料速度可以将涂层的应力由拉伸应力调节到压缩应力。
比较例2-5也以类似的方式进行，如表1所示，只是气体进料的类型和等离子流有改变。如表1所示，通过比较在没有氧化性气体进料的情况下，与空气的反应性将引起涂层剥离而与等离子体活化的水平无关。在高等离子体活化下和使用高流速的氧的确会产生非反应性涂层，但由于加料速度或等离子体流的任何降低导致了涂层的剥离，所以操作窗是不够的。
表1
             利用ARE制成的二氧化硅涂层
实例     等离子体(安)    气体流量(升/分)    应力        结果说明
1        2×200          N2O2×2             T          清晰，无剥离，附着好
2        2×200          -                    C          几分钟内剥离
3        2×200          O22×1              T          清晰，无剥离，附着差
4        2×200          O22×0.5            T          几分钟内剥离
5        -               O22×1              -          几分钟内剥离
6        -               N2O2×2             T          清晰，无剥离，附着好
7        2×125          N2O2×1             C          清晰，无剥离，附着好
T＝拉伸应力
C＝压缩应力
表2的例2-4是以类似的方式进行的，只是有机硅的流速和等离子体有变化，这显示了本发明方法的第二个长处。本发明方法的主要长处在于，由于使用了联合的CVD和PVD来达到沉积涂层，有机硅的引入增加了涂层的柔软性和抗磨损性。
如表所示，通过比较，在没有有机硅气体加料的情况下，泰伯尔磨损和开裂的应变％很低。使用有机硅增加了开裂的应变％和泰伯尔磨损，可是在有机硅超过某个水平之上，会造成泰伯尔磨损的降低。
表2
           利用ARE制成的硅、氧、碳涂层
实例    六甲基二硅氧烷(克/分)    流量(升/分)   ％雾霾  ％应变  ％C
 1                0                 2×2         18      0.8    0
 2                1                 2×2         12      1.2    2
 3                2                 2×2         4       1.5    6
 4                4                 2×2         13      1.9    12

Claims (4)

1.一种用抗磨损层涂覆聚碳酸酯基片的方法，该方法包括：将聚碳酸酯基片放入真空室中；在真空室内使硅、钛、铝或二氧化硅进行电子束蒸发，将硅、钛、铝或二氧化硅通入已经引入一氧化二氮的氩气等离子体中；使聚碳酸酯基片暴露于等离子体内，从而使抗磨损层沉积在基片的暴露表面上。
2.根据权利要求1的方法，进一步包括在真空室内形成真空。
3.根据权利要求1的方法，其中抗磨损层是二氧化硅。
4.根据权利要求1的方法，进一步包括将氧气通入氩气等离子体中。
CNB981151191A 1997-06-26 1998-06-26 等离子体活化蒸发法沉积二氧化硅 Expired - Fee Related CN1237200C (zh)

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CN1210899A (zh) 1999-03-17
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DE69800280D1 (de) 2000-10-05
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ES2149631T3 (es) 2000-11-01
CA2241678C (en) 2007-08-28
EP0887433A1 (en) 1998-12-30
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DE69800280T2 (de) 2001-04-05
US6379757B1 (en) 2002-04-30

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