CN102027155A - 涂层以及制备涂层的方法 - Google Patents
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Abstract
本发明涉及用PECVD而不用附加的生产步骤制备图案化涂层的方法。所述方法在基材上直接沉积制备出类似蛾眼睛的宏观结构。而且,所述宏观结构可以被在次波长范围内具有表面织构的微观结构调节。结果是,可以制备出包括由光学透明材料组成的负载层的保护性的、减反射的涂层,其至少一个表面为表现出与表面入射线的光波长相关的减反射性质,以及能使其表现出超疏水表面性质的表面结构。
Description
发明背景
1.发明领域
本发明通常涉及表面保护涂层。更明确地,本发明涉及与保护性或疏水性涂层相关的塑料和金属成分。
2.背景技术
在塑料或金属基材上由PECVD(等离子体增强化学气相沉积)制备的表面保护性涂层由于其硬度、耐磨性、附着力、具有吸引力的颜色和其他性能而具有广泛的应用潜力。由PECVD在透明或金属基材上制备的透明表面保护性涂层在室内光线条件下由于干涉效应而倾向于表现出所谓的牛顿环或折射条纹(一种装饰效果,是由多次反射制造的彩虹视觉效果)。这些干涉效应制约了所述涂层在装饰性功能中的使用。提出的保护性涂层的表面图案在第一表面抑制干涉效应,抑制牛顿环和条纹,以及提高涂层的光透射率。这些保护性涂层的应用覆盖(abrange)了用于手持设备的透明塑料窗口,部件被透明面层保护的所有涂漆(painting)应用,装置中金属的耐磨性对于预计的应用不够的所有装饰性和功能性金属部件,需要面层来保护金属层的真空涂金属化的塑料部件。
对物体例如玻璃片赋予减反射性是公知的技术,其通过在对象表面引入微波纹得到(例如参见:“Artificial Media Optical Properties-Subwavelength Scale”,Lalanne和Hutley,发表于“Encyclopedia of Optical Engineering(光学工程百科全书)”,2003)。我们称这种低反射率的表面为微结构减反射织构(MART)。MART的微波纹典型地在长度尺度上足够的小——一般在次波长尺度——从而防止通常由“无光泽的”或“不光滑的”面漆表现出的光的漫散射。也就是说,MART确实降低了表面的半球面反射比,而不是仅仅将反射波散射或漫射。在这种体系下,光和微结构表面之间的相互作用通常用“有效介质理论”来描述,在该理论下微织构化表面的光学性质由区域内材料性质的空间平均性决定(Raguin和Morris,“Antireflection Structured Surfaces for the Infrared Spectral Region”,Applied Optics(应用光学),第32卷第7期,1993)。对于适当设计的MART,光从玻璃返回空气的半球面反射比可以少于0.5%。如果表面波纹比入射光的波长大很多的话,那么这样小的半球面反射比是不可能得到的。对可视光而言,MART波纹的长度尺度典型的约为半微米。
可能最为人所知的MART是被称为“蛾眼睛”的表面,其具有的光学性能可能比市场上存在的薄膜涂层更有效。薄膜减反射涂层通常由一层或多层光学性不同于基材而且以精准控制的厚度溅射或蒸发在基材上的材料组成。蛾眼睛表面包含规则排列的微观尺度突起,而且目前在世界范围内可以从少数制造商处得到(例如在英国牛津郡的Autotype International Limited)。其他MART的例子有“SWS表面”(Philippe Lalanne,“Design,fabrication,and characterization ofsubwavelength periodic structures for semiconductor antireflection coating in thevisible domain”,第300-309页,SPIE Proceedings第2776卷,(1996)),和“MARAG”表面(Niggemann等,“Periodic microstructures for large areaapplications generated by holography”,第108页,Proceedings of the SPIE第4438卷(2001))。
透明或不透明的,由PECVD在透明或金属基材上制备的表面保护性涂层,可用于提高表面的疏水性。表面的疏水性取决于最表层的化学组成和表面形貌。提出的沉积技术得到的表面形貌可以将水的接触角从95°……105°增加到大于150°,这对于疏水性而言是显著的提高。
发明内容
用气体的化学反应在基材上形成薄膜是普遍使用的工业方法。这种沉积方法被称之为化学气相沉积或“CVD”。常规热CVD工艺是对基材表面提供反应气体,在基材表面发生热诱导的化学反应,以得到所需薄膜。另一方面,等离子体增强的CVD技术,是通过应用射频(RF)或微波能量来促进反应气体的激发和/或分解。所释放物质的高反应性降低了发生化学反应所需的能量,因此对于此类PECVD方法降低了所需温度。PECVD能将硬质保护性涂层沉积到塑料和金属基材上。所提出方法在沉积硬质层的末期期间影响基材上的气流,以形成图案化的表面。图案化的层具有所谓的蛾眼睛效应,抑制此类的多种光学反射。所提出方法的另一实施方案是表面图案,其提高表面的疏水性达到与水的接触角大于150°。
本发明实施例的这些和其他特征从以下说明和附加的权利要求可以更完整的表现,或可以从下文中给出的发明实施例中得到教导。
按照本发明的一个示范性方面,提供了用于沉积图案化的涂层的沉积过程或方法,所述方法包括:用等离子体增强化学气相沉积在弯曲的或平的基材上通过图案化装置直接沉积图案化的涂层。
在一实施方案中,图案化的涂层包括多个突起或由多个突起组成。在一实施方案中,所述突起的直径在1至100μm之间,突起的高度在0.01到0.5μm之间,以及突起之间的间隔在10至500μm之间。从而可以得到小分辨率的图案。所述图案化的涂层可以为均匀的。
在一个实施方案中,提供了用PECVD而无附加制备步骤的制备图案化涂层的方法。一实施方案通过所建议的方法在表面直接沉积制备出类蛾眼睛的宏观结构从而更优秀。此外,宏观结构可通过在次波长(subwavelength)范围内具有表面织构的微结构调节。结果,可以制备出包含由光学透明材料构成的负载层的保护性的、减反射的涂层,其至少在一个表面侧上相对于入射到表面的射线的光波长表现出减反射性质,也可以制备出能使表面具有超疏水性特性的表面结构。
附图简要说明
为了进一步阐明本发明及其实施方案的上述以及其他优点和特征,本发明更详细的说明将参考在附图中所描绘的详细的实施方案得到阐述。需要考量的是这些附图描述的仅是本发明的典型实施方案,因此不应视作对发明范围的局限。将通过附图用附加的特征和细节对本发明加以说明和解释,其中:
图1a和图1b为依照本发明实施方案的典型制备装置的示意图;
图2是图案化涂层的示意图;
图3a是依照本发明一实施方案的光学结构的示意图,以及图3b显示所示结构的光学反射图样;
图4a是依照本发明另一实施方案的结构的示意图,以及图4b是所示结构的光学反射图样。
本发明的详细说明
能实施本发明方法的一种适合的PECVD(等离子体增强化学气相沉积)装置在图1a和1b中示出,其为PECVD系统4的垂直剖面图,具有真空室或加工室。
PECVD系统4包含用于向装于底座7上的基材5分散加工气体3的气体分配集管面板2,位于加工室的中心。
沉积气体和载气通过常规的平的、圆形气体分配器2上的穿孔引入腔室4。更确切地,沉积加工气体从输入集管1通过常规的穿孔块继而通过气体分配面板2中的孔流入腔室。
在到达集管1之前,沉积气体和载气从气体源12通过气体供给线路通入到混合系统13中,于其中被混合并而后被送至集管1。通常,用于每种加工气体的供给线路包括(i)能够用来自动地或手动地关闭加工气体向腔室的流入的若干安全关闭阀(未显示),和(ii)测量通过供给线路的气体流量的质量流量控制器(也未显示)。当在工艺过程中使用有毒性气体时,所述若干安全关闭阀以传统的配置方式被置于各气体供给线路上。
PECVD系统4中发生的沉积过程可以为远程等离子体增强过程,或是阴极等离子体增强过程。在远程等离子体增强过程中,RF电源在绝缘的气体分配面板2和辅助的附加电极或腔室壁之间提供电能。所述底座7与腔室壁电连接。在阴极等离子体增强方法中,RF电源在绝缘的底座7和辅助的附加电极或腔室壁之间提供电能。气体分配面板继而与腔室壁电连接。在所述两种情况中,RF能量在面板2和底座7之间的圆柱形区域9(该区域在此被称为“反应区域”)中激发加工气体混合物形成等离子体。等离子体的成分发生反应,将所要得到的薄膜沉积到由底座7支撑的基材的表面上。RF电源通常以13.56MHz或更高的高RF频率(RF)提供能量。
基材5置于底座7之上,其中平板基材可以直接置于底座上,而弯曲的基材置于支撑设备上,该支撑设备在与基材接触的一面具有与基材相同的曲度而与底座7接触的一面是平面。
在图1a所示的一优选结构中,栅网或一穿孔板6置于基材和反应区域之间(该栅网或穿孔板在此称为“图案化设备”)。所述图案化设备6与底座7相连。所述图案化设备6和基材表面之间的距离可以在0.1到15mm之间变化,视孔的大小和孔之间距离而定。在一些实施方案中,所述图案化设备6小于2mm厚。所述图案化设备6可以由金属箔、织物卷幅、玻璃、陶瓷或塑料材料制成。
在图1b所示的替代性结构中,所述基材5直接置于图案化设备6之上。所述图案化设备6与底座7相连。在一些实施方案中,所述图案化设备6由导电的箔或金属丝制成。
未沉积于层中的气体混合物的剩余物,包括反应副产物,用真空泵(未示出)从腔室内排出。确切地,所述气体通过环形孔8,经过向下延伸的气体通道10,通过真空关闭阀门13,进入通过前级线路(未示出)连接到外部真空泵(未示出)的排出口(未示出),从而排出。
图2所示的是在透明的或不透明的基材20上的典型结构,其包括在其外表面具有宏观的表面浮雕性图案22的硬质保护性透光层21。
用于基材的适合材料包括几乎所有用于注塑成型的塑性物,包括塑料材料如聚氯乙烯、聚碳酸酯、PC-ABS聚丙烯酸酯和PET,金属如不锈钢和其它合金钢、铝和镁合金。
所述基材可以用不同的技术预涂覆,例如塑料基材可以用打底涂层涂漆从而平整所述表面,以及可以在真空或电化学过程中金属化出厚度为10-100nm的金属层。该金属层可由铝、铟、铬、硅、铁、镍、锡或这些材料的合金构成。
典型的前驱体和所得的涂覆组合物覆盖基于前驱体如TMOS、HMDSO、HMDS、OCMTS等的透明涂料型SiOx,基于前驱体如TiCl4、四异丙氧化钛、(TiO)2(叔丁acctoacctatc)2、TiO[CH3COCH_C(O-)CH3]2的TiOx,以及TiOx和SiOx的合金及其他。氩气、氦气和氧气可以用作载气并促进区域9中等离子体的形成。PECVD沉积方法的沉积条件为本领域技术人员所熟知。层21和层22可基于相同或不同的前驱体在相似的沉积条件下制出。
在典型的制备执行过程中,PECVD反应器可设定(1)为沉积如上文所述的具有所需厚度的硬质涂层21而不使用图案化设备。在随后的步骤(2)中,通过将图案化设备定位在反应区域中基材的上方或下方在相同或相似的反应器中施加所述图案化的层22,并且。如果需要的话,可通过用重复步骤(2)的图案化但在图案化设备中用不同的图案化结构(孔大小、孔形式和孔间距)将微图案叠加(3)于由(2)得到的宏观图案上。
实施方案1
在一优选的实施方案中,基材由平的或弯曲的透明塑料材料如PMMA30构成。HMDS用作前驱体,氧气和氦气用作载气。首先,移除图案化设备的同时,施加SiOx的厚为2…10μm的层31。其次,用图案化设备施加约1…2μm厚的SiOx层32,如图3a所示。所述图案化设备由0.2mm厚的金属箔片构成,该金属箔片具有直径0.15mm,间隔约0.3mm的孔形成的规则图案。图3b示出了PMMA基材33的光透射率图样,具有硬质保护性层但没有图案化的层34,以及具有硬质保护性层且具有图案化的层35(在步骤2中)。其对干涉效应和相关条纹的抑制,以及反射的减少是显而易见的。
实施方案2
图4a示出了另一优选的实施方案,基材40由平的或弯曲的塑料材料如PC-ABS构成。首先通过涂漆施加10…15μm厚的底凃层41。在第二步骤中,在真空工艺中施加由铝、铟、铬、硅、铁、镍、锡或这些材料的合金构成的具有5到100nm厚度的金属层42。第三,2…10μm厚的SiOx的层43在去除图案化设备的同时进行施加。第四,约1…2μm厚的SiOx44层用图案化设备进行施加。所述图案化设备由0.2mm厚的金属箔片构成,该金属箔片具有直径0.15mm,间隔约0.3mm的孔形成的规则图案。
图4b示出了薄铟薄膜在PC-ABS基材45上的光学反射图样,具有硬质保护性层但没有图案化的层46,以及具有硬质保护性层且具有图案化的层47(步骤4中所述的)。对干涉效应及其相关条纹的抑制是显而易见的。
实施方案3
在另一优选的实施方案中,基材由平的或弯曲的透明塑料材料构成。首先通过涂漆施加10…15μm厚的底凃层。在第二步骤中,在真空工艺中施加厚度为10到100nm的金属层。第三,2…10μm的SiOx的厚层在去除图案化设备的同时进行施加。第四,约1…2μm厚的SiOx层用图案化设备施加。所述图案化设备由0.2mm厚的金属箔片构成,该金属箔片具有直径0.15mm,间隔约0.3mm的孔形成的规则图案。第五,附加的SiOx层用不同的图案化设备施加。该图案化设备由0.2mm厚的织物栅网构成,该织物栅网具有由0.065mm直径的线和140μm的栅网开口构成的孔所形成的规则图案。第六,所述表面用可商业获得的产品进行处理以形成薄(小于10nm)的斥水层。
作为所述斥水涂层和表面图案化组合效应的结果,所述表面成为自身超疏水性的,且达到超过150°的与水的接触角。
本发明可用其他具体的方式实现而不脱离本发明的精神或基本特征。所述实施方案在任何方面都应仅被理解为举例性说明而非限制。因此,本发明的范围因而是由所附的权利要求所限定而不是前述的说明。所有来自于权利要求的相同的含义和范围的改动都落入了其范围。在已详述了本发明的数个实施方案后,许多基于本发明的其他与沉积保护性PECVD层等同或替换的方法对本领域技术人员而言将是显而易见的。这些替换和等同的方法应包含在本发明的范围内。
Claims (25)
1.在基材上形成的化学气相法涂层,所述基材置于基本上真空的压力腔室中,其特征在于所述涂层是图案化的涂层,优选基本上波纹状的涂层。
2.根据权利要求1所述的涂层,其特征在于所述涂层的厚度优选在20-5000nm之间。
3.根据权利要求1或2所述的涂层,其特征在于将提供有大量通孔的结构基本上置于所述基材的上方。
4.根据权利要求3所述的涂层,其特征在于所述结构为具有通孔的板。
5.根据权利要求3所述的涂层,其特征在于所述结构为网眼状结构。
6.根据权利要求3所述的涂层,其特征在于所述结构为狭缝状结构。
7.根据权利要求1或2所述的涂层,其特征在于将阴极基本上置于所述基材之下,所述阴极具有绝缘结构,所述绝缘结构包括一组彼此被一定距离隔开的导电脊,所述脊与阴极连接。
8.根据权利要求1-7任一项所述的涂层,其特征在于所述涂层是基于SiOx的涂层。
9.根据权利要求1-7任一项所述的涂层,其特征在于所述涂层是基于TiOx的涂层。
10.根据权利要求1-9任一项所述的涂层,其特征在于所述涂层由多个直径在1-100μm,高度在0.01-0.5μm之间以及所述高度之间的距离在10-500μm之间的层构成。
11.根据权利要求1-10任一项所述的涂层,其特征在于所述基材为透明塑料材料的基材。
12.根据权利要求1-10任一项所述的涂层,其特征在于所述基材为金属的基材。
13.根据权利要求1-10任一项所述的涂层,其特征在于所述基材为不透明的塑料材料的基材。
14.根据权利要求1-10任一项所述的涂层,其特征在于所述涂层为超疏水性涂层,其水接触角大于100度。
15.根据权利要求1-14任一项所述的涂层,其特征在于首先在不使用赋予图案化的形状的结构的情况下在基材上形成优选厚度为2-10μm的第一层,以及在赋予图案化的形状的结构的辅助下在该第一层上形成优选厚度为1-2μm的第二层。
16.根据权利要求11所述的涂层,其特征在于在不使用赋予图案化的形状的结构的情况下,在透明塑性材料的基材上形成硬质保护性层,以及在赋予图案化的形状的结构的辅助下在该硬质保护性层上形成具有图案化形状的第二层。
17.根据权利要求11所述的涂层,其特征在于在透明塑料材料的基材上形成优选厚度为10-15μm的第一层,在该第一层上形成优选厚度为10-100nm的第二层,在不使用赋予图案化的形状的结构的情况下在该第二层上形成优选厚度为2-10μm的第三层,以及在赋予图案化的形状的结构的辅助下在该第三层上形成优选厚度为1-2μm的第四层。
18.用于沉积图案化的涂层的方法,其特征在于所述方法包括:
用等离子体增强化学气相沉积方法,通过图案化设备将图案化的涂层直接沉积在弯曲或平面的基材上。
19.根据权利要求18所述的方法,其特征在于所述图案化设备包括通孔以获得包含多个凸起的图案化的涂层。
20.根据权利要求19所述的方法,其特征在于所述凸起的直径在1-100μm之间,凸起的高度在0.01到0.5μm之间,以及凸起之间的间距在10-500μm之间。
21.形成在基材上形成的化学气相涂层的方法,在所述方法中,将气体混合物引入到位于基本上真空的压力腔室中的基材上,其特征在于所述基材被提供了具有大量通孔的结构,从而在所述具有大量通孔的结构的辅助下,在该基材的表面上形成图案化的涂层,优选地基本上波纹状的涂层。
22.根据权利要求18或21所述的方法,其特征在于在基本上真空的压力腔室中,在等离子体增强化学气相沉积的辅助下形成所述图案化的涂层。
23.根据权利要求18或22所述的方法,其特征在于由RF或微波技术产生等离子体,所述基材置于与等离子体产生和移除相同的腔室中。
24.根据权利要求18或22所述的方法,其特征在于置于基本上真空的压力腔室中的所述基材与RF电源相连。
25.包括基材和根据权利要求1-17任一项所述的涂层的产品。
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Cited By (9)
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CN102815052A (zh) * | 2012-06-29 | 2012-12-12 | 法国圣戈班玻璃公司 | 超疏水减反基板及其制作方法 |
CN102815052B (zh) * | 2012-06-29 | 2016-08-24 | 法国圣戈班玻璃公司 | 超疏水减反基板及其制作方法 |
CN106126768A (zh) * | 2015-05-06 | 2016-11-16 | 波音公司 | 用于空气动力微观结构的光学效果 |
CN106126768B (zh) * | 2015-05-06 | 2021-11-02 | 波音公司 | 用于空气动力微观结构的光学效果 |
CN107949658A (zh) * | 2015-09-21 | 2018-04-20 | Posco公司 | 经过显色处理的基板及该基板的显色处理方法 |
CN107779815A (zh) * | 2016-08-24 | 2018-03-09 | 现代自动车株式会社 | 用于涂布车辆运转部件的表面的方法以及通过该方法制造的车辆运转部件 |
CN107779815B (zh) * | 2016-08-24 | 2021-04-02 | 现代自动车株式会社 | 用于涂布车辆运转部件的表面的方法以及通过该方法制造的车辆运转部件 |
CN108059359A (zh) * | 2017-12-11 | 2018-05-22 | 大连理工大学 | 一种具有复合润湿性特征的表面的制备方法 |
CN108059359B (zh) * | 2017-12-11 | 2020-11-10 | 大连理工大学 | 一种具有复合润湿性特征的表面的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
FI20080248A0 (fi) | 2008-03-28 |
FI20080248L (fi) | 2009-09-29 |
WO2009118457A1 (en) | 2009-10-01 |
JP2011515586A (ja) | 2011-05-19 |
US20110097551A1 (en) | 2011-04-28 |
WO2009118457A8 (en) | 2011-02-03 |
EP2260121A1 (en) | 2010-12-15 |
AU2009229013A1 (en) | 2009-10-01 |
CA2719306A1 (en) | 2009-10-01 |
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