CN101384926B - 涂层系统 - Google Patents

涂层系统 Download PDF

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CN101384926B
CN101384926B CN2007800055229A CN200780005522A CN101384926B CN 101384926 B CN101384926 B CN 101384926B CN 2007800055229 A CN2007800055229 A CN 2007800055229A CN 200780005522 A CN200780005522 A CN 200780005522A CN 101384926 B CN101384926 B CN 101384926B
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CN101384926A (zh
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延斯·克里斯托·蒂斯
帕特里克·威廉默斯·安东尼厄·韦瑞嘉德豪温
纳尼·乔格·阿福斯坦
赫曼努斯·阿德里安努·兰格曼斯
爱丽丝·戴尔科特兰康
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Abstract

本发明提供了一种涂层系统，所述系统具有抗反射功能和UV吸收功能。本发明进一步提供了包括上述系统的方法、用途和制品。

Description

涂层系统
本发明涉及一种涂层系统。具体地，本发明涉及一种对紫外线(UV)辐射具有低反射性和低透射性的涂层系统。
UV辐射对于各种材料具有不利影响。例如，它会导致材料变黄和/或导致退色。具有高价值的产品诸如艺术品被暴露时尤其会存在上述问题，而对于较为普通的产品诸如窗帘、地毯、壁纸等也会存在上述问题。另外，UV辐射会使某些材料降解。
UV控制膜(UV control film)是已知的。参见例如美国专利4,275,118、美国专利4,455,205、美国专利4,799,963和欧洲专利0732356。也存在基于有机UV吸收剂的可商购薄膜。
本发明提供了一种涂层系统，该涂层系统具有抗反射功能和UV吸收功能。本发明还提供了包括上述系统的方法、用途以及制品。
本文中所用术语“纳米粒子”指胶体粒子，其初级粒子尺寸小于1μm，优选小于500nm，更优选小于350nm。
本文中所用术语“粘合剂”指，一种可以使粒子之间、优选也使粒子与基材之间发生化学交联的物质。
本文中所用术语“预水解”指，使金属烷氧化物粘合剂前驱体水解至通过部分缩合会产生低聚物的点而非水解至形成凝胶的点。
除非另有声明，本文中的所有参考文献通过引用插入本文。
在一个实施方式中，本发明包括基材，含有氧化铈、氧化钛或氧化锌或其组合粒子的涂层以及含有金属氧化物纳米粒子的涂层。
任何适当的基材都可用在本文中。优选地，所述基材允许在可见光光谱和UV光谱范围内的光透过。优选地，所述基材是透明的或半透明的。所述基材优选具有高透明度。优选地，在厚度为2mm，波长为425至675nm的情况下，透明度为约94％或更高，更优选为约96％或更高，甚至更优选为约97％或更高，甚至更优选为98％或更高。
本文中的基材可以为有机基材。例如，所述基材可以为有机聚合物，诸如聚萘二甲酸乙二醇酯(PEN)、聚碳酸酯或聚甲基丙烯酸甲酯(PMMA)、聚酯或具有类似光学性质的有机材料。在这个实施方式中，优选使用的涂层可以在足够低的温度下固化，从而有机材料基本上保持其形状并且基本上不会由于热降解而发生变化。正如EP-A-1591804所述，优选的方法使用催化剂。WO2005/049757描述了另一种优选的固化方法。
本文中的基材可以为无机基材，优选玻璃或石英。优选的是浮法玻璃(float glass)。一般而言，玻璃板的厚度为0.5mm或更厚，优选为1mm或更厚，最优选为约1.8mm或更厚。一般而言，玻璃板的厚度为约20mm或更薄，优选为约10mm或更薄，更优选为约6mm或更薄，更优选为约4mm或更薄，最优选为约3mm或更薄。
本发明的系统包括UV保护层。该层优选被直接涂敷到基材上。该层包括氧化铈、氧化钛、氧化锌或其组合的粒子。优选地，该层包括二氧化铈、二氧化钛、氧化锌或其组合的粒子。优选地，该层包括氧化铈的粒子，更优选包括二氧化铈的粒子。
令人惊讶地发现，当对涂层组合物的pH进行控制时，该层更稳定且更容易处理。优选地，pH小于约6，更优选小于约5.5。
优选地，UV保护层包括粘合剂。优选地，粘合剂与粒子和基材之间形成共价键。为了这个目的，粘合剂在固化前优选包括带有烷基或烷氧基的无机化合物。而且，优选粘合剂本身发生聚合，从而形成基本上连续的聚合网络。
在一个实施方式中，UV层的粘合剂基本上由无机粘合剂组成。所述无机粘合剂优选由一种或更多种无机氧化物得到。优选地，粘合剂是可水解的化合物，诸如金属烷氧化物。优选地，粘合剂选自烷氧基硅烷、烷氧基锆酸盐、烷氧基铝酸盐、烷氧基钛酸盐、烷基硅酸盐、硅酸钠及其混合物。优选的是烷氧基硅烷，优选三烷氧基硅烷和四烷氧基硅烷。优选地，使用乙基硅酸盐、钛酸盐、锆酸盐和/或钛酸盐。最优选的是四烷氧基硅烷。
优选地，粘合剂被“预水解”。也就是说，粘合剂在与粒子进行配制前已经过一定程度的水解作用。
粒子与粘合剂之间的反应优选在溶剂中进行，该溶剂优选为水和有机溶剂的混合物。取决于粘合剂的化学性质，许多溶剂是可用的。合适的溶剂包括，但不限于，水、非极性有机溶剂、醇及其组合。合适的溶剂的实例包括，但不限于：异丙醇、乙醇、丙酮、乙基纤维素溶剂(ethylcellosolve)、甲醇、丙醇、丁醇、乙二醇、丙二醇、甲基-乙基-醚、甲基-丁基-醚、甲苯、甲基-乙基-甲酮及其组合。
UV吸收能力随着粒子浓度的增加而增强。然而，这也可能由于缺乏粘合剂而导致稳定性问题。因此，物理性质和UV吸收性之间总是存在一个动态平衡。一种增强UV吸收的方法是，添加掺杂剂。例如，钛掺杂剂可被添加到粒子中。
优选地，该层中粒子与粘合剂的重量比为约100∶1至约1∶100，更优选为约10∶1至约1∶10，甚至更优选为约5∶1至约1∶5。
优选地，该层具有约50nm至约500nm的干厚度。更优选地，该层具有约100nm至约250nm的厚度。
优选地，UV溶液通过如下制备：使粒子与粘合剂进行反应，并且允许该反应继续直到基本上完成。然后，添加更多的粘合剂到如上经预反应的粒子中。惊人的是，这有助于避免形成不希望的凝胶并且更容易涂敷到基材上。
该层可以以任何适当的方式涂敷到基材上。优选的涂敷方法包括，弯月面(吻合)涂布(meniscus(kiss)coating)、喷涂、辊涂、旋转涂布和浸涂。优选地，该层通过如下来涂敷：将基材浸渍在涂料组合物中然后取出。为了改善涂层的均匀程度，优选恒速拉出。可以涂敷第二层从而提供额外的UV保护。
本文中优选的涂布方法包括：
(i)清洁基材；
(ii)将所述基材浸渍在含有粒子和粘合剂的溶液中；
(iii)以基本上恒定的速率拉出所述基材；
(iv)使溶剂蒸发。
本发明的系统包括抗反射(AR)层。AR层优选包括金属氧化物的纳米粒子。合适粒子的实例包括，但不限于：含有氟化锂、氟化钙、氟化钡、氟化镁、二氧化钛、氧化锆、锑掺杂的氧化锡、氧化锡、氧化铝、二氧化硅及其混合物的粒子。优选地，粒子包括二氧化硅。更优选地，粒子包括至少90重量％的二氧化硅。
优选地，纳米粒子的长度小于1000nm，更优选小于500nm，甚至更优选小于350nm。
在一个实施方式中，粒子优选具有至少1.5的平均长径比。优选地，粒子的平均长径比至少为2，更优选至少为4，甚至更优选至少为6，还要更优选至少为8，甚至更优选至少为10。优选地，长径比约为100或更小，优选约为50或更小。
粒子的尺寸可以通过如下来测定：使粒子的稀悬浮液分散在一表面上，并利用显微技术(优选电子扫描显微镜(SEM)或原子力显微镜(AFM))来测量单个粒子的尺寸。优选地，通过测量至少100个单个粒子的尺寸来确定平均尺寸。长径比为粒子的长度与宽度的比。在棒状和蠕虫状粒子的情况下，长度为粒子两点间最远的距离，而宽度为垂直于粒子的中心轴测量的最大直径。在显微镜下观察粒子的投影来测量长度和宽度二者。
本文涂层中的AR层可以包括不同尺寸和形状粒子的混合物。
在一个实施方式中，本文中所用的粒子是非球形粒子，诸如棒状粒子或蠕虫状粒子，优选蠕虫状粒子。蠕虫状粒子是中心轴偏离直线的粒子。蠕虫状粒子的实例为商品名Snowtex(IPA-ST-UP)、直径为9-15nm、长度为40-300nm的粒子，可得自Nissan Chemical。此后，棒状和蠕虫状粒子也被称为细长粒子。
在优选的实施方式中，本文中所用粒子基本上是球形的。优选地，球形粒子具有约1.2或更小，优选约1.1或更小的平均长径比。优选地，粒子具有约10nm或更大，优选20nm或更大的平均尺寸。优选地，粒子具有200nm或更小，优选150nm或更小，甚至更优选约100nm或更小的平均尺寸。基本上球形的粒子具有如下优点：它们形成的涂层中，粒子间隙间的纳米孔的体积相对于由非球形粒子形成的体积要小。因此，涂层很少会由于毛细作用力而使纳米孔填充，从而不会导致抗反射性能的损失。这些粒子可以具有窄粒子尺寸分布或宽粒子尺寸分布，优选具有宽粒子尺寸分布。
本文中的粒子通常被提供在溶剂中。例如，溶剂可以为水或醇，诸如甲醇、乙醇或异丙醇(IPA)。
纳米粒子优选与表面改性剂发生反应，从而得到与粘合剂反应的粒子。表面改性剂与纳米粒子发生反应会使粒子具有活性，从而使其能更有效地与粘合剂进行反应。表面改性剂优选为能够形成氧化物的试剂。优选地，表面改性剂为可水解的化合物，诸如金属烷氧化物。合适的实例包括，但不限于：烷氧基硅烷、烷氧基锆酸盐、烷氧基铝酸盐、烷氧基钛酸盐、烷基硅酸盐、硅酸钠及其混合物。优选使用烷氧基硅烷，更优选使用三烷基硅烷和四烷基硅烷。更优选四烷基硅烷。
一般而言，反应在溶剂中进行。取决于粘合剂的化学性质，许多溶剂都可用。溶剂的适合实例包括，水、非极性有机溶剂和醇。合适溶剂的实例包括，但不限于：异丙醇、乙醇、丙酮、乙基纤维素溶剂、甲醇、丙醇、丁醇、乙二醇、丙二醇、甲基-乙基-醚、甲基-丁基-醚、1-甲氧基丙-2-醇、甲苯、甲基-乙基甲酮及其混合物。优选的是异丙醇、乙醇、甲醇、丙醇及其混合物。
AR层优选包括粘合剂。粘合剂的主要作用在于，保持表面活性粒子附着在基材上。优选地，粘合剂与粒子和基材形成共价键。为了这个目的，粘合剂在固化前优选包括带有烷基或烷氧基的无机化合物。而且，优选粘合剂本身发生聚合，从而形成基本上连续的聚合网络。
在本发明的一个实施方式中，涂层的粘合剂基本上由无机粘合剂组成。所述无机粘合剂优选由一种或更多种无机氧化物得到。优选地，粘合剂是可水解的化合物，诸如金属烷氧化物。优选地，粘合剂选自烷氧基硅烷、烷氧基锆酸盐、烷氧基铝酸盐、烷氧基钛酸盐、烷基硅酸盐、硅酸钠及其混合物。优选的是烷氧基硅烷，优选三烷氧基硅烷和四烷氧基硅烷。优选地，使用乙基硅酸盐、钛酸盐、锆酸盐和/或钛酸盐。最优选的是四烷氧基硅烷。
优选地，溶液的pH约为2或更高，更优选约为3或根高。pH优选约为5.5或更低，更优选约为4.5或更低。
纳米粒子与粘合剂以一定的比率进行混合，从而得到所需光学性质和机械性质。除了粒子和粘合剂以外，还可以添加其它组分，诸如其它溶剂、催化剂、疏水试剂、流平剂等。在一个实施方式中，本发明的涂层组合物包括：
(i)金属氧化物纳米粒子，
(ii)金属氧化物基粘合剂，
其中，(i)与(ii)中金属氧化物的重量比为99∶1至1∶1。优选地，金属氧化物的重量比为85∶1至3∶2，更优选为65∶1至2∶1。
优选地，AR层涂敷到基材制品上，从而使所得干涂层厚度为约50nm或更厚，优选为约70nm或更厚，更优选为90nm或更厚。优选地，干涂层的厚度为约300nm或更薄，更优选为200nm或更薄。
AR层可以以任何适当的方式涂敷到基材上。优选地，AR层在UV保护层以后涂敷。优选地，AR层被涂敷到UV保护层的顶部。优选的涂敷方法包括，弯月面(吻合)涂布、喷涂、辊涂、旋转涂布和浸涂。优选的是浸涂，因为它为所浸渍基材的所有侧面提供涂层，并使厚度可重复且恒定。如果使用较小玻璃板(例如宽度或长度为20cm或更小)，那么易于使用旋转涂布。弯月面涂布、辊涂和喷涂可用于连续工艺。
令人惊奇地，本发明的AR层可以容易地涂敷到UV保护层的顶部，而不会显著影响两者任意一方的功能，甚至在涂敷AR层以前不需固化UV保护层。本发明系统的优选实施方式包括：
(i)采用UV保护层涂覆基材；
(ii)在所述UV保护层的顶部涂覆AR层。
优选地，本发明的涂层系统如下：当在425至675nm的波长(可见光区域)下对一个涂覆侧面进行测量时，最小反射约为2％或更低，优选约为1.5或更低，更优选约为1％或更低。在425至675nm的区域上，一侧的平均反射优选约为2.5％或更低，更优选约为2％或更低，甚至更优选约为1.5％或更低，还要更优选约为1％或更低。一般而言，在425至650nm的波长下，优选在450nm或更高的波长下，更优选在500nm或更高的波长下，反射最小。
可以采用耐钢丝性来测定机械性质。优选地，涂层系统具有“可接受的”耐钢丝性，所述“可接受的”耐钢丝性被定义为，采用负载250g的0000号钢丝擦拭10次后，存在小于10条的可见擦痕。更优选地，耐钢丝性为“优良”，所述优良耐钢丝性被定义为，采用负载250g的0000号钢丝擦拭10次后，存在3条或更少的可见擦痕。
优选地，本发明的系统使通过基材的UV透射减少了50％或更多，更优选减少了60％或更多，甚至更优选减少了70％或更多。
优选地，至少约20％或更多，优选约50％或更多，甚至更优选约90％或更多的基材的表面之一被本发明的系统涂覆。
对于所有的涂覆过程，清洁是重要的步骤，因为少量污染物(诸如灰尘、油脂和其它有机化合物)会导致抗反射涂层或其它涂层具有缺陷。可以以多种方式进行清洁，诸如烘烤(如果所使用的无机基材可承受的话，加热至600-700℃)；和/或采用清洁液体(例如在软化水中的肥皂、醇、或酸性或碱性洗涤体系)清洁。当使用清洁液体时，通常将玻璃板在20℃至400℃的温度下可选通过空气流进行干燥。
在一个实施方式中，包括本发明系统的基材用于图画、照片、油画、海报、铜版画、画像、织物、挂毯等的框架。
本发明的系统还可用于如下应用，诸如陈列柜、建筑玻璃、太阳能电池板、汽车玻璃等。
本发明通过以下实施例进一步阐述，但并不局限于此。
实施例
将98g四乙氧基硅烷(TEOS)加入267g异丙醇(IPA)、90g水和10g乙酸中，然后在室温(RT)下搅拌72小时。然后，用270g IPA和2g浓盐酸来稀释该混合物。这形成了预水解的TEOS。
将91.22g IPA与31.36g Snowtex(IPA-ST-UP，在IPA中为15.6wt％)粒子、11.76g TEOS和15.66g水进行混合。将该溶液在80℃下搅拌4小时。然后，将150g IPA连同11.5g预水解的TEOS一起加入。这形成了AR配制品。
将60g二氧化铈粒子与2.25g TEOS进行混合，并搅拌三小时。然后，将4.3g TEOS连同93.5g IPA一起加入。这形成了UV配制品。
将玻璃板(10cm×10cm)进行洗涤并擦洗，然后将其浸入UV配制品的溶液中4秒钟。以0.33cm/s的恒定速度取出玻璃板。蒸发溶剂。该过程再重复三次。然后，将玻璃板浸入AR配制品中4秒钟，并以0.2cm/s的速率拉出。
所得玻璃板在450℃下固化4小时。
该玻璃板对UV辐射的透射减少了75％，在470nm下的反射为0.42％。
然后，对该玻璃板进行耐磨损测试。在平坦的圆形钢表面(直径＝2.1cm)上均匀地覆盖正常重量为250g的钢丝(等级：0000)。然后，将钢丝在表面上往复移动5次，从而在5至10cm的距离上总共擦拭10次。此时，对涂层的表面进行目测，并根据可见擦痕的数目来分级。0-3条擦痕为A级；4-10条擦痕为B级；11-15条擦痕为C级；16-30条擦痕为D级；涂层被完全除去为E级。上述实施例的玻璃板为A级。

Claims (10)

1.一种涂层系统，所述系统由如下部分组成：
(i)基材；
(ii)紫外线保护层，所述紫外线保护层包括氧化铈、氧化钛、氧化锌或其混合物的粒子，所述紫外线保护层的干厚度在50至250nm之间，所述紫外线保护层使通过基材的紫外线透射减少了50％或更多；
(iii)抗反射层，所述抗反射层包括金属氧化物纳米粒子；
其中，当在425至675nm的波长下对一个涂覆侧面进行测量时，最小反射约为2％或更低。
2.如权利要求1所述的系统，其中，所述紫外线保护层包括氧化铈。
3.如权利要求1-2中任意一项所述的系统，其中，所述基材选自聚萘二甲酸乙二醇酯、聚碳酸酯或聚甲基丙烯酸甲酯(PMMA)、聚酯、石英、玻璃及其组合。
4.如权利要求1-2中任意一项所述的系统，其中，所述紫外线保护层包括粘合剂。
5.如权利要求1-2中任意一项所述的系统，其中，所述抗反射层包括粘合剂。
6.如权利要求1-2中任意一项所述的系统，其中，所述抗反射层包括二氧化硅纳米粒子。
7.如权利要求1-2中任意一项所述的系统，其中，所述紫外线层通过包括如下步骤的方法来制备：
(i)使所述粒子与粘合剂反应，
(ii)将更多的粘合剂加入经预反应的粒子中。
8.被固化的如权利要求1-2中任意一项所述的涂层系统。
9.如权利要求1-8中任意一项所述的涂层系统用于提供玻璃框架的用途。
10.一种制品，其包括权利要求1-8中任意一项所述的涂层系统。
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