CN102405533A - 用于光学透明基板的抗反射涂层 - Google Patents

用于光学透明基板的抗反射涂层 Download PDF

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CN102405533A
CN102405533A CN2010800172760A CN201080017276A CN102405533A CN 102405533 A CN102405533 A CN 102405533A CN 2010800172760 A CN2010800172760 A CN 2010800172760A CN 201080017276 A CN201080017276 A CN 201080017276A CN 102405533 A CN102405533 A CN 102405533A
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S·穆克霍帕赫亚伊
Y·潘迪
L·丹克斯
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Abstract

本发明描述了抗反射涂层和涂层溶液，光学透明元件以及制备抗反射涂层和涂层溶液的改进工艺。所述抗反射涂层由至少两种不同的烷氧基硅烷材料经碱催化反应形成。

Description

用于光学透明基板的抗反射涂层
相关申请
本申请主张享有根据美国法典35U.S.C§119(e)条具有的、2009年6月10日提交的、临时申请序列号为：61/268231、标题为“ANTI-REFLECTIVECOATINGS FOR SOLAR MODULE GLASS AND SOLAR CELLS AND LENS(用于太阳能模块玻璃和太阳能电池和透镜的抗反射涂层)”的利益。该申请全文在此以引用方式引入。
技术领域
本申请一般涉及用于光学透明元件的抗反射涂层，且更具体地涉及用于在光电电池应用中使用的玻璃盖板的抗反射涂层。
背景技术
抗反射(AR)涂层被应用于包括光电(PV)模块制造的数种工业中，以降低当光穿过光学透明元件如玻璃时入射光的反射率。AR涂层的目标是折射率尽可能接近1.23以使宽波长带的光的透射最大化。
一层或多层低折射率涂层能够提高宽波长范围和宽范围的入射角度下的透射率。这些涂层可以以溶胶-凝胶材料形式沉积(在大气压力下或非真空下)形成，并且是高度成本有效的。已经有报道，可以由二氧化硅溶胶-凝胶通过常规涂覆技术施涂在玻璃盖板上而形成的这些薄的抗反射涂层，使光谱中可见光波段的阳光透射率提高了百分之二到百分之三。这样的溶胶-凝胶已经由数种机理形成，包括通过烷氧基硅烷的水解/缩合反应。参见，例如，G.Wu等，“A novelroute to control refractive index of sol-gel derived nanoporous films used as broadbandantireflective coatings(控制用作宽带抗反射涂层的溶胶-凝胶衍生纳米多孔膜的折射率的新方法)”，Materials Scinece and Engineering(材料科学与工程)B78(2000)，第135-139页。不管怎样，由二氧化硅涂层形成的AR涂层将受益于提高的硬度、粘合性、贮藏寿命和/或工艺效率。
发明内容
这里公开的实施方案涉及AR涂层和涂层溶液，光敏元件如应用AR涂层的光电模块，和用于制备AR涂层和涂层溶液的改进工艺。
第一个实例提供了一个光学透明元件，其包括光学透明基板；和设置在光学透明基板的至少一个表面上的抗反射涂层，该抗反射涂层包含聚合物，该聚合物包含至少一个四烷氧基硅烷残基；和选自由三烷氧基硅烷，二烷氧基硅烷，单烷氧基硅烷及其组合构成的组中的至少一个第二种烷氧基硅烷残基，其中该聚合物相对于聚合物的总摩尔量含有至少50％摩尔百分含量的该至少一个四烷氧基硅烷残基，且该涂层含有平均尺寸不大于100nm的的聚合物粒子。
第二实例提供了权利要求1的光学透明元件，其中所述至少一个烷氧基硅烷残基是四乙氧基硅烷。第三实例提供了如实例1-2任何一项的光学透明元件，其中该第二种烷氧基硅烷残基选自由甲基三乙氧基硅烷和乙烯基三乙氧基硅烷构成的组。第四实例提供了如实例1-3任何一项的光学透明元件，其中该至少一个四烷氧基硅烷残基是四乙氧基硅烷且该第二种烷氧基硅烷是甲基三乙氧基硅烷。
第五实例提供了如实例四的光学透明元件，进一步包含乙烯基三乙氧基硅烷残基。第六实例提供了如实例1-5任何一项的光学透明元件，其中聚合物基本由四乙氧基硅烷残基和甲基三乙氧基硅烷残基组成且具有15到100nm的平均粒子尺寸。第七实例提供了如实例1-6任何一项的光学透明元件，其中该聚合物进一步含有金属醇盐残基。
第八实例提供了如实例1-7任何一项的光学透明元件，其中该聚合物进一步含有异丙氧基钛残基。第九实例提供了如实例1-8任何一项的光学透明元件，其包含至少约20％摩尔百分含量的所述第二种烷氧基硅烷残基。第十实例提供了如实例1-9任何一项的光学透明元件，其包含约20％摩尔百分含量到40％摩尔百分含量的所述第二种烷氧基硅烷残基。
第十一实例提供了一种光电模块，其包括至少一层半导体层；设置在该至少一层半导体层上的光学透明层；和设置在该光学透明基板的至少一个表面上的抗反射涂层，该抗反射涂层包含聚合物，该聚合物包含至少一个四烷氧基硅烷残基；和选自由三烷氧基硅烷、二烷氧基硅烷、单烷氧基硅烷及其组合构成的组中的至少一个第二种烷氧基硅烷残基，其中该聚合物含有相对于聚合物的总摩尔量至少50％摩尔百分比的该至少一个四烷氧基硅烷残基，且该涂层含有平均尺寸不大于100nm的聚合物粒子。
第十二实例提供了如实例11的光电模块，其中该至少一个四烷氧基硅烷是四乙氧基硅烷和该第二种烷氧基硅烷残基选自由甲基三乙氧基硅烷和乙烯基三乙氧基硅烷及其组合构成的组。
第十三实例提供了一种制备涂层溶液的方法，其包括混合至少第一种四烷氧基硅烷材料，第二种烷氧基硅烷材料，碱催化剂和溶剂来形成涂层，其中该第二种烷氧基硅烷材料选自由三烷氧基硅烷，二烷氧基硅烷，单烷氧基硅烷及其组合构成的组；在足够的温度下保持涂层溶液的pH值一段充分的时间以形成具有约15nm到约100nm平均粒子尺寸的聚合物粒子；和降低涂层溶液的pH值到低于约5.0。
第十四实例提供了如实例13的制备方法，其中该碱催化剂包含至少一种季铵。
第十五实例提供了如实例13-14任何一项的方法，其中该碱催化剂包含四丁基铵氢氧化物、四甲基铵氢氧化物或其组合。第十六实例提供了如实例13-15任何一项的方法，其中该涂层溶液在降低pH值之前被维持在约35℃到约70℃之间约1小时到约5小时。
第十七实例提供了如实例13-16任何一项的方法，其中该溶液含有水。第十八实例提供了如实例13-17任何一项的方法，其中pH值被降至不大于2.0。第十九实例提供了如实例13-18任何一项的方法，其进一步包括存储该涂层溶液至少约24小时的步骤。第二十实例提供了如实例13-19任何一项的方法，其进一步包括冷冻该涂层溶液的步骤。
第二十一实例提供了一种形成光学透明元件的方法，其包括分配涂层溶液至光学透明基板上，该涂层溶液由以下步骤形成：混合至少第一种四烷氧基硅烷材料，第二种烷氧基硅烷材料，碱催化剂和溶剂，其中该第二种烷氧基硅烷材料选自由三烷氧基硅烷，二烷氧基硅烷，单烷氧基硅烷及其组合构成的组，在足够的温度下维持涂层溶液的pH值一段充分的时间以形成具有约15nm到约100nm平均粒子尺寸的聚合物粒子，和降低涂层溶液的pH值到低于约5.0；和固化该分配的涂层溶液以在光学透明基板上形成抗反射涂层。
第二十二实例提供了如实例21的方法，其中该涂层溶液由喷雾分配。第二十三实例提供了如实例21-22任何一项的方法，其中在分配之前，该涂层溶液由冷冻状态转变至液态。第二十四实例提供了由实例21-23任何一项的方法制备的光学透明元件。
第二十五实例提供了一种抗反射涂层溶液，其包含聚合物，该聚合物包含：至少一个四烷氧基硅烷残基，和选自由三烷氧基硅烷，二烷氧基硅烷，单烷氧基硅烷及其组合构成的组中的至少一个第二种烷氧基硅烷残基，其中该聚合物相对于聚合物的总摩尔量含有至少50％摩尔百分含量的该至少一个四烷氧基硅烷残基，且该涂层含有平均尺寸不大于100nm的聚合物粒子；溶剂，其中该涂层溶液具有的聚合物粒子浓度最高约25wt％和粘度不大于2.0cP，且其中该涂层溶液在25℃下至少24小时具有不大于2.0cP的粘度和不大于5.0的pH值。
第二十六实例提供了如实例25的抗反射涂层溶液，其中该聚合物基本由四乙氧基硅烷残基和甲基三乙氧基硅烷残基组成。
附图说明
图1是依据本发明一个实施方案的制备含有AR涂层的光学透明元件的方法的流程图。
图2是依据本发明一个实施方案的含有AR涂层的光电电池的示意图。
图3是依据本发明一个实施方案的聚合物分子片段的示意图。
发明详述
图1是依据一个实施方案形成AR涂层溶液和光学透明元件的方法10的流程图。根据该方法10，AR涂层溶液通过在溶剂中并在碱催化剂存在下在合适的反应条件下混合至少两种不同烷氧基硅烷材料，从而引起所述烷氧基硅烷材料的聚合(方块20)来形成。该生成的AR涂层溶液包含具有至少两种不同烷氧基硅烷残基的聚合物。
在混合所述烷氧基硅烷材料后，可以将酸加入到该AR涂层溶液中以调节该溶液的pH值(方块30)，和/或所述AR涂层溶液可以进一步与至少一种额外的溶剂混合(方块40)。在一个实施方案中，示例的AR涂层溶液的形成不使用制孔剂，如聚乙二醇或聚环氧乙烷，它们在热处理步骤中蒸发而形成孔隙。另外，所述AR涂层溶液的形成不用象在其它反应方法中所需要的那样必需从反应溶液中过滤出生成的聚合物或者去除溶液中的成分。
所述AR涂层溶液被分配到光学透明基板上，如玻璃基板(如，碱石灰玻璃，浮法玻璃，硼硅酸盐和低铁碱石灰玻璃)，塑料盖板，丙烯酸菲涅耳(Fresnel)透镜或其它光学透明基板(方块50)。所述AR涂层溶液随后被固化以在光学透明基板上形成AR涂层(方块60)。
各种市售可得的烷氧基硅烷可以被用于形成AR涂层溶液。构成所述至少两种烷氧基硅烷材料中的第一种的合适的烷氧基硅烷包括四烷氧基硅烷，其可以含有一个或多个乙氧基，甲氧基，和/或丙氧基基团以及氢，甲基，乙基或丙基基团。在一个实施方案中，所述烷氧基硅烷材料的至少一种是四乙氧基硅烷(TEOS)。
第二种烷氧基硅烷材料可以被加入以提高改进的AR涂层的粘合性和/或其它改进的涂层性质。这些材料的实例包括三烷氧基硅烷，例如甲基三乙氧基硅烷(MTEOS)，氨基丙基三乙氧基硅烷(APTEOS)和三氟甲磺酸-APTEOS盐，乙烯基三乙氧基硅烷(VTEOS)，和二乙基磷酸(phosphato)乙基三乙氧基硅烷。实例还包括二烷氧基硅烷如甲基二乙氧基硅烷(MDEOS)，二甲基二乙氧基硅烷(DMDEOS)和苯基二乙氧基硅烷(PDEOS)。合适的单烷氧基硅烷包括三甲氧基硅烷例如(3-环氧丙氧基(glycidoxy)丙基)-三甲氧基硅烷。碳硅烷(carbosilane)，巯基硅烷，氢化(hydrido)硅烷和硅氮烷如二甲基二硅氮烷也可能是合适的。这些第二种烷氧基硅烷材料的组合也可使用。例如，MTEOS和/或VTEOS可特别适于提高粘合性和/或硬度。在一个实施方案中，所述第二种烷氧基硅烷材料或材料的组合可以与第一种烷氧基硅烷混合，相对于烷氧基硅烷材料的总摩尔量，其量的范围为从最高约50mol％到40mol％到35mol％到25mol％到15mol％。在另一个实施方案中，所述第二种烷氧基硅烷材料相对于两种烷氧基硅烷材料的总摩尔量以至少约10mol％到至少约40mol％的量被添加。第一种烷氧基硅烷与第二种烷氧基硅烷材料的摩尔比可以在1∶1-1000∶1，更优选10∶1到500∶1且甚至更优选25∶1到100∶1的范围内。
除了所述烷氧基硅烷材料外，所述AR涂层溶液中可以含有至少一种金属醇盐。合适的金属醇盐包括金属异丙醇盐和金属丁醇盐。金属异丙醇盐的实例包括异丙醇锆和异丙醇钛(TIPO)。合适的金属丁醇盐的实例包括正丁醇铪和正丁醇锆。TIPO可以特别适合于提高AR涂层的硬度。在一个实施方案中，所述AR涂层溶液相对于金属醇盐和烷氧基硅烷的总摩尔量含有少于1mol％的金属醇盐。
前述材料的组合可以用来实现所需的涂层性质。在一个实施方案中，所述AR涂层溶液包含TEOS和MTEOS。在另一个实施方案中，所述AR涂层溶液包含TEOS，MTEOS，VTEOS。在另一个实施方案中，所述AR涂层溶液包含TEOS，MTEOS，VTEOS和TIPO。
被加入到所述AR涂层溶液中的合适的碱催化剂包括，例如，季铵化合物，其通式为R1R2R3R4N+OH-，其中R1，R2，R3，R4各自独立地是苯基，氢或C1-16烷基。在一些实施方案中，合适的碱催化剂包括氢氧化季铵，例如氢氧化四丁基铵和氢氧化四甲基铵。在一些实施方案中，合适的碱催化剂包括含有这些组分的水溶液，且可以任选在碱催化剂水溶液中所存在的水之外含有额外的蒸馏水。
在AR涂层溶液中可以使用的合适的溶剂或稀释剂的实例包括但不限于丙酮，水，丙二醇甲基醚醋酸酯(PGMEA)，异丙醇(IPA)，四氢呋喃(THF)，乙醇，二丙二醇，四甘醇，乙酸乙酯，PGME和其组合。在一些实施方案中，所述溶剂是无丙酮的。
这些组分可以在例如有夹套的搅拌釜式反应器(STR)中被混合并反应，通过间歇或半连续模式反应约1小时到约6小时，更优选1到3.5小时的适合反应时间，且在约35℃到70℃的适合温度范围内进行。
在前述的条件下，在溶液中发生水解反应生成聚合物。依据反应条件，包含在溶液中的所述聚合物可以发生变化，从线性或无规支化链，到多孔基质，到致密胶体粒子。在任何情况下，生成的聚合物将包含上述至少两种不同的烷氧基硅烷材料和/或任选的金属醇盐材料的残基。这里使用的术语“残基”是指由最初加入AR涂层溶液的烷氧基硅烷和/或金属醇盐材料衍生出的聚合物分子部分。例如，通常知道四乙氧基硅烷在前述条件下反应生成SiO4单元，该单元构成了四乙氧基硅烷残基的一个实例。还应承认，可能形成某些副产物并包含在AR涂层溶液中，作为聚合物的部分或作为独立的成分。例如，TEOS的水解可能生成副产物乙醇。图3示意了一个具有所圈起来的特定残基的示例聚合物分子部分的画面。
在任何情况下，所述聚合物包含至少两种不同的由前面讨论的烷氧基硅烷材料衍生而来的烷氧基硅烷残基。在一个实施方案中，所述聚合物包括至少一个TEOS残基，至少一个MTEOS残基或两者。在另一个实施方案中所述聚合物还包括至少一个VTEOS残基。在另一个实施方案中，所述聚合物还包括至少一个TIPO残基。
为了进一步控制反应条件，在合适的反应时间之后，AR涂层溶液的pH值可使用酸，如硝酸，被调至约0到约4.0之间，更具体地，从约0到约2.0之间，甚至更具体地，从约0.5到约1.7之间。这个pH值的降低可以影响聚合反应的条件，该条件进而控制所述AR涂层溶液和随后固化的涂层中聚合物的粒子尺寸。在一个实施方案中，所述AR涂层溶液中聚合物的平均粒子尺寸可以小于10nm，更具体地，小于1nm。固化后的AR涂层的平均粒子尺寸可以在约15到约100nm之间，更具体地，在约25到约75nm之间，且所述聚合物可具有在约25000到约150000道尔顿之间的分子量。所述AR涂层还可以进一步被包括水，IPA，丙酮和/或PGMEA中的一种或多种的溶剂稀释。额外的酸可以在稀释的过程中被加入以维持所需的pH值。
所述AR涂层溶液可以通过各种通常已知的涂覆方法，包括旋转涂布，狭缝模头涂布，喷涂，浸渍涂布，辊涂和其他的涂布工艺，而分配到光学透明元件的表面上。取决于分配方法，在初始的反应中含有的或加入到所述AR涂层溶液中的溶剂的量可以变化，以此来使所述AR涂层溶液的固体浓度范围在约1到约25重量百分含量之间。在一些实施方案中，在STR中形成更浓缩的批次，然后通过稀释得到所需浓度，可能具有制造上的优势。在可替换的实施方案中，稀释可以在最初混合阶段之前或期间进行。对于浸渍涂布，固体浓度在约10到20重量百分含量之间是希望的。对于其他的涂布方法，如旋转涂布，狭缝模头涂布和喷涂，可能希望在约1到6重量百分含量之间的较低的固体浓度。本发明的实施方案可能更适用于喷涂施涂，原因是由前述的制造工艺可以得到相对较小的聚合物颗粒尺寸。所得到的涂层溶液的粘度可以在约0.75cP到约2.0cP之间变化。
不同于其他的形成AR涂层材料的方法，本发明的AR涂层溶液不需要从溶液中移除粒子就可使用。另外，由本发明的实施方案形成的AR涂层溶液可以在长时间内保持稳定。如这里所使用的，稳定性涉及涂层溶液的光学和/或机械性能特征，包括但不限于，光透射度，粘度，粘合性和/或pH值。在室温下，本发明的涂层溶液可以在至少24小时内保持稳定，更具体地，在约一周内，甚至更具体地，在约4周内保持稳定。另外，本发明的涂层溶液可在-20℃到-40℃的冷冻机中保存至少6个月，而不实质上影响玻璃涂层所需的光学或机械性能。特别地，如果所述涂层溶液需要运送到外地和/或在使用之前需要保存一段时间时，这种在长时间保存AR涂层的能力具有明显的制造上的好处。
在施涂后，所述AR涂层溶液在光学透明基板上被固化。当被施涂到玻璃基板上时，所述AR涂层溶液可以经过高温热回火步骤来固化涂层，根据玻璃的组成，温度范围在约600℃到约750℃之间，时间在约1分钟到约1小时之间。应该意识到，前述的各种烷氧基硅烷和/或金属醇盐残基可以在固化步骤中进一步改性。然而，这些附加的衍生残基仍构成烷氧基硅烷和/或金属醇盐残基以实现本发明的目的。
根据本发明实施方案的带有AR涂层的光学透明元件可具有提高的光学透射性能。例如，所述AR涂层可具有在约1.15到约1.3之间的折射率，在光谱的可见光波段(350到800nm)中获得最高4.26％的透射性能的提高和/或在光谱的红外波段(800到2500nm)中获得最高约3％的透射性能的提高。
如果光学透明基板的两面都被涂覆，光谱中可见光波段的透射性能可提高最高约8-9％，并且光谱中红外波段的透射性能可提高最高约5-7％。在以下的实施例部分将展示与这些性能相关的示例性数据。在一些实施方案中，只要所述AR膜的厚度适合于(turned to)入射光的波长(AR膜的厚度是入射光波长的约1/4)，透射性能的绝对提升不依赖于涂覆方法。
如实施例中进一步揭示的那样，相对于普通的溶胶-凝胶，本发明的AR涂层可具有提升的粘合性和/或硬度。另外，包含TIPO的AR涂层可具有自我净化特性，原因是在水和太阳紫外线存在下产生羟基基团。所述羟基基团可以氧化玻璃表面上水不溶性有机污物，形成高度水溶性的化合物，它们能够在下雨时被冲洗掉。这种自我净化特性可以根据TIPO的添加量而实现最优化。在一些实施方案中，TIPO的含量例如是在约0.0005摩尔到约0.003摩尔。
图2是根据本发明实施方案的一个将光转化为电能的光电模块(例如太阳能电池)的截面图。来自太阳等的进入或入射光，在到达模块的光电半导体(活性膜)4之前，首先照射在AR涂层1上并穿过，然后穿过玻璃基板2和前透明电极3。所述模块还可以含有，但不是必需的，反射增强氧化物和/或EVA膜5，和/或后金属接触器和/或反射器6，如图2所示。其他类型的光电装置当然也可以使用，且图2的模块只是为了举例和便于理解的目的提供的。还应该理解，模块可以含有遮盖多个串联的光电电池的单一AR涂覆的光学透明基板。
如上面解释的那样，AR涂层1降低了入射光的反射和允许更多的光到达光电模块的薄膜半导体膜4，以此使装置更有效地工作。虽然前面讨论的特定的AR涂层1被应用于光电装置/模块的描述中，但本发明并不局限于此。本发明的AR涂层可用于其他的应用中。而且，其他的层可以在玻璃基板上在AR涂层下被提供，因此AR涂层被认为是设置在玻璃基板上，即使在两者之间提供了其他层。
具体实施方式
实施例1-16
在实施例1-16中，122克异丙醇和62克丙酮被放入反应器中。在实施例1-10中，0.09摩尔四乙氧基硅烷(TEOS)和0.01摩尔甲基三乙氧基硅烷(MTEOS)被加入到反应器中同时用搅拌器搅拌。在实施例12-16中，TEOS和MTEOS之间的摩尔比例是变化的。所有单体的总摩尔量保持在0.1摩尔的恒定总量以简化动力学测量。下面的表1显示了每个实施例中使用的特定组分的含量。
氢氧化四丁基铵(TBAH)(40％水溶液中0.002摩尔)或氢氧化四甲基铵(TMAH)(25％水溶液中0.002摩尔)作为碱催化剂被加入且所述反应混合物随后被加热到35-70℃保持1-3.5小时。随后将反应混合物冷却，以半连续方式将硝酸加入到反应混合物中以调整所述反应混合物的pH值到0.5-1.7。然后将所述反应混合物冷却且用IPA，丙酮和/或PGMEA稀释。分子量通过凝胶渗透色谱法测量，且基于反应条件，它的范围在约25000-150000道尔顿。稀释和pH值控制之后，将所述聚合物制剂保存在-20℃到-40℃的冷冻机中。
在冷冻状态保存后，这些制剂随后被沉积在玻璃或透明基板上。浸渍涂布，狭缝，模头涂布，辊涂，和旋转涂布工艺被尝试。在几乎所有情况下，通过在空气或氮气下，在200-700℃、更有利地在600-750℃下固化3分钟到1小时，获得了125nm的所希望的涂层厚度。来自n&k Technology，Inc.的宽带光谱装置被用来测量涂层厚度。通过SEM分析，涂层中平均聚合物粒子尺寸在10到100nm之间。
透射数据通过可测量300-2500nm的紫外-可见光谱测量仪进行测量获得。来自n&k Technology，Inc.的宽带光谱装置被用来测量折射率。表1和2提供了实施例1-16的组成和性能数据。
铅笔硬度测试被用作抗擦性和/或硬度的指示，且通过尝试不同硬度的铅笔(例如，3B，4B等)在AR涂层上的擦拭来进行。胶带测试被用作涂层粘合性的指示，且通过在涂层中形成交叉排线(cross-hatchs)，按压背衬粘合剂的胶带材料到被涂覆的基板上，从涂层上拉开胶带，然后研究胶带在涂层中交叉排线部分上的影响来进行测量。接触角测试通过使用来自AST Products，Inc.的VCA2500仪器来确定AR涂覆基板的接触角。这些测试的结果在表2中展示。
表1
Figure BPA00001473360400101
表2
Figure BPA00001473360400111
可以看出TBAH的摩尔量在约0.0005到约0.003，或更具体地，约0.002摩尔，将导致优化的反应速率。较低量的TBAH降低反应速率，而较高量将增加反应速率到形成凝胶的水平。
可以确定，实施例1-16都具有接近1.23的折射率且透射率(相对于无涂覆的基板)提高了最高4％。铅笔硬度结果一般地揭示了可接受的抗擦性，而实施例16具有特别高的抗擦性。实施例3-5，7-9和16还展示了由胶带测试得出的可接受的到优异的涂层粘合性。
实施例11修改为在反应溶液中含有0.00015摩尔的二乙基磷酸乙基三乙氧基硅烷(而维持1摩尔的总单体量)。如此提高了硬度和粘合性，但是涂层膜的折射率由1.2提升到1.3。某些实施例在固化前还用乙醇与水的50-50混合物处理，以此去除TBAN(硝酸四丁基铵)，否则其将作为TBAH和硝酸反应的产物而留在膜上。已经发现，这步清洗步骤进一步提高了膜的硬度。在一些情况下，在固化步骤前这样处理后，硬度能够达到3H。
实施例16进一步进行一些如下面表3所述的耐久性测试以确定粘合性或透射性是否损失。
表3
Figure BPA00001473360400121
“通过”指小于0.02的透射率损失和粘合性无可检测的变化。如上面所示，实施例16通过所有的耐久性测试。
实施例16中的样品在室温下在大约10天后进一步进行测试以确认其稳定性。如下面的表4所示，涂层溶液样品被制成具有不同的聚合物材料摩尔浓度。
表4
Figure BPA00001473360400131
表4中展示的结果，表明了样品在存储后维持小于2.0cP的粘度和约3～4的pH值，确认了涂层溶液的稳定性。
实施列17-42
表5-6提供了实施例17-42的组成和性能数据，其中添加了不同类型和量的一种或多种粘合性提升材料。在实施例17-40中，将122克异丙醇和62克丙酮放入反应器中。在实施例41-42中，将366克异丙醇和250克丙酮放入反应器中。
在每个实施例中，四乙氧基硅烷(TEOS)和/或甲基三乙氧基硅烷(MTEOS)被加入到反应器中同时用搅拌器搅拌。VTEOS，DMDEOS，MDEOS和/或TIO中的至少一种也被加入。
在实施例17-40中，TBAH(40％水溶液中有0.002摩尔)被用做碱。在实施例41和42中，0.006摩尔的TBAH被加入作为碱催化剂，且额外的水也被加入。
所述反应混合物随后被加热至35-70℃保持3.5小时。所述反应混合物随后被冷却至45℃，且以半连续方式将硝酸加入到反应混合物中以调节所述反应混合物的pH值至0.5-1.7。随后，所述反应混合物被冷却，且用IPA，丙酮，PGMEA，和/或水稀释。在实施例41和42中，所述反应混合物用14重量百分比的PGMEA，46.472重量百分比的IPA，37.38重量百分比的丙酮和1.87重量百分比的水的混合物稀释。
在稀释和pH控制之后，所述聚合物制剂被存储在-20℃到-40℃的冷冻机内。分子量由GPC测量，且依据反应条件，其大约为25000-150000道尔顿。
这些制剂随后通过旋涂被沉积在玻璃基板上。在几乎所有情形下，在空气或氮气下，在200-700℃下、优选在600-750℃下固化3分钟到1小时，获得125nm的所希望的涂层厚度。
在实施例1-16中进行的测试同样在实施例17-40中进行，如下面的表6所示。实施例41和42包含些许不同的测试，包括350-1200nm下平均光透射率的提高和由扫描力显微镜测量的表面粗糙度(RMS)测试，如下面的表7所示。擦拭测试按照EN-1096-2测量。
表5
Figure BPA00001473360400141
Figure BPA00001473360400151
表6
Figure BPA00001473360400152
Figure BPA00001473360400161
表7
Figure BPA00001473360400162
实施例17-42表明VTEOS，DMDEOS，MDEOS和TIPO的加入提高了AR涂层的一些物理性能，包括抗擦性/硬度和/或粘合性。特别是VTEOS，能够提高膜的硬度和一致性。
可以确定的是，这里描述的反应可以没有困难地，或在不损失制成的膜的光学和机械性能的情况下，放大到100到1000升批量规模。
在不背离本发明的范围情况下，可以对讨论的示例性实施方案进行各种不同的修正和增加。例如，虽然上面讨论的实施方案涉及特定的特征，但是本发明的范围还包括具有不同特征组合的实施方案和不包含所有上述讨论的特征的实施方案。相应地，本发明的范围意图包含落入权利要求和其等同物的保护范围之内的所有的替代，修正，和变化。

Claims (15)

1.一种光学透明元件，其包括：
光学透明基板；和
在所述光学透明基板的至少一个表面上设置的抗反射涂层，所述抗反射涂层含有聚合物，所述聚合物包括：
至少一个四烷氧基硅烷残基；和
选自包含三烷氧基硅烷、二烷氧基硅烷、单烷氧基硅烷及其组合构成的组中的至少一个的第二种烷氧基硅烷残基，其中所述聚合物中相对于聚合物的总摩尔数含有至少50％摩尔百分含量的所述至少一个四烷氧基硅烷残基，且所述涂层中含有平均尺寸不大于100nm的聚合物粒子。
2.如权利要求1所述的光学透明元件，其中所述至少一个烷氧基硅烷残基是四乙氧基硅烷。
3.如权利要求1-2中任一项所述的光学透明元件，其中所述第二种烷氧基硅烷残基是选自由甲基三乙氧基硅烷和乙烯基三乙氧基硅烷构成的组。
4.如权利要求1-3中任一项所述的光学透明元件，其中所述至少一个四烷氧基硅烷残基是四乙氧基硅烷，且所述第二种烷氧基硅烷是甲基三乙氧基硅烷。
5.如权利要求4所述的光学透明元件，其进一步包含乙烯基三乙氧基硅烷残基。
6.如权利要求1-5中任一项所述的光学透明元件，其中所述聚合物进一步含有金属醇盐残基。
7.如权利要求1-6中任一项所述的光学透明元件，包含至少约20％摩尔百分含量的所述第二种烷氧基硅烷残基。
8.如权利要求1-7中任一项所述的光学透明元件，其进一步包含邻近所述光学透明元件设置的至少一个半导体层。
9.一种形成光学透明元件的方法，其包括：
分配涂层溶液至光学透明基板上，所述涂层溶液由以下步骤形成：
混合至少第一种四烷氧基硅烷材料、第二种烷氧基硅烷材料、碱催化剂和溶剂，其中所述第二种烷氧基硅烷材料选自由三烷氧基硅烷、二烷氧基硅烷、单烷氧基硅烷及其组合构成的组；
在足够的温度下维持涂层溶液的pH值一段充分的时间以形成具有约15nm到约100nm平均粒子尺寸的聚合物粒子，和
降低所述涂层溶液的pH值到低于约5.0；和
固化所述分配的涂层溶液以在所述光学透明基板上形成抗反射涂层。
10.如权利要求9所述的方法，其中所述碱催化剂包括至少一种季铵。
11.如权利要求9-10中任一项所述的方法，其中所述碱催化剂包括四丁基铵氢氧化物、四甲基铵氢氧化物或其组合。
12.如权利要求9-11中任一项所述的方法，其中所述涂层溶液在降低pH值之前被维持在约35℃到约70℃之间约1小时到约5小时。
13.如权利要求9-12中任一项所述的方法，，其中所述pH值被降至不大于2.0。
14.如权利要求9-13中任一项所述的方法，其在分配之前，进一步含有在液态或冻结状态下存储该涂层溶液至少约24小时的步骤。
15.如权利要求9-14中任一项所述的方法，其中所述涂层溶液通过喷雾分配。
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