CN103619965B - 用于光学元件的涂料组合物 - Google Patents

用于光学元件的涂料组合物 Download PDF

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CN103619965B
CN103619965B CN201280026804.8A CN201280026804A CN103619965B CN 103619965 B CN103619965 B CN 103619965B CN 201280026804 A CN201280026804 A CN 201280026804A CN 103619965 B CN103619965 B CN 103619965B
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D·瓦拉普拉萨
B·科罗列夫
S·穆克霍帕赫亚伊
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Abstract

记载了抗反射涂层和涂料组合物，光学元件和制备涂料组合物和光学元件的工艺。所述涂料组合物由至少一种烷氧基硅烷材料和至少一种高沸点溶剂形成。所述涂料组合物可以采用辊涂工艺来施涂。

Description

用于光学元件的涂料组合物
技术领域
本发明总体涉及用于光学元件的涂料组合物，更特别地涉及在光伏电池应用中使用的玻璃盖板(glass cover)用的抗反射涂层。
背景技术
抗反射(AR)涂层应用于许多工业，包括光伏(PV)模块的制造，以在光穿透光学透明元件如玻璃时减少入射光线的反射部分。玻璃基底的AR涂层的目标是实现尽量接近1.23的折射率，以使得在宽的光波长谱带上的光透射最大化。
一层或多层低折射率涂料可以在宽波长范围和宽入射角范围内获得改善的透光率。这种涂料可以经由溶胶-凝胶工艺沉积(在大气压或非真空下)，并且可以是高成本效率的。这些薄的抗反射涂层，可以由采用常规涂布技术施涂到玻璃上的二氧化硅前体形成，据报道将光谱可见光部分的太阳光透光率提高了约二到三个百分点。已采用多种机理来形成这种溶胶-凝胶材料，包括经由烷氧基硅烷的水解/缩合反应。参见，例如，G.Wu等的，“Anovel route to control refractive index of sol-gel derived nanoporous filmsused as broadband antireflective coatings”，材料科学与工程B78(2000)，135-139页。
溶胶-凝胶涂料可以采用各种方法施涂到光学透明元件上，包括旋涂，狭缝挤压式涂布，喷涂，浸涂，幕涂，辊涂以及其它涂布技术。取决于施涂方法，包含在涂料组合物当中的以氧化物表示的固体总量可以在大约1到大约25重量百分数范围内变化。在溶胶-凝胶工艺当中使用的常规溶剂体系通常具有低沸点和高挥发性，以使得它们在涂料施涂到基材上之后快速蒸发，从而尽量减少固化时间和温度条件。
对于某些湿涂料施涂方法，并且特别是某些连续涂布方法的一个挑战是难以在光学透明基材上获得均匀的涂层。包含常规低沸点溶剂体系的溶胶-凝胶涂料组合物的使用，趋向于表现出随着时间流逝增大的固体浓度和/或粘度，从而导致不均匀的涂层。这会导致质量保证受到挑战以及材料成本的增加。
发明内容
本文公开的实施方案涉及涂料组合物，采用该涂料组合物的光学元件如光学模块，以及制备溶胶-凝胶组合物和/或将溶胶-凝胶组合物施涂到光学元件上的改进工艺。
一个实施方案是涂料组合物，其包含至少一种烷氧基硅烷残体(residue)和至少大约50wt％的在大气压下具有至少约125℃的沸点的溶剂。
另一个实施方案是形成光学透明元件的方法，其中在该光学透明基材的一部分上通过辊涂或其它涂布方式施涂涂料组合物，然后加热以形成涂层如抗反射涂层。所述涂料组合物包含至少一种烷氧基硅烷残体和至少大约50wt％的至少一种在大气压下具有至少125℃的沸点的溶剂。
更进一步的实施方案是生产涂料组合物的方法，其中在合适的条件下将至少一种烷氧基硅烷与高沸点溶剂混合从而形成组合物。
附图说明
附图1是根据本发明的一个实施方案的示例性辊涂系统的示意图。
附图2提供了依照本发明一个实施方案的包含涂层的光伏电池的示意图。
具体实施方式
在一个实施方案当中，本发明提供了涂料组合物，其包含至少一种烷氧基硅烷残体，至少一种高沸点溶剂，任选的水和任选的催化量的酸或碱。根据某些实施方案，所述涂料组合物可以不含或基本上不含低沸点溶剂。
各种从商业渠道获取的烷氧基硅烷均可用于形成所述涂料组合物。合适的烷氧基硅烷可以具有下面的通式：
其中，至少2个R基团独立地是C1到C4烷氧基且剩余的R基团，如果有的话，独立地选自由氢、烷基、苯基、卤素、取代苯基组成的组。术语烷氧基包括可在接近室温的温度下通过水解容易地从硅上解离(cleave)的任何其它有机基团。合适的烷氧基硅烷包括四乙氧基硅烷(TEOS)和四甲氧基硅烷(TMOS)。其它的例子包括三烷氧基硅烷如甲基三乙氧基硅烷(MTEOS)，氨丙基三乙氧基硅烷(APTEOS)和APTEOS-三氟甲磺酸酯，乙烯基三乙氧基硅烷(VTEOS)，和二乙基磷酰乙基三乙氧基硅烷(diethylphosphatoethyltriethoxy silane)。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)。进一步的实例包括单烷氧基硅烷如三甲氧基硅烷，且特别是(3-缩水甘油醚氧丙基)-三甲氧基硅烷。也可使用烷氧基硅烷材料的组合。
在一个实施方案当中，使用至少两种烷氧基硅烷材料，且第一烷氧基硅烷是四烷氧基硅烷，如TEOS。第二烷氧基硅烷可以包括任何三烷氧基硅烷，二烷氧基硅烷或单烷氧基硅烷，包括上面所列出的那些。例如，MTEOS和/或VTEOS可特别适用于改善粘附和/或硬度。在一个实施方案当中，以烷氧基硅烷材料的总摩尔数计，第二烷氧基硅烷材料或材料组合可以从至多约50mol％到40mol％到35mol％到25mol％到15mol％的量与第一烷氧基硅烷材料混合。在另一实施方案中，以两种烷氧基硅烷材料的总摩尔数计，第二烷氧基硅烷材料可以至少约10mol％到至少约40mol％的量添加。第一烷氧基硅烷与第二烷氧基硅烷材料的摩尔比可为1：1到1000：1，更特别地为10：1到500：1，且甚至更特别地为25：1到100：1。
可使用前述材料的组合来达到所需的涂层性质。在一个实施方案中，涂料组合物包含TEOS和MTEOS。在另一实施方案当中，涂料组合物包含TEOS、MTEOS、VTEOS。在又一实施方案中，涂料组合物包含TEOS、MTEOS、VTEOS。烷氧基硅烷的其它组合以及由这些烷氧基硅烷形成AR涂层材料的方法已公开于美国申请12/796,199中，其全文以引用方式并入本文中。
根据一个实施方案，可向涂料组合物当中添加低于约25重量％的烷氧基硅烷材料，更特别地低于约15重量％的烷氧基硅烷材料，甚至更特别地低于约10重量％的烷氧基硅烷材料，甚至更特别地低于约5重量％的烷氧基硅烷材料以及甚至更特别地低于约3重量％的烷氧基硅烷。
合适的高沸点溶剂在大气压下可具有至少约125℃的沸点，更特别地至少约150℃，更特别地至少约170℃，且甚至更特别地至少约185℃的沸点。在一个实施方案中，所述高沸点溶剂可以包括可与水及烷氧基硅烷混溶的二醇和/或C1到C4烷基的醚。这类亚烷基二醇可以具有0.021mol/cm3或更低的羟基浓度以及约100或更高的重均分子量。合适的高沸点溶剂组合物组分的实例包括乙二醇、丙二醇、二乙二醇、三乙二醇、四乙二醇、五乙二醇、二丙二醇、六乙二醇以及任意前述物质的烷基醚。特别合适的实例是二丙二醇甲醚。高沸点溶剂的混合物也是适用的。
在一个实施方案当中，涂料组合物包含至少约50重量％的高沸点溶剂(或溶剂组合)，更特别地至少约60重量％的高沸点溶剂，甚至更特别地至少约70重量％的高沸点溶剂，甚至更特别地至少约80重量％的高沸点溶剂，且甚至更特别地至少约90重量％的高沸点溶剂。
在另一实施方案当中，添加很少或不添加低沸点溶剂到涂料组合物中，从而它基本上不含或完全不含低沸点溶剂。应该注意的是，涂料组合物内发生的水解反应可导致低沸点溶剂副产物，例如甲醇和乙醇。尽管如此，无论低沸点溶剂是外加的还是作为副产物形成，在一个实施方案当中涂料组合物可包含低于10重量％的在大气压下具有低于125℃沸点的溶剂，更特别地低于5.0重量％的具有低于125℃沸点的溶剂，甚至更特别地低于1.0重量％的具有低于125℃沸点的溶剂，且甚至更特别地低于0.5重量％的具有低于125℃沸点的溶剂。在其它实施方案中，本文所提供浓度范围内的低沸点溶剂在大气压下具有低于150℃、更特别地170℃且甚至更特别地低于185℃的沸点。在另一实施方案当中，涂料组合物不含或基本上不含外加的乙醇和/或丙酮。
涂料组合物还可以包含任选的催化剂。合适的酸催化剂包括硝酸、盐酸、硫酸、乙酸及其它类似的有机酸。合适的碱催化剂包括氢氧化铵，具有式R1R2R3R4N+OH-的季铵化合物，其中R1、R2、R3和R4各自独立地为苯基、氢或C1-16烷基。在一些实施方案当中，合适的碱催化剂包括季铵化氢氧化铵，如四丁基氢氧化铵和四甲基氢氧化铵。在一些实施方案当中，合适的碱催化剂包括这些组分的水溶液，并且除了碱催化剂水溶液中的以外，可以任选地包含额外的蒸馏水。
在更进一步的实施方案当中，涂料组合物中可以包含一种或多种多元醇，其可以增强涂料组合物的涂布特性和其它性质。例如，涂料组合物可以包含羟值为约14mg KOH/g至约590mg KOH/g的多元醇。具体的多元醇种类包括己内酯多元醇，聚乙二醇，聚丙二醇及聚碳酸酯二醇。
根据一实施方案，涂料组合物通过混合至少一种烷氧基硅烷、至少一种高沸点溶剂、任选的水、任选的催化量的酸或碱和任选的多元醇形成。
取决于所使用的所述一种或多种烷氧基硅烷材料和任选的催化剂，涂料组合物可在施涂于基材上之前经由水解和/或酯交换机理在使得烷氧基硅烷材料部分或完全聚合的条件下形成。例如，包括碱催化剂在内的涂料组合物组分可在，例如，夹套式搅拌釜反应器(STR)中经由间歇或半间歇模式在约35℃至70℃的适合温度下混合并反应约1小时至约6小时的适合的反应时间，更特别地1小时至3.5小时。
在前述条件下，可发生水解和缩合反应从而在溶液中形成聚合物。取决于反应条件，溶液中所含的聚合物可在直链或无规支化链，到多孔基质，到致密胶体粒子之间变化。在任何情形下，所得的聚合物将包含前述的烷氧基硅烷材料的残体。本文所用的术语“残体(residue)”旨在表示衍生自起始添加到涂料组合物当中的烷氧基硅烷的聚合物分子的一部分。举例来说，众所周知1摩尔四乙氧基硅烷在前述条件下反应形成1摩尔SiO2，其将构成四乙氧基硅烷残体的一个实例。
还可以理解可形成某些副产物并作为聚合物的一部分或单独组分包含于涂料组合物当中。例如，TEOS的水解可导致生成作为副产物的乙醇。
在一个实施方案当中，涂料组合物可以包含低于15重量％的SiO2，更特别地低于约10重量％的SiO2，甚至更特别地低于约5重量％的SiO2，且甚至更特别地低于约3重量％的SiO2。由于已知(或可测定)烷氧基硅烷：SiO2的摩尔比，因此SiO2的固体浓度可基于添加到混合物当中的烷氧基硅烷的量(以克表示)以及烷氧基硅烷和SiO2的分子量来计算。
涂料组合物中SiO2的固体浓度也可以通过重力分析来测定，例如，通过添加强碱到涂料组合物中并随后蒸发液体组分以形成纯SiO2。
在另一实施方案当中，聚合物包含至少一个TEOS残体，至少一个MTEOS残体或二者。在另一实施方案当中，聚合物另外包含至少一个VTEOS残体。
为进一步控制反应条件，在于碱性条件下经过合适的反应时间后，可使用酸，例如硝酸，调节涂料组合物的pH值到约0到约4.0之间，更特别地约0到约2.0且甚至更特别地约0.5到约1.7。pH值的降低可以影响聚合反应条件，继而控制涂料组合物和随后固化的涂层中所含的聚合物的粒度。在一个实施方案当中，涂料组合物当中聚合物的平均粒度可低于10nm，更特别地低于1nm。固化后涂层的平均粒度可介于约15nm与约100nm之间，更特别地介于约25nm与约75nm之间，且聚合物分子量可在约25000到约150000道尔顿的范围内。涂料还可以用包含水、IPA，丙酮和/或PGMEA中的一种或多种的低沸点溶剂进一步稀释。在稀释期间可添加额外的酸以维持期望的pH。
在一个替代实施方案当中，涂料组合物于一定条件下形成，该条件使得所述一种或多种烷氧基硅烷材料保持聚合物前体的形式直至涂料组合物施涂到基材上并热固化使其聚合为止。
本发明实施方案中的涂料组合物是随时可用的，无需从溶液当中移除粒子。此外，通过本发明实施方案形成的涂料组合物可在环境温度下长时间保持稳定。此外，本发明的涂料组合物可在-20℃到-40℃冷冻箱中储存以延长保存期限，而不会实质性地影响玻璃涂层所期望的光学或机械性质。长时间保存AR涂料的能力可以提供显著的制造优势，特别是将涂料组合物运输至现场以外的位置和/或使用前长时间储存时。
涂料组合物可以施涂到光学透明基材上，例如玻璃基材(如钠钙玻璃、浮法玻璃、硼硅酸盐和低铁钠钙玻璃)、塑料盖板、丙烯酸菲涅尔透镜(Fresnel lense)或其它光学透明基材。
涂料组合物可通过各种通常已知的涂布方法施涂到光学透明元件的表面上，包括旋涂、狭缝挤压式涂布，喷涂，浸涂，辊涂以及其它涂布技术。取决于涂布方法，涂料组合物可以变化以使得涂料组合物的固体浓度在约1重量％到约25重量％的范围内。在一些实施方案当中，形成较为浓缩的批料，随后在现场稀释至期望的浓度可具有制造优势。在替代的实施方案当中，稀释可在初始混合阶段以前或在此期间发生。在任一情形下，可使用高沸点溶剂以进一步稀释涂料组合物。
涂料组合物可在光学透明基材上形成为一个或多个层。在某些实施方案中，可采用包含不同材料或不同组分浓度的多层。在其它实施方案中，一个或多个层可由非烷氧基硅烷材料形成。这些层可在施涂涂料组合物之前施加到基材上和/或施加到涂料组合物形成的涂层之上。
根据某些实施方式，涂料组合物可采用辊涂技术施涂。如图1当中示意性显示地，常规辊涂系统10通常包括输送带12；施涂辊14，其可以沿与输送带12相同的方向(正向辊)或相反的方向(反向辊)旋转；计量辊16，其用于控制涂料组合物的施涂；支撑或压力辊18；均衡辊19；至少一个稳定辊20和涂料容器22。当玻璃基材24沿输送带12移动时，从涂料容器22转移到施涂辊14的涂料组合物以大致均一的厚度施涂到基材24。本发明的一个显著的优点在于，涂料组合物由于使用了大浓度的高沸点溶剂从而具有低挥发性。因此，留存在容器22当中的涂料组合物的溶剂的蒸发速率显著降低，使得随时间流逝在连续辊系统10中更均匀地施涂涂料组合物。特别地，高沸点溶剂防止因容器22中溶剂的蒸发而造成固体浓度随时间显著增加。
施涂后，涂料组合物固化到光学透明基材上。当施涂到玻璃基材时，涂料组合物可经受高温热回火步骤，取决于玻璃的组成在约400℃至约750℃范围内持续约1分钟到1小时以固化涂层。在高温加热步骤之前，可先使涂覆基材经受约200℃到约300℃的低温加热步骤。可以理解前述各种烷氧基硅烷前体或聚合物在该加热过程期间可发生进一步改性。
经本发明实施方案的组合物涂覆的光学元件可具有改善的光透射特性。例如，涂层可具有介于约100到150nm的厚度，在约1.15到约1.3范围的折射率，在350nm到1100nm波长范围内高达约3.5％的透射增益。如果光学透明基材的两侧均经过涂覆，则可达到额外的透射增益。关于这些性质的例证数据在下面的实施例部分中阐述。
图2是根据本发明的实施方案用于将光转换成电的光伏模块(如太阳能电池)的截面图。来自太阳等的输入光或入射光首先入射到AR涂层1上，穿过它并然后穿过玻璃基材2和正面透明电极3，之后到达模块的光伏半导体(活性膜)4。如图2所示，该模块还可包括，但并非必需，反射增强氧化物和/或EVA膜5，和/或背面金属触点和/或反射镜6。当然，可使用其它类型的光伏器件，且提供图2的模块仅仅是出于示例和理解的目的。还应理解，模块可包括单个AR涂覆的光学透明基材，该基材覆盖多个串联连接的光伏电池。
如上所述，涂层1降低入射光的反射并允许更多的光到达光伏模块的薄膜光伏半导体膜4，由此使得该装置更有效地起作用。尽管上文论述的某些涂层1用于光伏装置/模块的情形，但本发明并不限于此。根据本发明的AR涂料可用于其它的应用中。而且，在玻璃基材上在该涂层之下可提供其它的一层或多层，使得即使有其它层提供在其间该涂层也视为布置在玻璃基材上。
实施例1
将二丙二醇甲醚(“DMP”)((640.90g)沸点190℃，蒸气压0.37毫巴)，80.62g(0.387mol)四乙氧基硅烷及38.89g(0.218mol)甲基三乙氧基硅烷添加到具有机械搅拌器的2L圆底烧瓶中。当用搅拌器剧烈混合各组分时，将存于6.242g甲醇中的1.0M四丁基氢氧化铵(“TBAH”)(7.52mmol)与200.243g(11.11mol)去离子水(DI water)的混合物逐步添加(经约30秒)至反应混合物中。于室温下搅拌反应混合物24小时后，添加3.12g35％HNO3，并将所得的混合物再搅拌15分钟。
将5g混合物的样品(“混合物A”)用5g二丙二醇甲醚稀释以形成涂料组合物(“组合物A”)。将组合物A的第一样品旋涂于4”的Si晶片的表面上(使用实验室规模的旋涂机在1300rpm下15秒)。将经涂覆的晶片在100℃下加热2分钟，且随后于625℃下加热4分钟。所得膜具有128nm的厚度和1.28的折射率(550nm)。两者的测量均使用购自n&k技术公司(SanJose，CA)的n&k Analyzer1200。
将组合物A的第二样品旋涂于4”的正方形低铁太阳能浮法玻璃片上(使用实验室规模旋涂机在1300rpm下15秒)。将经涂覆的晶片在100℃下加热3分钟，且随后于625℃下加热4分钟。使用Hitachi牌分光光度计进行经涂覆玻璃的透射扫描，显示350nm至850nm范围内的透射比未涂覆的参照玻璃提高约2.8％。
实施例2
如实施例1所述形成一定体积的组合物A并添加到图1中示意性显示的连续反向辊涂布工艺所用的容器中。橡胶施涂辊设定为以与布置于输送带上的玻璃基材相反的方向转动。辊涂布控制器设定为沉积约6ml组合物/平方米玻璃，以得到厚度约6微米的湿膜。然后将经涂覆的玻璃基材在以约12英尺/分钟移动的输送带式烘箱中在200℃到250℃加热，且随后在箱式炉中于约650℃下加热约7分钟。使用Hitachi牌分光光度计进行经涂覆玻璃的透射扫描，显示350nm至850nm范围内的透射比未涂覆的参照玻璃提高约2.5％。
实施例3
将一定体积的组合物A用二丙二醇甲醚稀释以得到固体浓度为1.5重量％的涂料组合物。将所得到的涂料组合物应用于如实施例2所述的反向辊涂布工艺，以及其中施涂辊以与传送带上的玻璃相同的方向转动的正向辊涂布工艺。对于反向辊涂布工艺，施涂辊设定为沉积约8ml涂料组合物/平方米玻璃，以得到厚度约8微米的湿膜。对于正向辊涂布工艺，施涂辊设定为沉积厚度约6微米的湿涂料。然后将经涂覆的玻璃基材在以约12英尺/分钟移动的输送带式烘箱中在200℃到250℃加热，且随后在箱式炉中于约650℃下加热约7分钟。使用Hitachi牌分光光度计进行经涂覆玻璃的透射扫描，显示对于反向工艺而言，在350nm至850nm范围内的透射比未涂覆的参照玻璃提高约2％，且对于正向工艺而言提高约3％。
实施例4
将2g实施例1中形成的混合物A的样品用3g二丙二醇甲醚稀释(组合物B)且分为5份样品。向四份样品中分别添加0.0100g、0.0175g、0.0250g、和0.0375g存于乙醇中的10％的BYK-307组合物。BYK-307是购自于BYK USA公司的聚醚改性的聚二甲基硅氧烷。所得的样品包含0.0重量％、0.02重量％、0.035重量％、0.50重量及0.075重量％的BYK-307。将样品旋涂于4”的正方形太阳能浮法玻璃片上(在650rpm下15秒)，在250℃下加热5分钟，且随后于650℃下加热5分钟。与不包含BYK-307的样品相比，包含BYK-307的样品具有改善的润湿性。
实施例5
将4.05g实施例1中形成的混合物A的样品用5.95g二丙二醇甲醚稀释(“组合物C”)。另一4.05g混合物A的样品用3.00g CAPA-2043(聚己内酯多元醇)和2.95g二丙二醇甲醚稀释，使得所得到的组合物(“组合物D”)包含30重量％的CAPA-2043。混合物A的第三样品用3.00g CAPA-3022(具有二乙二醇和甘油的己内酯聚合物)和2.95g二丙二醇甲醚稀释，使得所得的组合物(“组合物E”)包含30重量％的CAPA-3022。
将组合物C、D和E各自旋涂于4”的Si晶片上(于800rpm下15秒)，在250℃下加热5分钟且于650℃下加热5分钟。在n&k Analyzer1200上测量每一个经涂覆晶片的膜性质。由组合物C形成的涂层具有144nm的厚度和1.30的折射率。由组合物D形成的涂层具有260nm的厚度和1.16的折射率。由组合物E形成的涂层具有250nm的厚度和1.17的折射率。
组合物C、D和E也各自旋涂于4”的正方形太阳能浮法玻璃片上(在650rpm下15秒)，在250℃下加热5分钟，且随后于650℃下加热5分钟。由AR溶液D形成的涂层具有这三种涂层中最佳的润湿特性。
实施例6
表1当中列出的涂料组合物是通过将实施例1的混合物A与溶剂以及任意所列的添加剂混合制备的。
表1
涂料组合物 混合物A DPM CAPA-2043 CAPA-3022
F 4.05g 5.95g
G 4.05g 4.95g 1.00g
H 4.05g 4.95g 1.00g
I 4.05g 5.45g 0.50g
J 4.05g 5.45g 0.50g
将每一涂料组合物旋涂于4”的Si晶片(在650rpm下15秒)，在250℃下加热5分钟，并于650℃下加热5分钟。使用n&k1200Analyzer测量每一个涂覆晶片的膜性质。结果在下表2中列出。
表2
AR涂料组合物 厚度 折射率
F 142 1.30
G 332 1.15
H 352 1.14
I 318 1.14
J 316 1.13
还将每一AR涂料组合物旋涂在4”的正方形太阳能浮法玻璃片上(于650rpm下15秒)，在250℃下加热5分钟且随后于650℃下加热5分钟。每一样品的润湿性质类似。
实施例7
将三乙二醇二甲醚((13.80g)沸点216℃)、1.736g(8.33mmol)四乙氧基硅烷及0.837g(4.70mmol)甲基三乙氧基硅烷在具有磁力搅拌子的60mL玻璃瓶中混合。将0.134g存于甲醇中的1.0M四丁基氢氧化铵(0.16mmol)与2.875g(160mmol)去离子水的混合物逐步(经约30秒)添加到剧烈搅拌的反应混合物中。在室温下搅拌19小时后，反应混合物用64.0μL35％HNO3酸化，并搅拌15分钟。
将5g量的混合物用5g二丙二醇甲醚稀释。将组合物旋涂于4”的Si晶片上(在1100rpm下15秒)，在100℃下加热2分钟且随后于625℃下加热4分钟。涂层厚度(68nm)和折射率(在550nm处1.32)是使用n&k1200Analyzer测量的。
实施例8
将二丙二醇甲醚((23.24g)沸点190℃，蒸气压0.37毫巴)、2.923g(14.0mmol)四乙氧基硅烷、1.411g(7.90mmol)甲基三乙氧基硅烷、0.513g(28.5mol)去离子水，和0.226g1.0M四丁基氢氧化铵(0.27mmol)在具有磁力搅拌子的60mL玻璃瓶中混合。在室温下搅拌2小时后，添加106.0μL35％HNO3并将涂料组合物再搅拌15分钟。
将1g混合物样品旋涂于4”的Si晶片上(在1300rpm下15秒)，在100℃下加热2分钟且随后于625℃下加热4分钟。使用n&k测量工具测量涂层厚度(198nm)及折射率(在550nm处1.33)。
实施例9
将二丙二醇甲醚((123.25g)沸点190℃，蒸气压0.37毫巴)、15.5g(7.44mmol)四乙氧基硅烷、7.48g(4.2mmol)甲基三乙氧基硅烷、38.51g(2.14mol)去离子水和0.26g35％HNO3(1.45mmol)混合，并在充分混合后将混合物分成3等份。对于这三部分分别在室温和酸性条件下实施溶胶-凝胶工艺达22分钟、37分钟和54分钟后，添加0.80g1.0M四丁基氢氧化铵溶液(0.97mmol)，以增加每一反应混合物的pH并在碱性条件下实施溶胶-凝胶工艺。在室温下搅拌1.5小时后，向每一部分中添加35％HNO3以降低pH再次至酸性条件，并搅拌15分钟。
将1g每部分样品旋涂于4”的Si-晶片上(在2000rpm下15秒)，在100℃下加热2分钟且于625℃下加热4分钟。使用n&k1200Analyzer测量涂层厚度(150-220nm)及折射率(在550nm处1.33到1.36)。
实施例10
向配备有冷凝器、热电偶、取样口(sample port)和搅拌棒的1L反应器中在搅拌下装入616gm二丙二醇甲醚、丙二醇、乙二醇或前述任一者的混合物且随后添加77.49g TEOS和37.38g MTEOS到反应器中。在搅拌下向反应混合物中添加6g存于甲醇中的26％TBAH与64.155g去离子水的混合物。然后将混合物加热到55℃，并在55℃下保持2-3小时。反应完成后，在55℃下直接向混合物中添加3.6g35％HNO3的水溶液以淬灭反应。然后将反应混合物冷却至室温并用溶剂如DPM、丙二醇和共溶剂或添加剂稀释至特定浓度。然后将经过稀释的组合物在1500rpm下旋涂于硅和玻璃上持续35秒以制作膜。然后将湿膜在675℃下加热5分钟，并且测量厚度(100-150nm)、折射率(1.21-1.23)及透射率(在350-850nm内3％增益)。
可在不偏离本发明范围的前提下对所论述的示例性实施方案作出各种修改及添加。例如，尽管以上所记载的实施方案涉及具体特征，但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括所有所述特征的实施方案。因此，本发明的范围旨在涵盖所有落入权利要求范围内的所有这类替代方案，变型和变体，以及它们的所有等同方案。

Claims (18)

1.涂料组合物，其包含：
至少一种烷氧基硅烷残体；和
至少80 wt％的至少一种在大气压下具有至少185℃的沸点的溶剂，
其中所述涂料组合物的pH值为0到4.0。
2.权利要求1的涂料组合物，其中所述涂料组合物包含低于5 wt％的至少一种在大气压下具有低于125℃的沸点的溶剂。
3.权利要求1的涂料组合物，包含低于10 wt％的二氧化硅固体浓度。
4.权利要求1的涂料组合物，进一步包含至少一种多元醇。
5.权利要求1的涂料组合物，其包含至少90 wt％的所述至少一种溶剂。
6.权利要求1的涂料组合物，其中所述涂料组合物的pH值为0.5到1.7。
7.形成光学元件的方法，包括：
在光学透明基材的至少一部分上施涂至少一层涂料组合物，其中该涂料组合物包含至少一种烷氧基硅烷残体和至少80 wt％的至少一种在大气压下具有至少185℃的沸点的溶剂，以及
加热所述涂料组合物以在所述光学透明基材上形成反射涂层，其中所述涂料组合物的pH值为0到4.0。
8.权利要求7的方法，其中所述施涂步骤包括将所述涂料组合物辊涂到光学透明基材的至少一部分上。
9.权利要求7的方法，其中所述涂料组合物基本上不含在大气压下沸点低于125℃的溶剂。
10.权利要求7的方法，其中所述加热步骤包括起始在200℃到400℃下加热所述涂料组合物，然后在400℃到750℃下加热所述涂料组合物。
11.权利要求7的方法，其中所述涂料组合物包含至少90 wt％的所述至少一种溶剂。
12.权利要求7的方法，其中所述基材为玻璃基材，且所述加热步骤进一步包括将所述涂料组合物加热至400℃到750℃的温度。
13.权利要求7的方法，其中所述施涂步骤进一步包括将所述至少一层涂料组合物通过辊涂施涂到光学透明基材的至少一部分上。
14.权利要求7的方法，其中所述涂料组合物的pH值为0.5到1.7。
15.制备涂料组合物的方法，包括：
混合至少一种烷氧基硅烷、至少一种催化剂和至少一种在大气压下具有至少185℃的沸点的溶剂以形成涂料组合物，其中所述涂料组合物包含至少80 wt％的所述至少一种溶剂，其中调节所述涂料组合物的pH值到0至4.0。
16.权利要求15的方法，其中所述涂料组合物基本上不含在大气压下沸点低于125℃的低沸点溶剂。
17.权利要求15的方法，其中所述涂料组合物包含至少90 wt％的所述至少一种溶剂。
18.权利要求15的方法，其中调节所述涂料组合物的pH值到0.5至1.7。
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