CN108424007A - 一种光伏玻璃减反膜 - Google Patents

一种光伏玻璃减反膜 Download PDF

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CN108424007A
CN108424007A CN201810605255.9A CN201810605255A CN108424007A CN 108424007 A CN108424007 A CN 108424007A CN 201810605255 A CN201810605255 A CN 201810605255A CN 108424007 A CN108424007 A CN 108424007A
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Abstract

本发明公开了一种光伏玻璃减反膜，包括玻璃基底和复合在玻璃基底表面的减反膜，玻璃基底为压花玻璃或超白低铁玻璃，减反膜为由物理气相沉积所制得的多层膜，多层膜自内而外依次层叠在玻璃基底的表面，其中，第一层为Al2O3镀层，第二层为SiO2镀层，第三层为Al2O3镀层，第四层为TiO2镀层，第五层为SiO2镀层，第六层为TiO2镀层，第七层为SiO2镀层；该光伏玻璃减反膜不显著增加物理气相沉积镀膜产线长度及物料和生产成本，其在300～1200纳米波长范围内具有增透效果，单面镀膜条件下，360～1200纳米波长范围的平均透过率高于94 %；垂直入射条件下观测色中性良好，相对于化学镀膜减反膜更接近于超白玻璃原色，与后续玻璃钢化工艺的兼容性好。

Description

一种光伏玻璃减反膜
技术领域
本发明属于减反膜及其制备技术领域，具体涉及一种光伏玻璃减反膜。
背景技术
光伏玻璃减反膜不仅需要具备较高的光学透过率，还需要具有优异的机械力学特性与耐候性。目前普遍采用溶胶-凝胶法，通过辊涂、提拉、旋涂或喷涂等方式制备具有一定孔隙率的SiO2减反膜。通常，此类利用化学湿法制备的减反膜的折射率在可见光和近红外波段(约300～1200纳米波长范围)与单层减反膜的理想折射率1.23较为接近，因而在此波段可获得较高的太阳光谱加权平均透过率。尽管，各类SiO2纳米颗粒(实心、介孔、核壳)可与粘结剂形成具有一定强度的膜层，但出于光伏组件较为严苛的实际户外工作环境考虑，对具有更高硬度、更好膜基结合力和更强耐候性的光伏减反膜仍有着十分迫切的需求。
利用化学湿法制备减反膜具有成本低、面积大、减反性能好的特点，但膜层的机械力学特性和耐候性仍有进一步提升的空间，此外由于通常采用单层减反结构，其色中性相对较差，膜面多呈现浅蓝色。物理气相沉积，如：溅射、真空蒸镀和离子镀等，适于各类复杂多层膜系的精确制备，所制膜层的大面积均匀性、平整度更为优异，在相机、显微镜、望远镜、显示屏、建筑玻璃等众多产品中已实现了广泛的应用。但物理气相沉积目前普遍被用来制备针对可见光波段(约400～700纳米波长范围)的减反膜，无法用于制备光伏玻璃减反膜，其减反效应未能在小于400纳米和大于700纳米波长处有明显体现。
专利CN104309196A公开了一种可见光和近红外光双波段减反射膜玻璃，通过在玻璃基片交替沉积3对Al2O3和ZrO2薄膜，最外层沉积MgF2，组成7个膜层的复合膜系，可在430～900纳米与1540纳米两个波段实现高增透。由此可见该发明并未涉及900～1540纳米处的光学特性，因而无法应用于光伏玻璃减反。专利CN104046950A公开了一种由Nb2O5(或TiO2)、SiO2、Al2O3(或SiNx)和CNx四类材料所组成的6层膜系，单面镀膜条件下可在380～780纳米波段将反射率降低至5％以下，双面镀膜条件下降至1.5％以下。尽管其在可见光波段具有优异的减反特性，但仍无法达到光伏玻璃所要求的在300～1200纳米波长范围的增透要求。此外，专利CN105585253A公开了一种由高低折射率介质交替沉积组成的4层膜系，单面镀膜条件下可见光反射率低于5％。同样，该专利并未提供300～1200纳米波长的增透方法。类似地，专利CN104553126A公布的也是一种可见光波段的增透方法。专利203818661U公开了一种适用于显示和光伏玻璃的减反镀膜技术，该4层膜系在400～800纳米平均透过率可达到94.39％，380～1100纳米峰值透过率可达到96～97％，380～80纳米积分透过率可达到96～97％。可见，其主要面对的是显示行业及光伏响应曲线在400～800纳米波长范围的光伏组件，而对标目前化学镀膜光伏玻璃360～1200纳米的减反标准仍有距离。相对于目前业界采用的光伏玻璃化学镀膜技术，物理气相沉积技术的采用无疑将进一步提升光伏减反膜的强度和可靠性，获得更好的色中性，但针对目前物理气相沉积的减反膜光谱较窄的问题，迫切需要发明一种在300～1200纳米具有良好色中性和宽带减反特性的多层膜结构，同时确保物理气相沉积镀膜产线长度不显著增加以及确保镀膜材料与钢化工艺的兼容和匹配。
发明内容
本发明所要解决的技术问题是，针对现有技术的不足，提供一种低成本的光伏玻璃减反膜，该光伏玻璃减反膜在300～1200纳米波长范围内具有增透效果，垂直入射条件下观测色中性良好，相对于化学镀膜减反膜更接近于超白玻璃原色，与后续玻璃钢化工艺的兼容性好。
本发明解决上述技术问题所采用的技术方案为：一种光伏玻璃减反膜，包括玻璃基底和复合在玻璃基底表面的减反膜，所述的玻璃基底为压花玻璃或超白低铁玻璃，所述的减反膜为由物理气相沉积所制得的多层膜，所述的多层膜自内而外依次层叠在所述的玻璃基底的表面，其中，第一层为Al2O3镀层，第二层为SiO2镀层，第三层为Al2O3镀层，第四层为TiO2镀层，第五层为SiO2镀层，第六层为TiO2镀层，第七层为SiO2镀层。
作为优选，所述的第一层的Al2O3镀层的厚度为5～55nm，所述的第二层的SiO2镀层的厚度为15～65nm，所述的第三层的Al2O3镀层的厚度为45～115nm，所述的第四层的TiO2镀层的厚度为85～135nm，所述的第五层的SiO2镀层的厚度为5～55nm，所述的第六层的TiO2镀层的厚度为5～55nm，所述的第七层的SiO2镀层的厚度为75～125nm。
作为优选，所述的减反膜的表面设置有功能层，所述的功能层包括低折射率镀层、亲水层或疏水层。功能层可进一步降低反射率或实现自清洁特性，以增强光伏玻璃减反膜的户外应用特性。
进一步地，所述的亲水层的水接触角为0～20°，所述的疏水层的水接触角为95～180°。
进一步地，所述的低折射率镀层的折射率低于所述的多层膜中的SiO2镀层的折射率。
进一步地，所述的低折射率镀层为MgF2薄膜、掠射角沉积的多孔SiO2薄膜、MgF2-SiO2共溅射薄膜和Ag-Cu-SiO2多层薄膜中的任一种。除了MgF2薄膜、掠射角沉积的多孔SiO2薄膜、MgF2-SiO2共溅射薄膜和Ag-Cu-SiO2多层薄膜外，也可以选用现有技术中已知的其他折射率低于SiO2镀层的镀层。
作为优选，所述的多层膜中的各膜层在510纳米波长处的折射率分别为：SiO2镀层1.3～1.5，Al2O3镀层1.5～2.0，TiO2镀层2.0～2.5。
作为优选，所述的多层膜中的Al2O3镀层由Si3N4镀层或ZnO镀层替代。Si3N4镀层或ZnO镀层与SiO2镀层的折射率相近，可替代SiO2镀层。
作为优选，所述的多层膜中的TiO2镀层由ZrO2镀层或Nb2O5镀层替代。ZrO2镀层或Nb2O5镀层与TiO2镀层的折射率相近，可替代TiO2镀层。
作为优选，所述的物理气相沉积包括磁控溅射、电子束蒸发、热蒸发和真空离子镀中的任一种。磁控溅射是产业界大面积制备薄膜最常用的技术手段，除磁控溅射外，也可以选用电子束蒸发、热蒸发和真空离子镀等方法。
与现有技术相比，本发明具有如下优点：
(1)、本发明光伏玻璃减反膜引入Al2O3镀层，Al2O3的折射率介于SiO2和TiO2之间，Al2O3镀层作为缓冲层，起到平滑透射光谱的作用，使光伏玻璃减反膜获得良好的色中性。
(2)、本发明光伏玻璃减反膜中的多层膜由物理气相沉积制得，其膜系层数为7层，不显著增加物理气相沉积镀膜产线长度及物料和生产成本。
(3)、本发明光伏玻璃减反膜在300～1200纳米波长范围内具有增透效果，单面镀膜条件下，360～1200纳米波长范围的平均透过率高于94％；垂直入射条件下观测色中性良好，相对于化学镀膜减反膜更接近于超白玻璃原色。
(4)、本发明光伏玻璃减反膜采用高温稳定的膜系材料，可耐受500～700℃热处理温度，与后续玻璃钢化工艺的兼容性好。
附图说明
图1为实施例1的光伏玻璃减反膜的结构示意图；
图2为实施例1的光伏玻璃减反膜的透过率谱图；
图3为实施例1的光伏玻璃减反膜的静态水接触角测试图；
图4为实施例2的光伏玻璃减反膜的透过率谱图；
图5为实施例2的光伏玻璃减反膜的静态水接触角测试图。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。
实施例1的光伏玻璃减反膜，如图1所示，包括玻璃基底10和复合在玻璃基底10表面的减反膜，玻璃基底10为超白低铁玻璃，减反膜为由反应直流磁控溅射沉积所制得的多层膜，多层膜自内而外依次层叠在玻璃基底10的表面，其中，第一层21为Al2O3镀层，第二层22为SiO2镀层，第三层23为Al2O3镀层，第四层24为TiO2镀层，第五层25为SiO2镀层，第六层26为TiO2镀层，第七层27为SiO2镀层。
实施例1中，第一层21的Al2O3镀层的厚度为15nm，第二层22的SiO2镀层的厚度为25nm，第三层23的Al2O3镀层的厚度为90nm，第四层24的TiO2镀层的厚度为120nm，第五层25的SiO2镀层的厚度为20nm，第六层26的TiO2镀层的厚度为30nm，第七层27的SiO2镀层的厚度为110nm。
实施例1中，多层膜中的各膜层在510纳米波长处的折射率分别为：SiO2镀层1.45，Al2O3镀层1.62，TiO2镀层2.35。
实施例1中，在减反膜表面利用十三氟辛基三甲氧基硅烷气相沉积制得单分子疏水功能层30。
实施例1的光伏玻璃减反膜的具体制备过程为：采用厚度1mm的超白低铁玻璃作为基底，用丙酮、乙醇、去离子水对玻璃进行超声清洗，并用干燥N2吹干，然后放入多靶磁控溅射腔体内，开始抽真空。待磁控溅射腔体真空度抽至5×10-4Pa以下，通入高纯氩气和氧气混合气体作为反应溅射气体，氩氧流量分别为25sccm和15sccm。其中，Al2O3、SiO2、TiO2镀层分别采用直流磁控溅射Al、SiAl、Ti靶材获得，直流功率均为200W，通过控制溅射时间获得上述各膜层厚度，各镀层的沉积速率和折射率均通过椭偏仪测量确定。制备过程中基底温度为室温，保持基片旋转以保证薄膜均匀性。减反膜制备完成后，将其置于装有1mL十三氟辛基三甲氧基硅烷的容器中，放入真空干燥箱内，抽真空至0.1MPa，加热至150℃，保温1小时后取出样品，乙醇冲洗除去表面未充分反应的残余物后，在80℃干燥后进行紫外-可见-近红外分光光度计测试，透过率谱图如图2所示。从图2可见，该光伏玻璃减反膜的宽带减反特征明显，透过率谱较为平滑。样品在4μL水滴条件下稳态接触角为136°，属于疏水表面，如图3所示。
实施例2的光伏玻璃减反膜，与实施例1的区别在于，实施例2中，玻璃基底10为压花玻璃，采用射频磁控溅射在压花玻璃10上制备减反膜，并以ZnO镀层替代Al2O3镀层，以Nb2O5镀层替代TiO2镀层。
实施例2中，在减反膜表面利用六甲基二硅胺烷气相沉积制得单分子疏水功能层30。
实施例2中，第一层21的ZnO镀层的厚度为10nm，第二层22的SiO2镀层的厚度为25nm，第三层23的ZnO镀层的厚度为70nm，第四层24的Nb2O5镀层的厚度为110nm，第五层25的SiO2镀层的厚度为30nm，第六层26的Nb2O5镀层的厚度为20nm，第七层27的SiO2镀层的厚度为90nm。
实施例2中，多层膜中的各膜层在510纳米波长处的折射率分别为：SiO2镀层1.45，ZnO镀层2.00，Nb2O5镀层2.34。
实施例2的光伏玻璃减反膜的具体制备过程为：采用厚度1mm的压花玻璃作为基底，用丙酮、乙醇、去离子水对玻璃进行超声清洗，并用干燥N2吹干，然后放入多靶磁控溅射腔体内，开始抽真空。待磁控溅射腔体真空度抽至5×10-4Pa以下，通入40sccm的高纯氩气作为沉淀气体。其中，ZnO、SiO2、Nb2O5镀层分别采用射频溅射ZnO、SiO2和Nb2O5靶材获得，直流功率均为200W，通过控制溅射时间获得上述各膜层厚度，各镀层的沉积速率和折射率均通过椭偏仪测量确定。制备过程中基底温度为室温，保持基片旋转以保证薄膜均匀性。减反膜制备完成后，将其置于装有5mL六甲基二硅胺烷的容器中，放入60℃水浴中保温1小时后取出样品，乙醇冲洗除去表面未充分反应的残余物后，在80℃干燥后进行紫外-可见-近红外分光光度计测试，透过率谱图如图4所示。从图4可见，该光伏玻璃减反膜具有宽带减反特性，透过率谱较为平滑，与图2相比，具有更高的平均透过率。由此可见，通过合适的膜层替换和厚度优化可以进一步提升其增透效果。样品在2μL水滴条件下稳态接触角为130°，属于疏水表面，如图5所示。

Claims (10)

1.一种光伏玻璃减反膜，包括玻璃基底和复合在玻璃基底表面的减反膜，其特征在于，所述的玻璃基底为压花玻璃或超白低铁玻璃，所述的减反膜为由物理气相沉积所制得的多层膜，所述的多层膜自内而外依次层叠在所述的玻璃基底的表面，其中，第一层为Al2O3镀层，第二层为SiO2镀层，第三层为Al2O3镀层，第四层为TiO2镀层，第五层为SiO2镀层，第六层为TiO2镀层，第七层为SiO2镀层。
2.根据权利要求1所述的一种光伏玻璃减反膜，其特征在于，所述的第一层的Al2O3镀层的厚度为5～55 nm，所述的第二层的SiO2镀层的厚度为15～65 nm，所述的第三层的Al2O3镀层的厚度为45～115 nm，所述的第四层的TiO2镀层的厚度为85～135 nm，所述的第五层的SiO2镀层的厚度为5～55 nm，所述的第六层的TiO2镀层的厚度为5～55 nm，所述的第七层的SiO2镀层的厚度为75～125 nm。
3.根据权利要求1所述的一种光伏玻璃减反膜，其特征在于，所述的减反膜的表面设置有功能层，所述的功能层包括低折射率镀层、亲水层或疏水层。
4.根据权利要求3所述的一种光伏玻璃减反膜，其特征在于，所述的亲水层的水接触角为0～20°，所述的疏水层的水接触角为95～180°。
5.根据权利要求3所述的一种光伏玻璃减反膜，其特征在于，所述的低折射率镀层的折射率低于所述的多层膜中的SiO2镀层的折射率。
6.根据权利要求5所述的一种光伏玻璃减反膜，其特征在于，所述的低折射率镀层为MgF2薄膜、掠射角沉积的多孔SiO2薄膜、MgF2-SiO2共溅射薄膜和Ag-Cu-SiO2多层薄膜中的任一种。
7.根据权利要求1所述的一种光伏玻璃减反膜，其特征在于，所述的多层膜中的各膜层在510纳米波长处的折射率分别为：SiO2镀层1.3～1.5，Al2O3镀层1.5～2.0，TiO2镀层2.0～2.5。
8.根据权利要求1所述的一种光伏玻璃减反膜，其特征在于，所述的多层膜中的Al2O3镀层由Si3N4镀层或ZnO镀层替代。
9.根据权利要求1所述的一种光伏玻璃减反膜，其特征在于，所述的多层膜中的TiO2镀层由ZrO2镀层或Nb2O5镀层替代。
10.根据权利要求1所述的一种光伏玻璃减反膜，其特征在于，所述的物理气相沉积包括磁控溅射、电子束蒸发、热蒸发和真空离子镀中的任一种。
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