CN110809566A - 获得涂有溶胶-凝胶型抗反射涂层的纹理化玻璃基材的方法 - Google Patents
获得涂有溶胶-凝胶型抗反射涂层的纹理化玻璃基材的方法 Download PDFInfo
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Abstract
本发明涉及一种用于获得一种材料的方法,该材料包括纹理化玻璃基材,该基材在其至少一个纹理化面上涂覆有基于多孔二氧化硅的溶胶‑凝胶类型抗反射涂层,所述方法包括以下步骤:‑将包含至少一种二氧化硅前体和至少一种成孔剂的溶液施加到所述基材的所述至少一个纹理化面上的步骤,然后‑目的为固结所述抗反射涂层的热处理步骤,所述方法使得:在所述施加步骤之前,使玻璃基材经受预热步骤,以使打算用所述抗反射涂层涂覆的所述至少一个纹理化面在紧临在该施用步骤之前具有在30℃至100℃,尤其50℃至80℃范围内的温度。
Description
本发明涉及材料领域,该材料包括涂覆有至少一个抗反射涂层的玻璃基材。它尤其涉及可用作农业、园艺或城市温室的屋顶的材料。
打算用作为温室用玻璃的玻璃材料必须满足在光学性能和耐久性方面的某些要求。它们的透光率必须是尽可能高的,为此,已知使用超透明玻璃基材,并在这些基材上涂以通过溶胶-凝胶类型方法获得的基于多孔二氧化硅的抗反射层。由于它们的低折射率(理想地接近玻璃基材的折射率的平方根)和由于它们的高化学耐久性,这些层被证明是特别合适的。这样的层特别在申请FR2908406中描述。
据证明,通过使用能够散射光的基材,放置在温室下的农作物的产量也得到了提高。这是因为散射均匀的照明可以优化植物的生长。为此,已经开发出具有至少一个纹理化面的玻璃基材。这样的基材例如通过使玻璃辊压而获得,也就是说,通过使热玻璃在本身具有纹理的辊之间通过而获得,该辊适合压印玻璃的表面并产生浮雕。在本领域中也使用术语“压印玻璃”。
然而,据证明,通过将溶液施加到纹理化面上来沉积上述类型的溶胶-凝胶抗反射层不允许获得完美优化的光学性能,特别地对于最大的纹理。发明人已经能够证明,即使溶液均匀地被沉积在玻璃的整个表面上,在干燥过程中,玻璃的纹理也会引起毛细作用力,毛细作用力促使在结构化结构的谷中流动,从而,在干燥后,形成厚度不均一的层,在其中该层是非常薄的,甚至在结构的峰位置不存在。这由此导致光反射因子的空间不均匀性,并且因此导致总的透光因子比该层完全均匀时更低。
本发明的目的是克服这些缺点,本发明的主题是获得一种材料的方法,该材料包括纹理化玻璃基材,该基材在其至少一个纹理化面上涂覆有基于多孔二氧化硅的溶胶-凝胶类型抗反射涂层,所述方法包括以下步骤:
-将包含至少一种二氧化硅前体和至少一种成孔剂的溶液施加到所述基材的所述至少一个纹理化面上的步骤,然后
-目的为固结所述抗反射涂层的热处理步骤,
所述方法使得:在所述施加步骤之前,使玻璃基材经受预热步骤,以使打算用所述抗反射涂层涂覆的所述至少一个纹理化面在紧临在该施用步骤之前具有在30℃至100℃范围内的温度。
玻璃基材通常以厚度在1mm至10mm,特别地2mm至8mm,甚至3mm至6mm的范围的板形式,通常为矩形板的形式存在。板的横向尺寸通常在0.5至3m的范围内。
玻璃基材优选由钠钙硅石类型的玻璃组成。但是,可以使用其它类型的玻璃,例如硼硅酸盐或铝硅酸盐玻璃。从氧化铁的总重量含量在10至200ppm,特别地20至150ppm的范围内的意义上,玻璃基材优选是超透明玻璃。玻璃基材的在标准EN 410的含义上的透光率有利地为至少90%,甚至91%。
“纹理化面”应理解为是指所讨论的面具有浮雕状体,由一系列的峰和谷构成。这种浮雕状体可以是周期的或随机的。
打算用抗反射涂层涂覆的基材的至少一个纹理化面优选具有这样的轮廓,该轮廓在标准ISO 4287:1997的意义下使得:
-参数Rz在18至200μm,特别地20至150μm,尤其50至120μm的范围内,和
-参数RSm在从500到2500μm,特别地从600到2000μm的范围内。
这些值是通过使用25µm的λs和8mm的λc滤波器获得的。
纹理能够产生雾度并因此使光散射。玻璃基材有利地具有至少20%,特别地40%,甚至50%或70%,甚至80%的雾度。通常,参数Rz的值越高,雾度越高。雾度根据标准ISO14782:1999测量。
玻璃基材可以仅具有一个纹理化面,还或可以具有两个纹理化面。
优选通过辊压玻璃来获得纹理化玻璃基材。这种技术在于,在熔融炉的出口处,在玻璃成形期间,使热玻璃在两个辊之间,通常是金属辊之间通过,其中至少一个辊是纹理化的,也就是说具有浮雕状体。然后,热玻璃被纹理化辊压印,由此产生的浮雕妆体在玻璃冷却期间得以保留。
其它纹理化方法也是可能的,如化学或机械侵蚀:以酸(尤其氢氟酸)侵蚀或喷砂,通过将磨料颗粒喷射到玻璃表面上。但是,这些方法是更昂贵的且对环境的影响更较大。
涂层是溶胶-凝胶类型的,也就是说通过溶胶-凝胶方法获得。
溶胶-凝胶方法通常包括:
-形成“溶胶”,即包含至少一种前体(在这里为二氧化硅)的溶液,
-将这种溶液施用于要涂覆的表面上,
-通过热处理使涂层固结或致密化。
溶液优选包含至多10重量%,特别地5重量%,并且通常至少1重量%的干提取物。
溶液的溶剂优选地选自水,有机溶剂以及水和有机溶剂的混合物。有机溶剂优选地选自醇(例如异丙醇,丙醇,乙醇等)和丙酮。术语“溶剂”在这里以其一般意义进行使用,因而溶剂可以由溶剂的混合物组成。
从溶液的溶剂包含按重量计至少50%,甚至60%,甚至70%或80%或90%或95%的意义上讲,溶液优选是含水的。就其由水组成的意义而言,溶剂甚至优选是完全含水的。这是因为使用水溶液或至少主要使用水溶液在环境,工业卫生和成本方面显示出优点,以及在获得的层的耐久性方面也显示出优点。另外,事实证明,溶剂中水含量的增加,在厚度均匀性方面与本发明有关的优点变得更大。
防反射涂层基于二氧化硅。涂层的二氧化硅含量优选为至少60重量%,特别地70重量%,甚至80重量%或90重量%。涂层有利地由二氧化硅组成。
二氧化硅前体优选是选自硅的烷醇盐和卤化物的化合物,例如原硅酸四乙酯(TEOS)。二氧化硅前体也可以是在这些化合物与溶液的其它成分(例如水,当溶剂包含水时)之间发生的化学反应的产物。事实上,这些化合物在溶液形成期间,因此在施加之前能够至少部分地水解。
造孔剂优选为固体,其尺寸的选择使得可以改变孔的尺寸。所述成孔剂优选是颗粒,特别是基本上球形的颗粒,例如空心或实心珠的形式。所述成孔剂优选具有有机性质。举例而言,成孔剂包括聚合物珠,特别地选自聚甲基丙烯酸甲酯(PMMA),(甲基)丙烯酸甲酯/(甲基)丙烯酸共聚物,聚碳酸酯,聚酯或聚苯乙烯的聚合物的珠。
要施加的溶液优选是酸性的。其pH优选为0至5,特别地1至3。
除了二氧化硅前体和成孔剂之外,溶液可以包含其它组分,例如pH调节剂,表面活性剂等。
溶液的施用优选通过使用至少一个辊的涂覆来进行,该技术也被称为“辊涂覆”,并且其使得可以精确地控制沉积的溶液的量以及沉积物的空间均匀性。根据这种技术,优选地使玻璃基材在在彼此几乎接触并沿相同方向或相反方向旋转的计量辊和施涂辊下方前进,使施涂辊与待涂覆的基材的面接触,待施用的溶液通过这两个辊之间的顶部倒入。穿过计量辊和涂覆辊之间的溶液可沉积在施涂辊的表面,然后转移到要涂覆的表面。
也可以使用其它已知的施加技术,例如喷涂,浸涂,幕涂等技术。
在施加步骤之后立即地,在热处理步骤之前,根据本发明的方法优选地包括干燥步骤。该步骤旨在加速在涂层中所含溶剂的蒸发。它可以通过任何已知的方式进行,例如通过吹入热空气。这时,空气温度优选在50℃至160℃之间,并且干燥时间优选在5至60秒之间。
热处理步骤允许加固抗反射涂层。在此步骤期间,成孔剂也被除去,在涂层内形成孔隙,因此允许降低其折射率。
热处理优选包括使涂层达到至少400℃,特别地500℃的温度。
热处理优选是玻璃的钢化处理。玻璃的钢化在于将玻璃再加热至通常大于600℃的温度,然后通常通过排放冷空气的喷嘴将其快速冷却。这种快速冷却使得可以在玻璃基材的表面上产生压缩应力,从而增强其机械强度和冲击强度。
该抗反射涂层优选地包括具有特征性较小尺寸的封闭孔,其有利地平均至少为20nm,特别地40nm,甚至50nm,并且至多1μm,特别地500nm,甚至100nm。孔的分布优选在厚度上基本均匀。涂层中的孔的体积比例优选在10%至90%之间,特别地在20%至80%之间,甚至在30%至70%之间。
抗反射涂层的平均厚度优选在10nm至10μm,特别地20nm至1μm,甚至30至300nm或50至200nm的范围内。
该抗反射涂层有利地具有对于600nm的波长为至多1.40,特别地1.30的折射率。
抗反射涂层可以是由玻璃基材承载的唯一涂层。或者,其它涂层可以存在于基材的同一面上或另一面上。特别地,有利的是,在玻璃基材和抗反射涂层之间插入包含硅,氧和任选地氮和/或碳的底层,例如二氧化硅层,碳氧化硅或氮氧化硅层。当玻璃包含碱金属离子时,这样的底层特别地是有用的,因为它能够形成对所述离子的阻挡层。折射率在1.35和1.45之间的无孔二氧化硅底层也被证明可用于增加材料的透光率。这样的底层优选具有在10至200nm,特别地80至120nm的范围内的厚度。它们可以通过任何类型的方法来沉积,例如,溶胶-凝胶,化学气相沉积(CVD),阴极溅射等类型。
无需知道原因,据证明,预热步骤允许使抗反射涂层的厚度均匀化。这由此引起在材料的半球形透光率方面的增益。
进行预热步骤,使得要用所述抗反射涂层涂覆的至少一个纹理化面紧邻在施加步骤之前的温度在30℃至100℃,特别地50℃至80℃的范围内。“紧邻”优选地应理解为是指在开始施加溶液之前的至多5秒,特别地3秒,甚至1秒,要被涂覆的纹理化面具有在上述范围内的温度。
可以通过任何已知的方式,例如通过高温计,来测量待涂覆面的温度。
预热步骤优选通过辐射进行,例如借助红外灯或微波辐射,或者通过对流进行,例如通过吹入热空气。
根据本发明的方法通常是连续的,并且特别地使玻璃基材顺次通过预热装置中,例如烘箱中,然后用于施加溶液的装置中,例如使用至少一个辊的装置中,然后通过热处理设备中,例如钢化炉中。预热装置优选地位于施加装置的紧邻上游,以便能够在施加开始之前能够最好地控制待涂覆面的温度。干燥装置有利地插入在施加装置和热处理装置之间。优选地,干燥装置采用在热处理装置处预热的空气。
根据本发明获得的材料的特征尤其在于抗反射涂层的厚度特别均匀。
因此,本发明的另一主题还是一种材料,特别地能够通过根据本发明的方法获得的材料,其包括在其至少一个纹理化面上涂覆有基于多孔二氧化硅的溶胶-凝胶类型抗反射涂层的纹理化玻璃基材。所述纹理化面具有由一系列峰和谷组成的浮雕状体,并且在峰位置的抗反射涂层的局部厚度为至少60nm,特别地80nm,甚至100nm,并且在所述峰位置的抗反射涂层的局部厚度为700nm,特别地600nm,甚至500nm。
优选地,在所述峰位置的抗反射涂层的局部厚度的值是在所述谷底位置的抗反射涂层的局部厚度的值的至少40%,特别地50%或60%。通过显微镜观察,特别地使用扫描电子显微镜的观察,特别地对材料的边缘面进行的观察允许测量这些局部厚度。
如上所述,玻璃基材可仅具有一个纹理化面或两个纹理化面。至少一个纹理化面涂覆有溶胶-凝胶类型的抗反射涂层。基材的另一面,无论它是否是纹理化的,都可以涂覆或不涂覆有溶胶-凝胶类型的抗反射涂层。在这种情况下,所有特征的组合都是可能的。
该材料优选在标准EN410的意义上具有至少92%,特别地93%,甚至94%的透光率。当基材的两个面都涂覆有抗反射涂层时,透光率甚至可以为至少96%,特别地97%或98%。
当抗反射涂层被沉积在基材的面上时,其允许使透光率提高至少1%,特别地2%,甚至3%。在这种情况下,这是绝对的而不是相对的提高。
在对根据本发明的方法的描述期间,特别是上面介绍的与基材和抗反射涂层有关的特征也适用于根据本发明的材料。
本发明的另一主题是温室,特别地农业、园艺或城市的温室,其包含至少一种根据本发明的材料。该材料优选地被结合到温室的屋顶中。涂覆有抗反射涂层的材料的纹理化面可以被朝向温室的内侧或外侧。
根据本发明的材料的其它应用也是可能的。根据本发明的材料例如可以用作为光伏电池的正面。
以下实施例非限制性地说明了本发明。
按照在申请FR2908406中描述的方法,通过使用包含TEOS作为二氧化硅前体的完全水溶液和呈聚合物珠粒形式的成孔剂,将两个具有纹理化面的玻璃基材涂覆有溶胶-凝胶抗反射涂层。
被称为基材A和基材B的两个基材在未涂覆状态下具有下表1中给出的在表面状态和光学性质方面的特征。粗糙度参数Rz和RSm根据标准ISO 4287:1997定义,雾度根据标准ISO 14782:1999定义,透光率(TL)根据标准EN410定义。
基材 | Rz (µm) | RSm (µm) | 雾度(%) | TL(%) |
A | 72 | 1530 | 50 | 91 |
B | 100 | 1800 | 55 | 91 |
表1。
在比较例中,在施加溶液之前玻璃基材不进行预热。在根据本发明的实施例中,使用红外灯将玻璃基材进行了预热,使得在紧邻施加溶液之前,基材的温度为70℃。该温度使用高温计进行测量。
对于每个实施例,在下表2中给出了获得的透光率的增益。表示为ΔTL的绝对增益以%表示。
A | B | |
ΔTL(%)-比较 | 1.3 | 0.9 |
ΔTL(%)-发明 | 1.8 | 1.4 |
表2。
因此可以看出,预热步骤使得可以改善涂层的抗反射效率,使得材料具有更高的透光率。以绝对值表示的与预热步骤有关的增益约为0.5%。
Claims (14)
1.获得一种材料的方法,该材料包括纹理化玻璃基材,该纹理化玻璃基材在其至少一个纹理化面上涂覆有基于多孔二氧化硅的溶胶-凝胶类型抗反射涂层,所述方法包括以下步骤:
-将包含至少一种二氧化硅前体和至少一种成孔剂的溶液施加到所述基材的所述至少一个纹理化面上的步骤,然后
-目的为固结所述抗反射涂层的热处理步骤,
所述方法使得:在所述施加步骤之前,使玻璃基材经受预热步骤,以使打算用所述抗反射涂层涂覆的所述至少一个纹理化面紧临在施用之前具有在30℃至100℃,尤其50℃至80℃的范围内的温度。
2.根据权利要求1所述的方法,使得所述溶液是含水的。
3.根据前述权利要求中任一项所述的方法,使得所述玻璃基材的旨在用抗反射涂层涂覆的基材的至少一个纹理化面具有这样的轮廓,该轮廓在标准ISO 4287:1997的意义下使得:
-参数Rz在18至200μm,特别地20至150μm,尤其50至120μm的范围内,和
-参数RSm在500到2500μm,特别地600到2000μm的范围内。
4.根据前述权利要求中任一项所述的方法,使得所述玻璃基材具有至少20%,尤其40%,甚至50%的雾度。
5.根据前述权利要求中任一项所述的方法,使得在玻璃基材的在标准EN 410的意义内的透光率为至少90%,甚至91%。
6.根据前述权利要求中任一项所述的方法,使得所述溶液的施加通过用至少一个辊的涂覆来实现。
7.根据前述权利要求中任一项所述的方法,使得所述二氧化硅前体是选自硅的烷醇盐和卤化物的化合物。
8.根据前述权利要求中任一项所述的方法,使得至少一种成孔剂是有机性质的,尤其包含聚合物珠,特别地选自聚甲基丙烯酸甲酯,(甲基)丙烯酸甲酯/(甲基)丙烯酸共聚物,聚碳酸酯,聚酯或聚苯乙烯的聚合物的珠。
9.根据前述权利要求中任一项所述的方法,使得所述预热步骤是通过辐射,特别地通过红外灯,或通过对流,特别地通过吹入热空气来进行的。
10.根据前述权利要求中任一项所述的方法,使得所述热处理是玻璃的钢化处理。
11.根据前述权利要求中任一项所述的方法,该方法包括紧临在施加步骤之后并在热处理步骤之前的干燥步骤。
12.如前述权利要求中任一项所述的方法,使得所述抗反射涂层具有为10nm至10μm,特别地为20nm至1μm的平均厚度。
13.一种材料,特别地能够根据权利要求1至12中任一项的方法获得的材料,其包含纹理化玻璃基材,该纹理化玻璃基材在其至少一个纹理化面上涂覆有基于多孔二氧化硅的溶胶-凝胶类型的抗反射涂层,所述纹理化面具有由一系列峰和谷组成的浮雕状体,所述材料使得在峰位置的抗反射涂层的局部厚度为至少60nm,特别地80nm,甚至100nm,和抗反射涂层在谷位置的局部厚度为至多700nm,特别地600nm,甚至500nm。
14.一种温室,其包括至少一种根据前一项权利要求所述的材料。
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CN115135140A (zh) * | 2020-03-11 | 2022-09-30 | 日本板硝子株式会社 | 温室和带涂布膜的玻璃板 |
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CA3192510A1 (en) * | 2020-08-28 | 2022-03-03 | Agc Glass Europe | Improved greenhouse glazing |
EP4396144A1 (en) * | 2021-08-31 | 2024-07-10 | AGC Glass Europe | Greenhouse glazing |
WO2023198912A1 (fr) | 2022-04-15 | 2023-10-19 | Saint-Gobain Glass France | Procédé de fabrication d'un substrat transparent comprenant un revêtement |
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CN115135140A (zh) * | 2020-03-11 | 2022-09-30 | 日本板硝子株式会社 | 温室和带涂布膜的玻璃板 |
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Also Published As
Publication number | Publication date |
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RU2020102711A3 (zh) | 2021-11-02 |
EP3649091B1 (fr) | 2022-02-16 |
RU2770760C2 (ru) | 2022-04-21 |
RU2020102711A (ru) | 2021-08-10 |
MX2019015597A (es) | 2020-08-03 |
EP3649091A2 (fr) | 2020-05-13 |
ES2910156T3 (es) | 2022-05-11 |
KR20200027957A (ko) | 2020-03-13 |
KR102608292B1 (ko) | 2023-12-01 |
FR3068690B1 (fr) | 2019-08-02 |
US20200131082A1 (en) | 2020-04-30 |
US11465934B2 (en) | 2022-10-11 |
WO2019008282A3 (fr) | 2019-02-28 |
CN110809566B (zh) | 2023-08-01 |
FR3068690A1 (fr) | 2019-01-11 |
WO2019008282A2 (fr) | 2019-01-10 |
PL3649091T3 (pl) | 2022-04-25 |
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