CN101351521A - 用于光生伏打组件的含氟聚合物涂敷的薄膜 - Google Patents

用于光生伏打组件的含氟聚合物涂敷的薄膜 Download PDF

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Publication number
CN101351521A
CN101351521A CNA2006800500097A CN200680050009A CN101351521A CN 101351521 A CN101351521 A CN 101351521A CN A2006800500097 A CNA2006800500097 A CN A2006800500097A CN 200680050009 A CN200680050009 A CN 200680050009A CN 101351521 A CN101351521 A CN 101351521A
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fluoropolymer
film
coating
polymer
multipolymer
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CN101351521B (zh
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M·德伯加利斯
L·G·斯诺
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DuPont Electronics Inc
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EI Du Pont de Nemours and Co
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    • Y10T428/31935—Ester, halide or nitrile of addition polymer

Abstract

包括聚合物基底薄膜和在聚合物基底薄膜上的含氟聚合物涂层的含氟聚合物涂敷的薄膜。含氟聚合物涂层包括选自氟乙烯的均聚物和共聚物以及偏二氟乙烯的均聚物和共聚物聚合物的含氟聚合物，含氟聚合物混有包括选自羧酸、磺酸、氮杂环丙烷、酐、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物中的官能团的相容性粘合剂聚合物。聚合物基底薄膜在其表面上包括与相容性粘合剂聚合物相互作用促进含氟聚合物涂层粘结到基底薄膜上的官能团。

Description

用于光生伏打组件的含氟聚合物涂敷的薄膜
发明领域
本发明涉及形成用作光生伏打组件中背板的含氟聚合物涂敷的薄膜。
发明背景
光生伏打电池用于由日光产生电能，提供电力产生传统方法的绿色替代方案。这些太阳能电池由必须被保护以免受环境影响如湿气、氧气和UV光的各种半导体系统构成。电池通常被玻璃和/或塑料薄膜封装层护封在两侧上形成称为光生伏打组件的多层结构。含氟聚合物薄膜由于它们的极好强度、耐侯性、耐UV性和防潮性被视为光生伏打组件中的重要部件。这些组件中尤其有用的是用作组件背板的含氟聚合物薄膜和聚酯薄膜的薄膜复合材料。这类复合材料传统上由含氟聚合物尤其是聚氟乙烯(PVF)的预成型薄膜粘着到聚酯基底薄膜尤其是聚对苯二甲酸乙二醇酯上来制备。当使用含氟聚合物如PVF作为组件的背板时，它的性质明显提高了组件寿命，允许组件保证期至最高25年。含氟聚合物背板经常以具有聚对苯二甲酸乙二醇酯(PET)薄膜的层合材料的形式使用，一般是PET夹在两个含氟聚合物薄膜之间。
但是，具有在户外暴露多年后不会脱层的结合的聚合物基底上预成型含氟聚合物薄膜的层合材料难以制备。现有技术体系如Simms的美国专利3133854、Kim等的美国专利5139878和Schmidt等的美国专利6632518描述了能产生耐用叠层结构的预成型薄膜用底漆和粘合剂。但是，这些方法在实际层压步骤前要求施加至少一个粘合剂层或底漆和粘合剂层两者。层压步骤然后要求施加热和压力形成层合材料。因此，使用预成型含氟聚合物薄膜的现有技术层合材料制造昂贵和/或要求资本密集设备。由于预成型含氟聚合物薄膜必须具有足够的厚度以为制造和随后加工期间的处理提供强度，因此得到的层合材料还可能结合厚的昂贵含氟聚合物层，即比有效保护层所需要的厚。
发明概述
本发明提供包括聚合物基底薄膜和在聚合物基底薄膜上的含氟聚合物涂层的含氟聚合物涂敷的薄膜。含氟聚合物涂层包括选自氟乙烯的均聚物和共聚物以及偏二氟乙烯的均聚物和共聚物的含氟聚合物，含氟聚合物混有包括选自羧酸、磺酸、氮杂环丙烷、酐、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物中的官能团的相容性粘合剂聚合物。聚合物基底薄膜在其表面上包括与所述相容性粘合剂聚合物相互作用促进含氟聚合物涂层粘结到基底薄膜上的官能团。
本发明提供含氟聚合物涂敷的聚合物薄膜，其具有比用预成型含氟聚合物薄膜制造层合材料少的全部加工步骤，同时提供对基底的强粘合性和含氟聚合物涂敷的基底的良好耐久性。另外，提供涂料形式的含氟聚合物能在需要时使较薄的含氟聚合物层成为可能来节约成本。使用含氟聚合物涂料还能为含氟聚合物涂敷薄膜的预定用途而设计的含氟聚合物层内引入添加剂，例如，改善阻透性的填料。
发明详述
含氟聚合物
用在本发明的含氟聚合物涂敷的薄膜中的含氟聚合物选自氟乙烯(VF)的均聚物和共聚物以及偏二氟乙烯(VF2)的均聚物和共聚物聚合物。优选地，含氟聚合物选自包括至少60mol％氟乙烯的氟乙烯均聚物和共聚物以及包括至少60mol％偏二氟乙烯的偏二氟乙烯均聚物和共聚物。更优选地，含氟聚合物选自包括至少80mol％氟乙烯的氟乙烯均聚物和共聚物以及包括至少80mol％偏二氟乙烯的偏二氟乙烯均聚物和共聚物。含氟聚合物与不含氟聚合物例如丙烯酸类聚合物的混合物也适合本发明的实施。均聚物聚氟乙烯(PVF)和均聚物聚偏二氟乙烯(PVDF)完全适合本发明的实施。
对于利用VF共聚物或VF2共聚物的本发明的实施，共聚用单体可为氟化的或未氟化的或它们的混合物。术语“共聚物”指VF或VF2与任何数量其它氟化单体单元的共聚物，结果形成二元共聚物、三元共聚物、四元共聚物等。如果使用非氟化单体，则应限制使用的数量，以便共聚物保留含氟聚合物的所需性质，即耐侯性、耐溶剂性、阻透性等。优选地，使用氟化共聚用单体，包括含氟烯烃、氟化乙烯基醚或氟化间二氧杂环戊烯。有用的氟化共聚用单体的例子包括四氟乙烯(TFE)、六氟丙烯(HFP)、氯三氟乙烯(CTFE)、三氟乙烯、六氟异丁烯、全氟丁基乙烯、全氟(丙基乙烯基醚)(PPVE)、全氟(乙基乙烯基醚)(PEVE)、全氟(甲基乙烯基醚)(PMVE)、全氟-2，2-二甲基-1，3-间二氧杂环戊烯(PDD)和全氟-2-亚甲基-4-甲基-1，3-二氧戊环(PMD)以及许多其它的。
均聚物PVDF涂料可由高分子量PVDF形成。可使用PVDF和(甲基)丙烯酸烷基酯聚合物的混合物。聚甲基丙烯酸甲酯是尤其理想的。通常，这些混合物可包括50-70wt％的PVDF和30-50wt％的(甲基)丙烯酸烷基酯聚合物，优选聚甲基丙烯酸甲酯。这类混合物可包含稳定混合物的增容剂和其它添加剂。美国专利3524906、4931324和5707697中描述了作为主要成分的聚偏二氟乙烯或偏二氟乙烯共聚物和丙烯酸类树脂的这类混合物。
均聚物PVF涂料可由高分子量PVF形成。Uschold的美国专利6242547和6403740公开了合适的VF共聚物。
相容性粘合剂聚合物
在根据本发明的含氟聚合物涂敷的薄膜中使用的相容性粘合剂聚合物包括选自羧酸、磺酸、氮杂环丙烷、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物中的官能团。相容性粘合剂聚合物优选具有(1)与组合物中的含氟聚合物相容的骨架组成，和(2)能与基底薄膜表面上的互补官能团反应的侧链官能团。粘合剂聚合物骨架与含氟聚合物的相容性会变化但足够相容，以便粘合剂聚合物可以以所需数量被引入到含氟聚合物内以固定含氟聚合物涂层到基底薄膜上。但是，通常，主要由氟乙烯和偏二氟乙烯得到的均聚物和共聚物将表现出促成具有上述官能团的丙烯酸类、氨基甲酸酯、脂肪族聚酯、聚酯氨基甲酸酯、丙烯酰胺、脲和聚碳酸酯骨架的相容特性。
由丙烯酸类和丙烯酰胺单体得到的自由基加成聚合物也能很好地适合利用大量可用官能单体引入侧官能团。一些代表性例子包括用于引入环氧基的缩水甘油基的丙烯酸酯和甲基丙烯酸酯。然后通过环氧官能丙烯酸类基团与氨或伯烷基胺的反应将这些转变成反应性氨基醇基团。羧酸、异氰酸酯、羟基和酐官能团都是可得到的，分别使用丙烯酸/甲基丙烯酸、甲基丙烯酸异氰酸根合乙酯、甲基丙烯酸羟乙酯或马来酐。大量其它官能单体都可用于官能团引入，这在本领域中是众所周知的。
优选的相容性粘合剂聚合物为胺官能聚合物，更优选胺官能丙烯酸类聚合物。
颜料和填料
如果需要，可在制造过程中引入颜料和填料到含氟聚合物涂料组合物分散体内来获得各种颜色、不透明度和/或其它性质效果。基于含氟聚合物固体，优选使用数量为约1-约35wt％的颜料。可使用的典型颜料包括透明颜料如无机含硅颜料(二氧化硅颜料，例如)和常规颜料。可使用的常规颜料包括金属氧化物如二氧化钛和氧化铁；金属氢氧化物；金属小薄片，如铝小薄片；铬酸盐，如铬酸铅；硫化物；硫酸盐；碳酸盐；碳黑；二氧化硅；滑石；瓷土；酞菁蓝和绿、有机红；有机褐红和其它有机颜料和染料。优选的为在加工过程中在高温下稳定的颜料。还优选选择颜料的类型和数量以防止对含氟聚合物涂料所需性质如耐侯性的任何明显反面影响。
可通过混合颜料和分散树脂将颜料配制成研磨料，分散树脂可与要引入颜料的含氟聚合物组合物相同或相容。可通过常规手段如砂磨研磨、球磨研磨、立式球磨机研磨或双辊磨研磨来形成颜料分散体。尽管一般不需要或不使用，但可引入其它添加剂，如玻璃纤维和矿物填料、防滑剂、增塑剂、成核剂等。
UV添加剂和热稳定剂
含氟聚合物涂料组合物可包含一种或多种光稳定剂作为添加剂。光稳定剂添加剂包括吸收紫外辐射的化合物如羟基二苯甲酮和羟基苯并三唑。其它可能的光稳定剂添加剂包括位阻胺光稳定剂(HALS)和抗氧化剂。如果需要，还可使用热稳定剂。
阻挡颗粒
在优选实施方案中，含氟聚合物涂料组合物包括阻挡颗粒。优选地，该颗粒为板状颗粒。这类颗粒往往在施加涂料过程中进行排列，由于水、溶剂和气体如氧气不能容易地通过颗粒本身，因此在得到的涂层中形成机械阻挡，这减少了水、溶剂和气体的透过。例如，在光生伏打组件中，阻挡颗粒大大提高了含氟聚合物的防潮性和增强了为太阳能电池提供的保护。如果使用的话，基于涂料中含氟聚合物组合物的总干重，阻挡颗粒的存在数量优选为约0.5-约10wt％。
典型板状填料颗粒的例子包括云母、玻璃小薄片和不锈钢小薄片以及铝小薄片。板状颗粒优选为云母颗粒，包括涂有氧化物层如铁或钛氧化物的云母颗粒。这些颗粒具有约10-200μm、优选20-100μm的平均粒径，不超过50％的小薄片颗粒具有超过约300μm的平均粒径。美国专利3087827(Klenke和Stratton)、3087828(Linton)和3087829(Linton)中描述了涂有氧化物层的云母颗粒。这些专利中描述的云母涂有钛、锆、铝、锌、锑、锡、铁、铜、镍、钴、铬或钒的氧化物或水合氧化物。还可使用带涂层云母的混合物。
含氟聚合物涂料组合物配方
含氟聚合物涂料组合物可包含含氟聚合物溶液或分散体形式的含氟聚合物。使用沸点高到足以在薄膜形成/干燥过程中避免气泡形成的溶剂制备典型的含氟聚合物溶液或分散体。对于分散体形式的聚合物，有助于含氟聚合物聚结的溶剂是优选的。调整这些溶液或分散体中的聚合物浓度以获得可使用的溶液粘度，聚合物浓度可随具体聚合物、组合物的其它组分和所用的工艺设备和条件而变化。优选地，对于溶液，基于组合物的总重量，含氟聚合物的存在数量为约10wt％至约25wt％。对于分散体，基于组合物的总重量，含氟聚合物的存在数量优选为约25wt％至约50wt％。
涂料组合物中聚合物的形式取决于含氟聚合物的类型和所用溶剂。均聚物PVF通常为分散形式。均聚物PVDF可为分散体或溶液形式，取决于选择的溶剂。例如，均聚物PVDF可在室温下在许多极性有机溶剂如酮、酯和一些醚中形成稳定溶液。合适的例子包括丙酮、甲基乙基酮(MEK)和四氢呋喃(THF)。取决于共聚用单体含量和所选的溶剂，VF和VF2的共聚物可以以分散体或溶液形式使用。
在使用均聚物聚氟乙烯(PVF)的本发明的一种优选形式中，使用含氟聚合物的分散体制备合适的涂料配方。美国专利2419008、2510783和2599300中详细描述了分散体的特性和制备。优选的PVF分散体形成在二甲基乙酰胺、碳酸丙烯酯、γ-T内酯、N-甲基吡咯烷酮和二甲基亚砜中。
为了制备分散体形式的含氟聚合物涂料组合物，通常首先在合适的溶剂中共同研磨含氟聚合物和相容性粘合剂聚合物以及任选地一种或多种分散剂和/或颜料。或者，单独研磨或适当混合各种组分。在溶剂中可溶的组分如相容性粘合剂聚合物不需要研磨。
可使用各种磨用于分散体的制备。通常，磨使用搅拌的重研磨介质，如砂、钢丸、玻璃珠、陶瓷丸、氧化锆或砾石，如在球磨中，可从UnionProcess，Akron，Ohio得到的ATTRITOR，或搅拌介质磨如可从Netzsch，Inc.，Exton，Pennsylvania得到的“Netzsch”磨。研磨分散体足以引起PVF解附聚的时间。分散体在Netzsch磨中的典型停留时间为30秒直到10分钟。
在涂料组合物中使用水平足以提供对聚合物基底薄膜的所需粘结但低于会显著负面影响含氟聚合物所需性质的水平的粘合剂聚合物。优选地，涂料组合物包含约1-约40wt％的粘合剂聚合物，更优选约1-约25wt％的粘合剂聚合物，最优选1-约20wt％的粘合剂聚合物，基于含氟聚合物的重量。
基底薄膜和底漆
本发明中使用的聚合物基底薄膜可选自各种聚合物，热塑性塑料是优选的。聚合物基底薄膜在其表面上包括能与相容性粘合剂聚合物相互作用以促进含氟聚合物涂料对基底薄膜的粘结的官能团。聚合物基底薄膜优选为聚酯，更优选为选自聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二酯和聚对苯二甲酸乙二醇酯/聚萘二甲酸乙二酯共挤出物的聚酯。
基底薄膜中还可包括填料，其中它们的存在可改善基底的物理性质，例如，更高的模量和抗拉强度。它们还可提高含氟聚合物对基底薄膜的粘合性。一种示例性填料为硫酸钡，但也可使用其它的。
要被涂敷的聚合物基底薄膜表面可本来具有适合粘结的官能团，如聚酯薄膜中的羟基和/或羧酸或聚酰胺薄膜中的胺和/或酸官能团。但是，许多聚合物基底可能需要活化或进一步从活化受益，这可通过表面处理来实现。也就是说，可通过在表面上形成羧酸、磺酸、氮杂环丙烷、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物的官能团使表面有接受力。可通过化学暴露如到气态路易斯酸如BF3或到硫酸或到热氢氧化钠实现活化。优选地，可通过暴露一个或二个表面到明火同时冷却相对表面来活化表面。还可通过对薄膜进行高频火花放电如电晕处理或大气氮等离子处理实现活化。
在本发明的优选实施方案中，底漆层被沉积在聚合物基底薄膜上，并提供能与含氟聚合物涂料组合物中的相容性粘合剂聚合物相互作用以促进含氟聚合物涂料对基底薄膜的粘结的官能团。合适的底漆可包括聚胺、聚酰胺、丙烯酰胺聚合物(尤其是非晶态丙烯酰胺)、聚乙烯亚胺、乙烯共聚物或三元共聚物、酸改性聚烯烃(例如马来酸化聚烯烃)、丙烯酸酯或甲基丙烯酸酯聚合物(如乳液聚合物)、聚酯(如分散体)、聚氨酯(如分散体)、环氧聚合物、乙氧基丙烯酸类低聚物和它们的混合物。这个方面的一个例子是通过施加聚乙烯亚胺底漆涂料引入胺官能团。第二个例子是酸或酐官能热塑性聚合物如DuPont公司以商标BYNEL
Figure A20068005000900101
出售的聚合物与基础PET基底薄膜的共挤出。当在例如制造过程中被拉伸的PET基底薄膜上使用底漆时，可在拉伸基底薄膜前或后施加底漆。
涂料施加
可通过常规涂敷手段将用于制备根据本发明的含氟聚合物涂敷的薄膜的含氟聚合物组合物作为液体直接施加到合适的聚合物基底薄膜上，不需要形成预成型薄膜。产生这种涂层的技术包括常规方法流延、浸涂、喷涂和涂抹。当含氟聚合物涂料包含分散体形式的含氟聚合物时，一般通过流延分散体到基底薄膜上施加，使用常规手段，如喷涂、辊涂、刀涂、帘流、凹槽辊涂布机或允许施加没有条痕或其它缺陷的均匀涂层的任何其它方法。喷涂和辊涂施加是最常用的施加方法。流延分散体的干燥涂层厚度优选为约2.5μm(0.1密耳)和约250μm(10密耳)，优选在约13μm(0.5密耳)至约130μm(5密耳)之间。
施加后，干燥湿溶液或分散体除去溶剂和如果需要在基底薄膜上热聚结形成含氟聚合物涂层。对于含氟聚合物为溶液形式的一些组合物，组合物可被涂到基底薄膜上并在环境温度下风干。尽管不需要产生聚结薄膜，但通常需要加热以更快地干燥涂层。干燥温度因此优选在约25℃(环境条件)至约200℃(烘箱温度-薄膜温度将较低)的范围内。所用温度还应足以促进粘合剂聚合物中官能团与聚合物基底薄膜的官能团的相互作用以提供含氟聚合物涂层对基底薄膜的牢固粘结。该温度可随使用的粘合剂聚合物和基底薄膜的官能团变化很大，并可为室温到超过下面所述分散体形式含氟聚合物聚结所需温度的烘箱温度。
当组合物中的含氟聚合物为分散体形式时，必需除去溶剂和还必需加热含氟聚合物到含氟聚合物颗粒聚结成连续薄膜的足够高温度。优选地，加热涂层中的含氟聚合物至约150℃至约250℃的温度。使用的溶剂优选促进聚结，即与没有溶剂存在时所需温度相比能有用于聚结的较低温度。因此，用于聚结聚合物的条件将随使用的含氟聚合物、流延分散体和基底薄膜的厚度和其它操作条件变化。对于均聚物PVF涂料和约1-约3分钟的停留时间，可使用约340°F(171℃)至约480°F(249℃)的烘箱温度聚结薄膜，并发现约380°F(193℃)至约450°F(232℃)的温度尤其令人满意。当然，烘箱空气温度不代表含氟聚合物涂层达到的温度，含氟聚合物涂层达到的温度较低。
在本发明的优选形式中，将含氟聚合物涂料组合物施加到基底薄膜上。优选地，基底薄膜包括能提供与所述相容性粘合剂聚合物相互作用以促进粘结的官能团的底漆层。优选地，基底薄膜为聚酯如聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二酯和聚对苯二甲酸乙二醇酯/聚萘二甲酸乙二酯的共挤出物。在本发明的另一优选形式中，将含氟聚合物涂料施加到基底薄膜的两个表面上。这可在聚合物基底薄膜的两个侧上同时进行或交替进行，交替进行时，干燥被涂敷的基底薄膜，翻到未涂敷侧重新提交相同的涂敷头施加涂料到薄膜的相对侧上实现在薄膜两个侧上的涂敷。
光生伏打组件
按照本发明制备的含氟聚合物涂敷薄膜尤其用在光生伏打组件中。光生伏打组件的典型构造包括厚的玻璃层作为上釉材料。玻璃保护太阳能电池，太阳能电池包括嵌在防潮塑料密封胶如交联乙烯醋酸乙烯中的结晶硅片和线。或者，同样用封装材料护封在两侧上的载体片上的各种半导体材料如CIGS(铜-铟-镓-硒化物)、CTS(镉-碲-硫化物)、a-Si(非晶态硅)和其它一些能适用于薄薄膜太阳能电池。粘着到封装物上的是背板。按照本发明制造的含氟聚合物涂敷薄膜用作这类背板。含氟聚合物涂料包括选自氟乙烯的均聚物和共聚物以及偏二氟乙烯的均聚物和共聚物聚合物的含氟聚合物，并混合有包含选自羧酸、磺酸、氮杂环丙烷、酐、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物中的官能团的相容性粘合剂聚合物。聚合物基底薄膜在其表面上包括与相容性粘合剂聚合物相互作用促进含氟聚合物涂料对基底薄膜粘结的官能团。聚合物基底薄膜优选为聚酯，更优选为选自聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二酯和聚对苯二甲酸乙二醇酯/聚萘二甲酸乙二酯共挤出物的聚酯。聚酯提供电绝缘性和防潮性，为背板的一种经济部件。优选聚合物基底薄膜的两个表面都涂有含氟聚合物，形成聚酯在两个含氟聚合物涂料层之间的夹层。含氟聚合物薄膜为背板提供优异的强度、耐侯性、耐UV性和防潮性。
实施例
测试方法
180度剥离强度
使用Model 4201 Instron以2”/min测量剥离强度，记录最大值并对三个样品取平均值(ASTM D1876-01 T-剥离试验)。如果在剥离开始步骤期间容易用手剥离样品，则记录0的值。
湿度箱剥离试验
在将样品从湿度箱取出后，用剃刀和直尺划刻样品产生1/4”宽条。使用1”悬突作为把柄，用缓慢均匀的拉力以大致180度角度拉这个片，直到薄膜破裂或剥离产生。在EVA/玻璃或EVA/含氟聚合物涂层界面处薄膜破裂和剥离被认为是合格结果。在含氟聚合物涂层和PET基底之间剥离被认为不合格。
交叉粘合性
在将样品从湿度箱取出后，借助不锈钢模板，用剃刀划刻样品产生穿过薄膜到玻璃表面的11个相隔约3/32英寸(2.4mm)的平行切口。在与第一批切口成直角的位置重复该过程产生100个正方形的栅格。用一条透明带(3M Brand No.467 PSA tape)，0.75乘2.16英寸(1.9乘5.5cm)牢固地挤压到划刻区域上，带定位于划刻线的平行方向上。然后以90°角快速但无急拉地扯拉带。含氟聚合物涂层和PET基底之间的任何失败都被认为是不合格。
水蒸气传输速率(WVTR)
使用Mocon Permatron-W
Figure A20068005000900131
700仪器在37.8℃和100％的permiant相对湿度下测量水蒸气传输速率。
实施例1-5
实施例1-5说明了PFV基粘结涂料，该涂料包含胺官能丙烯酸类粘合剂或环氧官能丙烯酸类粘合剂，用于涂敷预先已用聚乙烯亚胺(PEI)或乙烯丙烯酸共聚物(EAA)作底漆的聚对苯二甲酸乙二醇酯(PET)薄膜。结果显示，通常，较多的粘合剂聚合物是较好的。结果表明，没有粘合剂聚合物时未获得有效的粘结。
PVF基涂料配方
表1：含氟聚合物涂料配方
  配方   PVF分散体*   粘合剂聚合物**   粘合剂聚合物数量   基于PVF的wt％粘合剂
  A   20.0   胺官能丙烯酸类   2.8   10
  B   20.0   胺官能丙烯酸类   5.6   20
  C   20.0   环氧官能丙烯酸类   2.2   10
  D   20.0   环氧官能丙烯酸类   4.4   20
  E   20.0   无   0   0
*PVF(可从DuPont得到)，预先分散到碳酸丙烯酯(可从Huntsman得到)中，42％固体
**胺官能丙烯酸类为甲基丙烯酸甲酯/甲基丙烯酸-2-羟基-3-氨基丙酯97.8/2.2，30％固体，在2-丙醇/甲苯55/45中。
**环氧官能丙烯酸类为甲基丙烯酸甲酯/甲基丙烯酸缩水甘油酯98/2，38％固体，在2-丙醇/甲苯55/45中。
PET+底漆基底
表2：具有PEI涂层的基底
Figure A20068005000900141
表3：具有EAA涂层的基底
  基底   PET厚度(微米)   涂料厚度(nm)
  样品4   100   40
  样品5   100   80
过程
1.合并表1的成分并在油漆振荡器上搅拌15分钟以混合。
2.使用12密耳刮刀在表2和3中4密耳PET薄片的每一个上制备表1中混合物的刮涂膜以产生大约1.2密耳干的含氟聚合物涂层。
3.沿湿的刮涂膜的1个边施加纯PVF分散体(在碳酸丙烯酯中42％)的大珠粒以帮助剥离测试。
4.将涂敷的薄片夹到金属框内并放到200℃或220℃下的预热烘箱中保持3分钟。
5.从烘箱中取出聚结且干燥的薄膜并冷却。
6.垂直于大PVF珠粒切割1英寸条。
7.使用解剖刀(scalpel)开始在PVF珠处的剥离。
8.使用Model 4201 Instron以2”/min测量剥离强度，记录最大值并对三个样品取平均值(ASTM D1876-01 T-剥离试验)。如果在剥离开始步骤期间容易用手剥离样品，则记录0的值。
表4：剥离测试结果
  样品   基底   含氟聚合物配方  200℃烘焙温度剥离强度(KG/in)   220℃烘焙温度剥离强度(KG/in)
  1A   样品1   A   0   0
  1B   样品1   B   0   0.76
  1C   样品1   C   0   0
  1D   样品1   D   1.18   1.14＊
  1E   样品1   E   0   0
  2A   样品2   A   0.78   0.57
  2B   样品2   B   1.2   1.47
  2C   样品2   C   0   0
  2D   样品2   D   1.46   1.28＊
  2E   样品2   E   0   0
  3A   样品3   A   0   0.59
  3B   样品3   B   1.36   1.26
  3C   样品3   C   0   0
  3D   样品3   D   1.48   1.42＊
  3E   样品3   E   0   0
  4A   样品4   A   1.39   1.44
  4B   样品4   B   1.53   1.33
  4C   样品4   C   0   1.07
  4D   样品4   D   1.29   1.35＊
  4E   样品4   E   0   0
  5A   样品5   A   1.15   1.35
  5B   样品5   B   1.44   1.59
  5C   样品5   C   1.2   1.13
  5D   样品5   D   0   1.38＊
  5E   样品5   E   0   0
*表示能经受1000小时85℃/85％湿度箱试验的配方/基底/烘焙温度组合(只测试选择的样品)。
湿度箱试验
样品制备
按与实施例1-5那些相同的方式制备含氟聚合物涂敷的PET基底，除了省略步骤3的边缘珠。在从烘箱取出样品并使它们冷却后，使用手持实验室电晕处理器电晕处理含氟聚合物涂层侧。然后使用以下过程将电晕处理的样品层压到玻璃板(4”x8”x1/8”)上。
利用1”含氟聚合物涂敷的PET悬突将以下夹层放在真空板上。
---------含氟聚合物涂敷的PET薄膜，含氟聚合物涂层面向下
----反应性EVA薄膜
-------玻璃板
1.使夹层居中并用硅橡胶垫盖住
2.将金属框放在橡胶垫上并施加真空20分钟
3.将夹层+真空板放到室温烘箱内并开始加热到150℃的目标
4.在150℃下保持样品20分钟
5.从烘箱中取出样品，释放真空并使样品冷却
6.将得到的层合材料放到控制在85℃/85％湿度的湿度箱中的涂料样品架上。
7.将样品暴露到湿度箱1000小时，然后使用剥离试验和交叉带试验检查粘合性。
实施例6-9
实施例6-9说明了PVF涂料组合物，其包含胺官能丙烯酸类粘合剂，用于涂敷用聚烯丙胺底漆作为底漆的PET薄膜。
实施例6
实施例6说明了将白色PVF涂料施加到用聚烯丙胺底漆作底漆的未着色和着色PET薄膜的两侧上。
由下面表5中的配方制备白色PVF涂料配方。表5中列出的热稳定剂溶液由4.0wt％Irganox
Figure A20068005000900161
1035(Ciba)、1wt％Weston
Figure A20068005000900162
THOP(Crompton)和95wt％碳酸丙烯酯制备。表5中列出的胺官能丙烯酸类聚合物溶液通过在甲苯和异丙醇溶剂中使甲基丙烯酸甲酯/甲基丙烯酸缩水甘油酯(98/2)与氨进行补充反应将缩水甘油基转化成2-羟基-3-氨基丙基产生伯胺官能丙烯酸类聚合物来制备。
表5
 成分   湿wt.   干wt.  基于PVF的Wt％
 PVF分散体(在PC中40％)   58.55   23.42   N.A.
 白色颜料分散体   23.55   10.65   45.5
 热稳定剂溶液   2.9   0.15   0.66
 胺官能丙烯酸类溶液   14.43   4.32   18.4
使用刮刀，将白色PVF涂料配方涂在用聚烯丙胺底漆作底漆的2密耳未着色PET薄膜上和在用聚烯丙胺底漆作底漆的硫酸钡着色3.8密耳宽PET薄膜上。在预热的烘箱中烘焙涂料10分钟，在200℃下10分钟。然后用相同的PVF配方在相对侧上涂敷冷却的带涂层薄膜，并在200℃下烘焙15分钟。表6显示了在着色和未着色PET薄膜上得到的涂层干薄膜厚度的范围：
表6
Figure A20068005000900171
实施例7
实施例7说明了施加包含珍珠般云母阻挡颗粒的PVF涂料到用聚烯丙胺底漆作底漆的着色和未着色PET薄膜的两侧上。
由下面表7中的配方制备珍珠般PVF涂料配方：
表7
Figure A20068005000900181
使用刮刀，将珍珠般PVF涂料配方涂在用聚烯丙胺底漆作底漆的2密耳宽未着色PET薄膜上和在用聚烯丙胺底漆作底漆的3.8密耳宽硫酸钡着色PET薄膜上。在预热的烘箱中烘焙该涂料10分钟，在200℃下10分钟。然后用相同的PVF配方在相对侧上涂敷冷却的带涂层薄膜，并在200℃下烘焙15分钟。表8显示了得到的干涂层厚度的范围：
表8
Figure A20068005000900182
实施例8
在实施例8中，通过测量水蒸气传输速率(WVTR)评价分别具有白色着色和云母着色含氟聚合物涂料的实施例6(样品7)和实施例7(样品2)的双侧涂敷PET薄膜的防潮性。表9显示了当使用阻挡颗粒如云母时防潮性的提高，如较低的WVTR值所示。
表9
Figure A20068005000900191
实施例9
在实施例9中，比较按照实施例6制备的白色两侧涂敷PET样品(样品1)和常规预成型PVF薄膜层压到两侧上的PET薄膜样品的收缩性。前者在PET基底中包含填料(硫酸钡)，而后者没有。表10显示了各种温度下测量的收缩数据。
表10
Figure A20068005000900192
注：两侧涂敷薄膜层厚度(密耳)1/3.8/0.7
    两侧层压薄膜层厚度(密耳)1.5/3/1.5
实施例10
实施例10说明了施加白色着色和未着色聚偏二氟乙烯(PVDF)涂料到用聚烯丙胺底漆作底漆的未着色和着色PET薄膜的一个侧上。
未着色PVDF涂料配方由表11中所示的以下组分制备：
表11
Figure A20068005000900201
在3mm玻璃珠存在下在油漆振荡器上分散混合物10分钟。
白色着色涂料配方由表12中显示的以下组分来制备：
表12
Figure A20068005000900202
使用7密耳刮刀，使用7密耳刮刀将透明PVDF配方和白色PVDF配方涂在用聚烯丙胺底漆作底漆的未着色2密耳PET薄膜上和着色3.8密耳PET薄膜上。类似地涂敷对比物3.8密耳没有底漆的PET。在预热的400°F对流箱中烘焙涂敷的薄膜5分钟。冷却后，使用解剖刀尝试从PET薄膜除去PVF薄膜。着色和未着色的薄膜都可从没有底漆的PET剥离，但不能从有底漆的PET剥离。

Claims (19)

1.一种含氟聚合物涂敷的薄膜，包括：
聚合物基底薄膜；和
在所述聚合物基底薄膜上的含氟聚合物涂层，所述含氟聚合物涂层包括选自氟乙烯的均聚物和共聚物以及偏二氟乙烯的均聚物和共聚物聚合物的含氟聚合物，含氟聚合物混有包括选自羧酸、磺酸、氮杂环丙烷、酐、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物中的官能团的相容性粘合剂聚合物；
所述聚合物基底薄膜在其表面上包括与所述相容性粘合剂聚合物相互作用促进所述含氟聚合物涂层粘结到所述基底薄膜上的官能团。
2.权利要求1的含氟聚合物涂敷的薄膜，其中所述聚合物基底薄膜在其表面上包括提供与所述粘合剂相互作用的所述官能团以促进所述含氟聚合物涂层对所述基底薄膜的粘结的底漆层。
3.权利要求1的含氟聚合物涂敷的薄膜，其中所述聚合物基底薄膜表面上的所述官能团选自羧酸、磺酸、氮杂环丙烷、胺、异氰酸酯、三聚氰胺、环氧基、羟基、酐及其混合物。
4.权利要求1的含氟聚合物涂敷的薄膜，其中所述相容性粘合剂聚合物为官能丙烯酸类聚合物。
5.权利要求1的含氟聚合物涂敷的薄膜，其中所述相容性粘合促进聚合物为胺官能丙烯酸类聚合物。
6.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物选自包括至少60mol％氟乙烯的氟乙烯均聚物和共聚物以及包括至少60mol％偏二氟乙烯的偏二氟乙烯均聚物和共聚物。
7.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物选自包括至少80mol％氟乙烯的氟乙烯均聚物和共聚物以及包括至少80mol％偏二氟乙烯的偏二氟乙烯均聚物和共聚物。
8.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物涂层包括约1-约40wt％的所述相容性粘合剂聚合物，基于含氟聚合物固体含量。
9.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物涂层还包括颜料。
10.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物涂层还包括约1-约35wt％的颜料，基于含氟聚合物固体含量。
11.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物涂层在所述基底薄膜的两个表面上。
12.权利要求2的含氟聚合物涂敷的薄膜，其中所述基底薄膜包括聚酯。
13.权利要求9的含氟聚合物涂敷的薄膜，其中所述底漆包括选自聚烯丙胺/三聚氰胺聚合物、聚乙烯亚胺聚合物、乙烯丙烯酸共聚物和酸改性聚烯烃中的聚合物。
14.权利要求1的含氟聚合物涂敷的薄膜，其中所述含氟聚合物涂层具有约0.1至约2.0密耳的厚度。
15.权利要求1的含氟聚合物涂敷的薄膜，其中所述基底薄膜具有约0.5至约10密耳的厚度。
16.权利要求1的含氟聚合物涂敷的薄膜，其中所述底漆层具有约20至约100nm的厚度。
17.权利要求1的含氟聚合物涂敷的薄膜，其中所述基底薄膜的表面被活化。
18.权利要求1的含氟聚合物涂敷的薄膜，其中所述基底薄膜包括填料。
19.包括权利要求1的含氟聚合物涂敷的薄膜作为背板的光生伏打组件。
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US8197933B2 (en) 2012-06-12
CA2628967C (en) 2015-03-17
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US20090260677A1 (en) 2009-10-22
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US7553540B2 (en) 2009-06-30
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