CN102325831B - 白色涂布的聚酯膜，其制备工艺和其作为太阳能组件中背面盖的用途 - Google Patents
白色涂布的聚酯膜，其制备工艺和其作为太阳能组件中背面盖的用途 Download PDFInfo
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- CN102325831B CN102325831B CN201080008685.4A CN201080008685A CN102325831B CN 102325831 B CN102325831 B CN 102325831B CN 201080008685 A CN201080008685 A CN 201080008685A CN 102325831 B CN102325831 B CN 102325831B
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Abstract
本发明涉及一种白色涂布的聚酯膜，它对典型的用作太阳能组件中的包封材料的乙烯-醋酸乙烯酯(EVA)具有优异的粘合性。通过包含至少一种聚氨酯和交联剂的聚合物涂层获得了所述良好的粘合性能。
Description
本发明涉及一种白色涂布的聚酯膜，它对典型的用作太阳能组件中的包封材料的乙烯-醋酸乙烯酯(EVA)具有优异的粘合性。通过包含至少一种聚氨酯和交联剂的聚合物涂层获得了上述良好的粘合性能。
太阳能组件用来把太阳光直接转化成电能。作为最重要的组件，他们包含众多太阳能电池，这些电池在太阳能组件内部以适宜的方式相互电连接并且嵌入不同的材料中。这些安排满足下面的目的，其中：
·太阳能电池的透明的，耐辐射和耐候的覆盖，
·保护易碎的太阳能电池防止力学影响，
·保护太阳能电池和电子连接防止湿气，
·防止与电子组件接触。
典型的，太阳能组件由下述组成(见图1)：
·透明的前盖，其通常为玻璃；
·太阳能电池嵌入到其中的透明的聚合物材料；最经常使用的材料是以膜形式的乙烯-醋酸乙烯酯(EVA)，其在相对较高的温度下熔融，通过合适的添加剂交联并因此非常能经受外部影响。根据EVA的类型和存在于其中的添加剂，交联工艺需要不同的时间量。在所谓“标准固化”和“快速固化”类型之间设置有区别。
·可以大体上是透明的或着色的背面盖。
典型的，采用聚合物膜或聚合物膜的层合体(例如氟聚合物和聚酯膜的)。白色不透明的背面盖提供的优势是落在太阳能电池之间的光被从所述背面盖的上部反射，这增加了太阳能组件的效率。
图1显示了用于光伏发电的太阳能组件的基本结构，其中1是前盖，2是太阳能电池，3是EVA，以及4是背面盖。
在太阳能组件的制备工艺中，在真空层合机中在大约150℃的温度下，把前盖、EVA与太阳能电池和背面盖相互结合到一起。为了获得太阳能组件20-40年的要求的长寿命，必须确保所述前和背部盖对EVA嵌入材料持久的优异粘合性。
具有带有EVA粘合涂层的白色不透明聚酯膜将会是所希望的，其对潮湿和升高的温度具有优异的长期稳定性并且适于用作太阳能组件中的背面盖。所述涂层应当具有良好的力学性能以没有损坏的经受发生于膜制备工艺中、膜的缠绕和展开时以及太阳能组件的制备中的应力。为了满足不太昂贵的获得太阳能电力能力的需要，所述聚酯膜也应当可以以经济上可行的方式生产；然而，目前这种白色涂布的膜是未知的。
EP-A-1 826 826描述了配置有EVA粘合涂层的聚酯膜。基膜也可以着色为白色的、黑色的或者别的颜色；然而，在实施例中，仅采用了透明膜。所述涂层包含交联剂和聚合物，所述聚合物选自玻璃化转变温度为20-100℃的聚酯类，玻璃化转变温度为20-100℃的丙烯酸酯类，这些聚酯类和丙烯酸酯类的组合，以及这些聚酯类和/或丙烯酸酯类与水解度为70-90mol％的聚乙烯醇的组合。根据公开的内容，所用交联剂可以是脲或环氧化合物、三聚氰胺或包含唑啉基团的聚合物，后者被描述为是特别适宜的。然而，由于已知的酯基的水解敏感性，聚酯基涂层并没有显示出很适合于能在高温和潮湿下在长期内确保对EVA的良好粘合性。甚至在聚酯膜制备工艺中升高的温度下或者在经受太阳能组件中的光和热施加的应力下，聚乙烯醇趋向于降解和褪色。因此请求保护的膜看起来很难适宜用作太阳能组件中耐久的背面盖。
EP-A-1 908 587请求保护对于可见光具有良好反射性的多层白色膜，其被描述为在UV光的影响下对于褪色是稳定的。通过改性膜层具有31-60重量％的惰性粒子以及另一层具有0-30重量％的惰性粒子，获得了对于可见光的良好反射性。根据公开的内容，硫酸钡特别适于这个目的。除了聚对苯二甲酸乙二醇酯外，所用的另一种原材料是聚萘酸乙二醇酯。据称该膜主要适于作为液晶显示器中的反射体， 但是也提到用于太阳能组件中的背面盖的膜的可能用途。由于添加了如此高比例的惰性粒子，在制备工艺中几乎可以避免膜的撕裂，然而令人怀疑的是对于太阳能应用这种膜是否还能以经济上可接受的价格生产。而且，该公开没提及应用于太阳能组件中的情况下如何在高温和潮湿下在长期内确保对EVA的良好粘合。
本发明的一个目的是提供具有耐久的，非常经受EVA粘合涂层的白色不透明的聚酯膜，其或者单独的或者为与别的材料的复合物，适宜作为太阳能组件中的背面盖。
除了别的特性，该膜值得关注的是甚至在升高的温度和潮湿下的低透明性、高白度、高光泽、低收缩性、对于EVA非常好的粘合值，以及涂层的耐机械性。而且，当采用其自身的再研磨物时，该膜也保持了低黄度指数。
根据本发明通过提供白色不透明涂布的聚酯膜实现了上述目的，该涂层包含至少下述组分：
1.)聚氨酯，
2.)交联剂。
涂布的聚酯膜的低透明性意味着透明度为＜40％，优选＜35％以及更优选＜30％。
高白度意味着涂布的聚酯膜具有＞70，优选＞75以及更优选＞80的伯杰白度。
高光泽度意味着涂布的聚酯膜在20°的测量角下测量的光泽度＞5，优选＞10以及更优选＞20。
低收缩性意味着涂布的聚酯膜在150℃在15分钟内在机器方向和横向的收缩低于2.5％，优选低于2.0％，以及更优选低于1.5％。
对于EVA非常好的粘合值意味着在180°的角度分离由根据本发明涂布的膜和EVA组成的层合体所需的力为＞50N/15mm，优选＞70N/15mm。
EVA粘合涂层对升高的温度和潮湿优异的长期稳定性意味着在85℃/85％的相对空气湿度下存储1000小时时期后，分离由本发明涂 布的膜和EVA组成的层合体所需的力仍旧至少为初始值的50％。
涂层良好的耐机械性意味着通过毫微压痕法测定的涂层硬度为＞0.2GPa，优选＞0.25GPa以及更优选＞0.3GPa。
当由玻璃、EVA和聚酯膜组成的层合体按照ISO4892在氙气候老化仪中经受加速气候老化20000小时期间后(相当于在中欧气候条件下大约20年的户外使用)而没有分层，那么该聚酯膜适于作为太阳能组件中的背面盖。制备后基膜的SV值大于700，优选大于650，以使得甚至在作为太阳能组件中的背面盖长期使用后仍能具有充足的机械强度。
为了膜的良好缠绕和加工性能，膜的平均粗糙度Ra应当为＞20，优选＞25，以及更优选＞30nm。而且，在相对高的温度和空气湿度下，缠绕的涂布膜不应当粘结到相邻的膜层上，因为这使得进一步的膜的加工复杂化或者甚至使得其不可能。这种性能指的是下文中的“膜粘连”并且通过在限定的气候条件下存储后相互之间的膜层分离所需的力来描述。在根据本发明涂布的膜的情况下，在40℃/80％的相对空气湿度下在20小时后需要低于50g的力来实现该目的。
尽管采用了其自身再研磨物的低黄度指数意味着在采用了最高达50％的由本发明涂布的膜制备的再研磨物的情况下，聚酯膜的黄度指数低于80，优选低于70。
本发明EVA粘合涂层的说明
本发明白色不透明聚酯膜在至少一边具有EVA粘合涂层，该涂层包含至少下述组分：
1.)聚氨酯，
2.)交联剂。
下文中详细说明了适于本发明的聚氨酯和交联剂。
可以通过多羟基化合物(下文中也指“多元醇”)和多异氰酸酯的反应来制备适于用于本发明涂层制剂的聚氨酯水分散体。多羟基化合物的实例为聚酯多元醇类、聚碳酸酯多元醇类和聚氧化烯多元醇类。
聚酯多元醇应当理解其含义是那些通过至少一种低分子量二元醇 与至少一种多元羧酸的聚缩合形成的化合物，或者别的通过诸如ε-己内酰胺的环化合物开环聚合制备的那些；所述二元醇选自乙二醇、二甘醇、三甘醇、1，2-丙二醇、1，3-丁二醇、1，5-戊二醇、1，4-丁二醇、1，6-己二醇、二丙二醇、三丙二醇、新戊二醇、环己二醇和环己二甲醇；所述多元羧酸例如丙二酸、马来酸、丁二酸、己二酸、壬二酸、酒石酸、庚二酸、癸二酸、草酸、对苯二酸、间苯二酸、富马酸、二聚酸、偏苯三酸或所述多元羧酸的衍生物。
聚碳酸酯多元醇是那些通过至少一种二元醇与至少一种碳酸酯的反应形成的化合物，所述二元醇例如乙二醇、丙二醇、1，3-丙二醇、1，4-丁二醇、1，5-戊二醇、1，6-己二醇、1，9-壬二醇、1，8-壬二醇、新戊二醇、二甘醇、二丙二醇、1，4-环己二醇或双酚A，所述碳酸酯例如碳酸二甲酯、碳酸二苯酯、碳酸亚乙酯或碳酰氯。
除了别的路线外，通过至少一种环醚采用低分子量二元醇作为引发剂的开环聚合来形成聚氧化烯多元醇，所述环醚例如氧杂环丁烷、四氢呋喃或四氢吡喃；所述二元醇例如乙二醇、二甘醇、三甘醇、1，2-丙二醇、1，3-丁二醇、1，4-丁二醇、1，6-己二醇、二丙二醇、三丙二醇或新戊二醇。在这些聚氧化烯多元醇中，优选其烯基包含2-7个碳原子以及更优选3-6个碳原子的那些化合物。
适宜的多异氰酸酯包括芳族二异氰酸酯、芳族-脂肪族二异氰酸酯、脂肪族二异氰酸酯、脂环族二异氰酸酯和它们的衍生物或改性物。
芳族二异氰酸酯的例子包括间-亚苯基二异氰酸酯、对-亚苯基二异氰酸酯、4，4’-二亚苯基二异氰酸酯、1，5-萘二异氰酸酯、4，4’-二苯基甲烷二异氰酸酯、2，4-或2，6-甲苯二异氰酸酯、4，4’-甲苯胺二异氰酸酯或4，4’-二苯基醚二异氰酸酯。
芳族-脂肪族二异氰酸酯的实例包括1，3-或1，4-二甲苯二异氰酸酯和这些组分的混合物。
适宜的脂肪族二异氰酸酯的实例包括三亚甲基二异氰酸酯、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯、五亚甲基二异氰酸酯、1，2-亚丙基二异氰酸酯、1，2-亚丁基二异氰酸酯、2，3-亚丁基二异氰酸酯、 1，3-亚丁基二异氰酸酯、2，4，4-或2，2，4-三甲基六亚甲基二异氰酸酯或2，6-二异氰酸甲基己酸酯。
脂环族二异氰酸的实例包括1，3-环戊烷二异氰酸酯、1，3-环己烷二异氰酸酯、1，4-环己烷二异氰酸酯、3-异氰酸甲基-3，5，5-三甲基环己基异氰酸酯(异佛尔酮二异氰酸酯)、4，4’-亚甲基-双(环己基异氰酸酯)、甲基2，4-环己烷二异氰酸酯、甲基2，6-环己烷二异氰酸酯、1，4-双(异氰酸甲基)环己烷、1，3-双(异氰酸甲基)环己烷或者2，5-或2，6-双(异氰酸甲基)二环[2.2.1]庚烷。
多异氰酸酯衍生物的实例为二聚体、三聚体、缩二脲化合物、脲基甲酸酯、碳二亚胺和上述多异氰酸酯的脲化合物。
多异氰酸酯改性物的实例为异氰酸酯终端的齐聚或聚合化合物，其由上述多元醇和化学计量过量的上述多异氰酸酯或其衍生物形成。这些改性的多异氰酸酯可以单独使用或者与进一步的多异氰酸酯结合使用。
聚氨酯的基本制造是现有技术，例如记载于G.Oertel的“聚氨酯手册”，第二版，Carl Hanser Verlag，1994中。
典型的，在聚氨酯的制备中，首先通过多元醇与化学计量过量的多异氰酸酯的反应(任选添加催化剂)来合成带有异氰酸酯端基团的预聚物，在随后的步骤中用进一步的多元醇或一元、二元、三元或更高官能的胺对所述预聚物进行扩链。
为了改善与水的相容性以及由此的可分散性，离子基团经常结合入聚氨酯中，例如诸如羧酸盐、磺酸盐或硫酸单酯的阴离子基团，或者诸如季铵基团的阳离子基团。在这些官能团中，优选阴离子基团，特别是羧基和磺酸基。
可以在此通过选择适当的改性反应物制备预聚物或者适当的改性扩链剂来把离子基团引入聚氨酯中。带有羧基官能的典型的扩链剂为例如二羟甲基丙酸、二羟甲基丁酸、二羟甲基戊酸或偏苯三酸二(乙二醇)酯。可以采用的进一步的带有羧基官能的扩链剂为例如氨基乙酸、β-丙胺酸、6-氨基己酸、4-氨基安息香酸、3，4-氨基安息香酸或 赖氨酸。二醇磺酸、氨基-或二氨基磺酸(例如磺胺酸、萘基-氨基磺酸、4，4’-二氨基二苯基二磺酸、2，2’-或4，4’-二氨基二苯基醚2-磺酸)作为扩链剂相反获得带有磺酸酯官能的聚氨酯。
最终聚氨酯分散体中的阴离子基团优选以他们的盐的形式存在，在一开始制备预聚物期间和/或由扩链后的聚氨酯制备水性分散体期间通过用碱中和来形成所述盐。对于中和，可能的是采用有机碱(例如三乙胺、氢氧化三乙铵)或无机碱(例如氢氧化铵、氢氧化钠、氢氧化钾)。对于中和优选采用无机碱，特别是氢氧化铵。
扩链典型的导致粘度的显著增加，因此这种形式的聚氨酯在水中几乎不能分散。在别的方法中，有两种一般的方法避免该问题：
a)在高剪切力下把预聚物分散在水和扩链剂中，扩链发生于水相中，但是在分散的粒子中。为了降低预聚物的粘度，或是采用升高温度或者添加有机溶剂(例如N-甲基吡咯烷酮、二甲基乙酰胺、丁基二甘醇)，然而所述溶剂保留于最后的分散体中。
b)在水混溶性低沸点有机溶剂(例如丙酮)中合成全部聚氨酯。把溶液分散在水中以及然后通过蒸馏除去所述溶剂。这种方法的优点是形成的聚氨酯不含溶剂，但是制备费用比方法a)中高。
为了制备本发明涂料制剂，优选由脂肪族聚氧化烯多元醇或脂肪族聚碳酸酯多元醇与多异氰酸酯制备水性聚氨酯分散体。
用于本发明涂层的交联剂是至少一种水可混溶的或水分散性组分，其带有能进入交联反应的反应性基团，例如带有噁唑啉基、碳二亚胺基、环氧基、异氰酸酯基或蜜胺基的聚合物。在这些中，特别是优选带有噁唑啉或碳二亚胺基的聚合物。
包含噁唑啉基的聚合物是通过下述的加成聚合形成的大分子化合物
a)根据结构式(I)到(II)的噁唑啉衍生物与
b)至少一种进一步的共聚单体。
在上述结构式(I)到(II)中，R1、R2、R3和R4基可以分别独立表示氢原子、卤原子、烷基、芳烷基、苯基或取代的苯基。R5是包含可聚合双键的非环基。
卤原子的例子是氟、氯、溴和碘，优选氯和溴。烷基的例子为甲基、乙基、正丙基、异丙基、正丁基、异丁基、戊基和己基。芳烷基基团理解为是指那些包含链长度为1-5个碳原子的烷基的基团，例如苄基、苯乙基、二苯甲基和萘基甲基基团。取代的苯基可以例如是氯苯基、溴苯基、甲氧基苯基、乙氧基苯基、甲基氨基苯基、乙基氨基苯基、二甲基氨基苯基、甲基乙基氨基苯基和二乙基氨基苯基。带有可聚合双键的非环基的例子为乙烯基和异丙烯基。
噁唑啉衍生物a)的实例包括2-乙烯基-2-噁唑啉、2-乙烯基-4-甲基-2-噁唑啉、2-乙烯基-5-甲基-2-噁唑啉、2-异丙烯基-2-噁唑啉、2-异丙烯基-4-甲基-2-噁唑啉和2-异丙烯基-5-乙基-2-噁唑啉。为了制备带有噁唑啉基的聚合物，单独采用噁唑啉衍生物a)或者采用所述化合物两种或更多种的组合是可能的。在所述噁唑啉衍生物中，特别优选2-异丙烯基-2-噁唑啉。
所用共聚单体b)原则上可以是能与噁唑啉衍生物a)共聚的所有化合物。共聚单体b)的实例为诸如甲基丙烯酸甲酯、甲基丙烯酸丁酯和甲基丙烯酸2-乙基己酯的甲基丙烯酸酯类，诸如甲基丙烯酸、衣康酸和丙二酸的不饱和羧酸类，诸如甲基丙烯腈的不饱和腈类，诸如甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺的不饱和酰胺类，诸如醋酸乙烯酯和丙酸乙烯酯的乙烯基酯类，诸如甲基乙烯基醚、乙基乙烯基醚的乙烯基醚类，诸如乙烯、丙烯的α-烯烃，诸如氯乙烯、偏二氯乙烯和氟乙烯的卤代α，β-不饱和化合物，还有诸如苯乙烯和α-甲基苯乙 烯的α，β-不饱和芳族化合物。所述共聚单体b)可以单独使用或者两种或更多种化合物结合使用。
例如可以通过把噁唑啉衍生物a)、至少一种共聚单体b)和例如过氧化苯甲酰或偶氮异丁腈的自由基引发剂添加到适宜的水混溶性有机溶剂中，并加热所得溶液来制备包含噁唑啉基的聚合物。在聚合结束后，可以添加水并且可通过蒸馏完全或部分除去所述有机溶剂，这会得到包含噁唑啉基的聚合物水分散体，其直接适于本发明涂料溶液的制备。
可替代地，阴离子聚合噁唑啉衍生物类a)和共聚单体类b)也是可能的，例如采用正丁基锂。
干聚合物中噁唑啉基的含量典型地为0.5-10毫摩/克，优选1.5-10毫摩/克。干聚合物的玻璃化转变温度在0和100℃之间，优选20到95℃。
来自Nippon Shokubai(日本)的名字为“Epocros
”是商业上可获得的适宜的包含噁唑啉基的聚合物水分散体。在本文中，来自上述生产商的水溶性的、不含溶剂的“Epocros
WS”系列产品特别适于本发明的涂料溶液。
包含碳二亚胺基的聚合物是每分子带有至少两个碳二亚胺基的大分子化合物，其可以在催化剂存在下通过二异氰酸酯的缩聚制备。相应的工艺是现有技术并和其他的事物记载于EP-A-0 878 496中。适宜的制备包含碳二亚胺基的聚合物的初始原料为芳族、脂肪族和脂环族二异氰酸酯，例如甲苯二异氰酸酯、二甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、环己烷二异氰酸酯、异佛尔酮二异氰酸酯和二环己基二异氰酸酯。为了改善可溶性或可分散性，包含碳二亚胺基的聚合物也可以包含表面活性剂、聚环氧烷或亲水单体，例如季铵盐、二烷基氨基醇和羟基烷基磺酸。
包含环氧基的聚合物为例如双酚-表氯醇基聚合物、环脂肪族聚合的环氧化物、基于线型酚醛清漆的环氧化合物、环氧-烯烃聚合物、基于多元醇-缩水甘油基化合物的环氧化合物以及环氧基硅烷聚合物。特 别适宜的是聚乙二醇二缩水甘油醚、聚丙二醇二缩水甘油醚、新戊二醇二缩水甘油醚、1，6-己二醇二缩水甘油醚、甘油(glyerol)聚缩水甘油醚、三羟甲基丙烷聚缩水甘油醚、山梨醇聚缩水甘油醚和双酚A二缩水甘油醚。
包含异氰酸酯基的聚合物为多异氰酸酯，例如2，4-甲苯二异氰酸酯、2，6-甲苯二异氰酸酯、间-亚苯基二异氰酸酯、对-亚苯基二异氰酸酯、4，4’-二苯基甲烷二异氰酸酯、2，4’-二苯基甲烷二异氰酸酯、2，2’-二苯基甲烷二异氰酸酯、3，3’-二甲基-4，4’-二亚苯基二异氰酸酯、3，3’-二羟甲基-4，4’-联亚苯基二异氰酸酯、3，3’-二氯-4，4’-联亚苯基二异氰酸酯、1，5-萘二异氰酸酯、1，5-四氢萘二异氰酸酯、四亚甲基二异氰酸酯、1，6-六亚甲基二异氰酸酯、十二亚甲基二异氰酸酯、三甲基六亚甲基二异氰酸酯、1，3-环亚己基二异氰酸酯、1，4-环亚己基二异氰酸酯、二甲苯二异氰酸酯、四甲基亚二甲苯基二异氰酸酯、氢化二甲苯二异氰酸酯、赖氨酸二异氰酸酯、异佛尔酮二异氰酸酯、4，4’-二环己基二异氰酸酯、3，3-二甲基-4，4’-二环己基甲烷二异氰酸酯、四甲基二甲苯二异氰酸酯，以及带有异氰酸酯端基的聚合物，所述端基来自上述化合物与异氰尿酸酯或缩二脲型的三官能多异氰酸酯或者二羟基或更高的多羟基多元醇的反应。
蜜胺理解为是指能通过羟甲基蜜胺衍生物的反应制备的化合物，所述衍生物通过蜜胺和甲醛与诸如甲醇、乙醇和异丙醇(或这些醇的混合物)的较低级醇的缩合获得。羟甲基蜜胺衍生物的实例为单羟甲基蜜胺、二羟甲基蜜胺、三羟甲基蜜胺、四羟甲基蜜胺、五羟甲基蜜胺和六羟甲基蜜胺。
本发明涂料组合物可以任选包含低于10重量％，优选低于5重量％含量的有机溶剂。
为了进一步改善性能，涂料组合物可以包含优选以水溶液或分散体形式添加的附加的聚合物。在最终涂料组合物中这些聚合物的含量低于50重量％，优选低于30重量％。适宜的聚合物为例如聚酯、丙烯酸酯、甲基丙烯酸酯、聚乙烯基吡咯烷酮或烷氧基硅烷的缩合产物。
任选地，该涂料可以包含防粘连剂。常规防粘连剂是无机和/或有机粒子，例如二氧化硅、碳酸钙、氧化铝、硅酸铝、高岭土或交联聚苯乙烯或丙烯酸酯粒子。优选诸如无定形二氧化硅的多孔二氧化硅。
涂料制剂可以进一步包含进一步的添加剂，例如表面活性剂、抗静电剂、抗氧化剂和/或泡沫调节剂。
涂料组合物因此优选仅由水和聚氨酯以及交联剂组分组成。“组成”在这里的意思是前述物质构成所述组合物的程度为至少50重量％，优选至少65重量％，以及更优选至少75重量％。
在涂布工艺后，涂层由所述涂料组合物的干残余物(干产物)组成，其随后同等优选仅由聚氨酯和交联剂组分，和任选的防粘连剂、进一步的聚合物和/或添加剂的干产物组成。
在一个特别优异的实施方案中，本发明干涂层仅由聚氨酯和包含噁唑啉基的聚合物的反应产物组成。涂层可以施加到聚酯膜的一边或两边。然而，仅向膜的一边提供本发明的涂层而在另一边施加另一涂层也是可能的。
为了在线涂布取向的聚酯膜，可以采用本发明涂料制剂。“在线”意思是在纵向和/或横向拉伸前在膜制备工艺期间施加所述涂层。
为了改善膜与该涂料水分散体的润湿性，涂布前任选可以对膜进行电晕处理。
可以采用一般的适当工艺施加所述涂层，例如用缝隙式流延机或喷射工艺。特别优选通过“逆向凹版辊涂布”工艺施用涂层，其中涂层可以非常均匀地施加。类似优选的是通过Meyer棒工艺的施加，采用它可以以简单的方式获得较大的涂层厚度。
在最终膜上的干涂层厚度为5-500纳米，优选10-250纳米。
涂料组分可以相互和/或与膜表面的聚酯反应，和/或在聚酯膜的干燥和拉伸时特别是随后的最高可达250℃的热处理过程中扩散进聚酯膜表面结构中。
甚至在相对高温和存在湿气时所述涂层(特别是在双轴取向聚酯膜上时)提供对EVA的非常好的持久粘合性能。
非常令人惊奇的是，所述由至少一种聚氨酯和交联剂组成的本发明涂层甚至在相对高温和存在湿气时在长时期内对标准固化和快速固化的EVA类型都具有优异的粘合性能。而且，更加令人惊奇的是，特别是那些通过毫微压痕法测定的硬度特别高的涂层类似地在相对高温和存在湿气时显示出对EVA特别好的粘合性能维持性。
本发明白色不透明基膜的说明
涂层要施用于其上的聚酯膜可以具有一层结构、由基层(B)和面层(A)组成的两层结构、或由基层(B)和两个面层(A’和C)组成的三层结构。在聚酯膜多层结构的情况下，面层(们)(A，A’和C)的厚度在0.1-10微米，优选0.2-5微米的范围。根据膜总厚度和施加的面层的厚度的差异相对应地计算基础膜层的厚度。
聚酯膜的总厚度典型地在5-750微米，优选10-500微米的范围。
本发明的膜包含作为主要成分的热塑性聚酯。这种聚酯详述于“热塑性聚酯手册，Ed.S.Fakirov，Wiley-VCH，2002”。实例为乙二醇和对苯二甲酸的聚酯(聚对苯二甲酸乙二醇酯，PET)、乙二醇和萘-2，6-二羧酸的聚酯(聚2，6-萘二甲酸乙二醇酯，PEN)和1，4-双(羟甲基)-环己烷和对苯二甲酸的聚酯(聚对苯二甲酸1，4-环己烷二亚甲基酯，PCDT)。根据本发明，聚酯应理解为指均聚聚酯、共聚聚酯、不同聚酯的混合物、研磨物和聚酯的其它变体。
为了获得前述的性能，特别是膜的低透明性和期望的白度，把适当的颜料结合入所述聚酯膜中。在多层结构的情况下，至少基础膜层，但是也有可能面层(A，A’和C)，可以用颜料改性。本文中，已经发现采用合适大小和合适含量的二氧化钛、碳酸钙、硫酸钡、硫化锌或氧化锌是令人满意的。颜料可以单独使用或者使用两种或多种前述颜料的组合。优选使用二氧化钛或硫酸钡，或否则的话二氧化钛和硫酸钡的混合物。
二氧化钛可以是金红石型或者锐钛矿型。二氧化钛的平均粒径在0.05和0.5微米之间，优选在0.1和0.3微米之间。碳酸钙的平均粒径在0.1和2.5微米之间，但是优选在0.2-2.0微米的平均粒径。硫酸钡 具有0.3-0.9微米，优选0.4-0.7微米的平均粒径。由于结合的颜料，膜获得明亮的白色外观。为了达到期望的白度(＞70)和期望的低透明性(＜40％)，膜(在至少基层和还有可能的面层的多层结构的情况下)必须具有高颜料填充水平。基于膜的总重量，获得期望的低透明性的粒子含量为≥3重量％但≤50重量％，优选≥4重量％但≤40重量％以及更优选≥5重量％但≤30重量％。
为了进一步增加白度，可以任选地向着色的膜(在多层结构中优选添加到着色层上)添加适当的光学增亮剂。适当的光学增亮剂为例如Hostalux
KS(来自德国的Clariant)或者EastobrightOB-1(来自美国的伊斯曼)。
本发明的膜可以进一步在一层或多层中包含作为防粘连剂的粒子。典型的防粘连剂是无机和/或有机粒子，例如二氧化硅(沉淀法或热解法)、碳酸钙、碳酸镁、碳酸钡、硫酸钙、磷酸锂、磷酸钙、磷酸镁、高岭土(水合的或煅烧的)、氧化铝、硅酸铝、氟化锂，所用二元羧酸的钙盐、钡盐、锌盐或锰盐，或交联的聚合物粒子，例如聚苯乙烯或聚甲基丙烯酸甲酯粒子。
此外，选择两种或多种粒子体系的混合物或者具有相同化学组成然而不同粒径的粒子体系的混合物作为防粘连剂也是可能的。
当粒子作为防粘连剂存在于膜的层中时，基于改性层的总重，这些粒子的总含量低于20重量％，优选低于15重量％以及更优选低于5重量％。粒子的平均粒径为0.01-15微米，优选0.03-10微米以及更优选0.05-5微米。
本发明的膜可以进一步包含添加剂，例如UV稳定剂、阻燃剂、水解稳定剂和抗氧化剂。
UV稳定剂(即作为光稳定剂的UV吸收剂)是能干预光诱导聚合物降解的物理和化学过程的化学物。适宜的UV稳定剂为例如2-羟基二苯酮类、2-羟基苯并三唑类、有机镍化合物、水杨酸酯类、苯乙烯酯衍生物类、间苯二酚单安息香酸酯类、草酰替苯胺类、羟基安息香酯类、苯并恶嗪酮类、空间位阻胺类和三嗪类，优选2-羟基苯并三 唑类、苯并恶嗪酮类和三嗪类。在一个特别优选的实施方案中，本发明的膜包含作为UV稳定剂的0.1-5.0重量％的分子式如下的2-(4，6-二苯基[1，3，5]三嗪-2-基)-5-己氧基苯酚
或者0.1-5.0重量％的分子式如下的2，2’-亚甲基双[6-苯并三唑-2-基]-4-(1，1，2，2-四甲基丙基)苯酚
或者0.1-5.0重量％的分子式如下的2，2’-(1，4-亚苯基)双([3，1]苯并恶嗪-4-酮)
在一个进一步的实施方案中，也可采用这些UV稳定剂的混合物或者这些UV稳定剂中的至少一种与其它的UV稳定剂的混合物，其中基于膜的重量光稳定剂的总含量优选在0.1和5.0重量％之间，更优选在0.5到3.0重量％范围。
在一个进一步的实施方案中，本发明的膜已被改性以使其是阻燃的。阻燃含义是在根据UL94VTM的火安全测试中，膜达到至少VTM-2级。
相应地，基于改性层的总重量，膜(在一或多层中)包含含量范围为0.2-30重量％，优选1.0-20重量％的阻燃剂。适宜的阻燃剂为例如有机磷化合物，如羧基次磷酸类、其酸酐类以及二甲基甲膦酸酯。本文中非常适宜的是其中磷化合物化学键合到聚酯上的阻燃剂，例如具有如下分子式的双(2-羟乙基)[(6-氧桥-6H-二苯[c，e][1，2]氧杂磷化-6-基)甲基]丁二羧酸酯
由于阻燃剂通常具有一定的水解敏感性，额外采用水解稳定剂可能是可取的。本文中适宜的水解稳定剂为例如聚合的碳二亚胺，例如来自Rheinchemie(德国)的Stabaxol
P。
用于获得膜的期望的白度和低透明性的颜料、防粘连剂和添加剂实际上在熔融前适当的添加到用于制备膜的聚酯中。在这种情况中，这种添加可以或者作为聚酯制备期间的乙醇酸分散体或者否则在膜制备工艺中挤出过程中经母炼胶而实现。
此外，在多层结构情况下的聚酯膜可以是可密封的或可剥离的。这通常通过在至少面层之一中采用低玻璃化转变温度的聚酯或其它可密封的聚合物来实现。
聚酯膜的制备工艺详述于例如“热塑性聚酯手册，Ed.S.Fakirov，Wiley-VCH，2002”中或者在“聚合物科学与工程百科全书，12卷，John Wiley & Sons，1988”的章节“聚酯，膜”中。在优选的制备膜的挤出工 艺中，熔融的聚合物材料通过缝隙式口模挤出，任选带有添加剂，以及在冷却辊上急冷作为实质上无定形的初级膜。该膜随后被再加热和在至少一个方向拉伸(“取向”)，可以在机器方向(MD)或者在横向(TD)，但是优选在纵向和横向。拉伸工艺中膜温度通常高于所用聚酯的玻璃化转变温度10-60℃，纵向拉伸的拉伸比典型地为2.0-6.0，特别是3.0-4.5，横向拉伸的拉伸比为2.0-5.0，特别是3.0-4.5，以及实施的任何第二纵向拉伸的拉伸比为1.1-5.0。
纵向拉伸也可以和横向拉伸同时进行(同时拉伸)或者以可想象的次序进行。这之后随后在180-260℃，特别是220-250℃的炉温下热固化膜。随后，膜被冷却和卷起。
为了当用作太阳能组件中的背面盖时在长时期后膜仍保持充足的机械稳定性，对于本发明基膜来说要在制备工艺后膜的SV为至少650，优选至少700，这是必须的。在其它方法中，可以通过选择适宜的具有充分高SV的聚酯原材料和有助于低SV降解的温和的工艺条件(例如挤出期间的低剪切应力)来影响膜的SV。
令人意想不到的是本发明涂层与本发明白色不透明基膜的结合得到了显著适用于作为太阳能组件的背面盖的聚酯膜(或者单独的或者与进一步的材料以层合体的形式结合)。
表1再次总结了涂布的聚酯膜的最重要的创造性特性。
所用测试方法的说明
用下面的测试方法表征涂布的白色聚酯膜：
涂层对EVA的粘合性
从涂布的聚酯膜中切掉300mm长和25mm宽的两个带。把50mm长和25mm宽的EVA膜带(厚度0.5mm)放置在所述两个聚酯膜带之间使得涂布的边每个都朝着EVA。随后通过热密封设备(TP-701-B，Sangyo有限公司，日本)层压聚酯膜和EVA。取决于所用EVA的类型，采用下述的密封条件。
| EVA类型 | 生产商 | 温度[℃] | 压力[MPa] | 时间[分钟] |
| 485.00(标准固化) | Etimex，德国 | 150 | 0.13 | 20 |
| 486.00(快速固化) | Etimex，德国 | 150 | 0.13 | 15 |
为了确定EVA粘合性，首先从25mm宽聚酯膜/EVA层合体切掉30cm长和15mm宽的带。把这些15mm宽的聚酯膜带的未层压到一起的端部夹到拉力测试机(EZ Graph
，Shimadzu，日本)中。随后，测试在180°的角度和100毫米/分钟的速度下分离所述聚酯膜/EVA层合体所需要的力。
涂层的热和潮湿稳定性
为了确定PET/EVA/PET层合体在升高的温度和湿度下的长期稳定性，如上所述制备25mm宽的测试样本，并基于标准IEC61215，在85℃，85％的相对湿度下在控制气候的橱(Hiflex
FX210C，来自Kusumoto化学，Etac分部，日本)中保存1000小时。
随后，如上所述，从层合体切掉15mm宽的带并测定平均分离力。在控制气候的橱中处理前后的平均分离力的比值R设定为：
＞50％的R值显示了涂层优异的热和潮湿稳定性。
对于太阳能组件的适应性测试
用异丙醇清洁尺寸25×25cm的玻璃板(Krystal Klear，厚度3毫米，来自AFG，美国)。然后，把同样尺寸的EVA膜和待测的PET膜(涂布的边对着EVA)放置到所述玻璃板上。首先把所述复合物引入温度为150℃可抽真空的加热橱中并把压力降到100毫巴(大约2分钟)。在另外5分钟后，取出复合物，然后在热压机(10t，来自Gonno，日本)中层压。取决于所用EVA，为了该目的采用了下面的条件：
| EVA类型 | 生产商 | 温度[℃] | 压力[MPa] | 时间[分钟] |
| 485.00(标准固化) | Etimex，德国 | 150 | 0.5 | 20 |
| 486.00(快速固化) | Etimex，德国 | 150 | 0.5 | 15 |
根据标准ISO4892采用Weather-O-Meter(C165，来自Atlas材料测试技术公司，美国)以下面的条件测试玻璃/EVA/PET层合体的气候稳定性：
气候时间：20000小时
强度：340纳米下0.35W/cm2(带有硼硅酸盐过滤器的氙灯辐射仪)
测试周期：102分钟干相，18分钟带有去离子水的喷射相
黑板温度：63℃
在这个过程中，聚酯膜在所述层合体背离氙灯的那一边。在气候老化结束后用视觉评估层合体的分层。
涂层硬度
通过毫微压痕技术测定涂层硬度。这种方法能使待测的涂层硬度与基底无关。采用“Berkovich”尖端与原子力显微镜(SPM-9500J2，来自Shimadzu，日本)连接的“TS70 TriboScope
”毫微压痕设备(来自Hysitron，美国)。测试在室温和50％的相对空气湿度下进行。所述尖端的穿透深度设定为10nm。
膜粘连性
两个15×14cm的在一边涂布的膜样本在40℃/80％的相对空气湿度下在控制气候的橱中保存2小时。随后，把所述样本的一个放在另一个的顶部(涂布边对着未涂布边)，用10千克重物(相当于48g/cm2)在上述条件下在控制气候的橱中相互挤压样本20小时。使用拉伸测试机(Autograph AG-1，Shimadzu，日本)用拉紧的0.1毫米粗的钢线以500毫米/分钟的速度牵拉所述样本，这样使其相互分离。以克表示的所需平均力由力-距离图表所测定。该值越低，涂布膜的膜粘连行为越好(值＜50克是优异的)。
涂层质量
用视觉评估涂层质量。
黄度指数
根据ASTM-D 1925-70通过来自Perkin Elmer(美国)的“Lamda 12”分光光度计确定涂布膜的黄度指数，标准光源D65，10°标准观测者。由测定的正常色值X，Y，Z根据公式
YID＝[100·(1.28·X-1.06·Z)]/Y
计算黄度指数。
透明性
根据ASTM-D1033-77测定透明性。
白度
按照Berger用来自蔡司公司(德国)的ELREPHO
电子反射比光度计测定白度，标准光源C，2°标准观测者。白度被定义为W＝RY+3RZ-3RX
SV(标准粘度)
基于DIN53726，在25℃下在二氯乙酸中测定标准粘度SV(DCA)。根据标准粘度计算特性粘度(IV)如下：
IV＝[η]＝6.907·10-4 SV(DCE)+0.063096[dl/g]
收缩性
根据DIN40634在150℃和15分钟的阻抗时间下测定收缩性。
粗糙度
根据DIN4762(切掉0.25mm)确定算术平均粗糙度值Ra。
光泽度
根据DIN67530测定光泽度。反射镜值被测定为膜表面的光学参数。基于标准ASTM-D 523-78和ISO 2813，入射角设置为20°。光束以设定的入射角击中平的测试表面并通过它反射或散射。把入射到光电接收器的光线显示为成比例的电参数。该测量是无量纲的并且必须用入射角来报告。
下文中参照实施例详细说明本发明。表2列出了所用的涂层材料， 表3给出了实施例和比较例的总的看法。采用下面的聚对苯二甲酸乙二醇酯原料用于制备膜。
·M80(Invista，德国)，具有810的SV和18重量％硫酸钡(Blanc fixe
XR-HX，Sachtleben Chemie，德国)
·M67(Invista，德国)，具有810的SV和7重量％二氧化钛(Hombitan
LW-S-U，锐钛矿同质异像体，Sachtleben Chemie，德国)
涂布膜样本的表征结果总结于表4、5和6中。
实施例1
采用聚酯原材料M80制备熔体，通过缝隙式口模把熔体挤出到保持在大约20℃的压延辊上，在此固化成无定形初级膜。在初级膜保持在95℃的温度过程中以3.6∶1的拉伸比纵向拉伸它。随后通过Meyer棒用固含量5重量％的涂料水分散体以4.7微米的厚度涂布所述纵向拉伸的膜，基于干涂层该分散体包含50重量％的Neorez
R-600和50重量％的Epocros
WS-700。在100℃的温度干燥该纵向拉伸和涂布的膜，然后以4.3∶1的拉伸比横向拉伸它，这样获得双轴取向的膜。在230℃热固化所述双轴拉伸的膜。最终膜厚为250微米。根据涂料制剂的固含量、涂层厚度(湿)和横向拉伸因子为55纳米计算干涂层的厚度。
通过上述的方法表征涂布的膜。甚至在潮湿和热的影响下，其特征为低透明性、高白度、高光泽度、对EVA很好的粘合。膜与EVA和玻璃的层合体经受20000小时的人工气候老化而没有分层。
实施例2
除了采用聚酯原材料M67的熔体制备膜以外，重复实施例1。涂布该膜，然后类似于实施例1表征它。其同样的甚至在潮湿和热的影响下，表现出低透明性、高白度、高光泽度、对EVA很好的粘合的特征。膜与EVA和玻璃的层合体经受20000小时的人工气候老化而没有分层。
实施例3
除了采用70重量％的M67和30重量％的M80的熔体制备膜以外，重复实施例1。涂布该膜，然后类似于实施例1表征它。其同样的甚至在潮湿和热的影响下，表现出低透明性、高白度、高光泽度、对EVA很好的粘合的特征。膜与EVA和玻璃的层合体同样经受20000小时的人工气候老化而没有分层。
实施例4
实施例1制备的膜在280℃熔融。把该熔体成形为线股，在水中淬火并处理成小球。把这些小球以50重量％的含量添加到用来制备基膜的聚酯中。涂布该膜，然后类似于实施例1表征它。涂布的膜具有类似于实施例1的性能。尽管采用了再研磨物，然而相对于实施例1该膜的黄度指数并没有显著增加。
实施例6-17
类似实施例1，如所述的用5重量％的组成列于表3中的涂料分散体制备并涂布聚酯膜。随后，通过上述方法表征该涂布膜。它们同样的甚至在潮湿和热的影响下，表现出低透明性、高白度、高光泽度、对EVA很好的粘合的特征。膜与EVA和玻璃的层合体经受20000小时的人工气候老化而没有分层。
比较例1
类似实施例1，制备聚酯膜，但是没有涂层。通过上述方法表征该未涂布的膜。在85℃和85％的相对空气湿度下1000小时后，EVA粘合性不充分，并且在20000小时的人工气候老化后膜与EVA和玻璃的层合体显示出分层。
比较例2
类似实施例2，制备聚酯膜，但是没有涂层。通过上述方法表征该未涂布的膜。在85℃和85％的相对空气湿度下1000小时后，EVA粘合性不充分，并且在20000小时的人工气候老化后膜与EVA和玻璃的层合体显示出分层。
比较例3
比较例1制备的膜在280℃熔融。把该熔体成形为线股，在水中 淬火并处理成小球。把这些小球以50重量％的含量添加到用来制备基膜的聚酯中。通过上述方法表征该未涂布的膜。在85℃和85％的相对空气湿度下1000小时后，EVA粘合性不充分，并且在20000小时的人工气候老化后膜与EVA和玻璃的层合体显示出分层。
比较例4-7
类似实施例1，如所述的用5重量％的组成列于表3中的涂料分散体制备并涂布聚酯膜。随后，通过上述方法表征该涂布膜。在85℃和85％的相对空气湿度下1000小时后，EVA粘合性不充分，并且在20000小时的人工气候老化后膜与EVA和玻璃的层合体显示出分层。
表1：涂布膜最重要的发明特性的总结
表2：所用涂层材料的总结
表3：实施例和比较例的总结
*％基于干涂层的重量
表3：实施例和比较例的总结(续)
*％基于干涂层的重量
表4：实施例和比较例的涂层表征和EVA粘合性
表4：实施例和比较例的EVA粘合性结果(续)
表5：实施例和比较例的表征结果
表5：实施例和比较例的表征结果(续)
表6：实施例和比较例用于太阳能组件的适应性测试结果
Claims (14)
1.白色涂布的聚酯膜中的涂层用于在太阳能组件中改进对EVA粘合性的用途，该涂层在该聚酯膜的至少一个表面上，所述涂层包含至少一种聚氨酯和至少一种交联剂，该聚氨酯由脂肪族聚氧化烯多元醇或脂肪族聚碳酸酯多元醇与多异氰酸酯反应制备；
该涂布的聚酯膜具有下面所列性能中至少一种：
-＜40％的透明性，
-＞70％的伯杰白度，
-在20°的测量角下测量的涂布侧的光泽度＞5，
-在150℃在15分钟内在机器方向和横向的收缩低于2.5％，
-涂布侧对于EVA粘合性，用在180°的角度分离由该涂布的聚酯膜和EVA组成的层合体所需的力表示，涂布侧对着EVA，该力＞50N/15mm，
-所述涂层对升高的温度和湿度的长期稳定性，用在85℃/85％的相对空气湿度下存储1000小时后，分离由该涂布的聚酯膜和EVA组成的层合体所需的力表示，涂布侧对着EVA，该力仍旧至少为初始值的50％。
2.权利要求1的用途，该涂布的聚酯膜具有下面所列性能中至少一种：
-＜35％的透明性，
-＞75％的伯杰白度，
-在20°的测量角下测量的涂布侧的光泽度＞10，
-在150℃在15分钟内在机器方向和横向的收缩低于2.0％，
-涂布侧对于EVA粘合性，用在180°的角度分离由该涂布的聚酯膜和EVA组成的层合体所需的力表示，涂布侧对着EVA，该力＞70N/15mm，
-涂层的耐机械性，通过纳米压痕法测定，其＞0.2GPa，
-由该涂布的聚酯膜、EVA和玻璃组成的层合体按照ISO4892在 氙灯气候老化仪中经受加速气候老化20000小时而没有分层，涂布侧对着EVA，
-膜中聚酯的SV值大于700，
-在涂布的表面上膜的平均粗糙度Ra＞20nm，
-低于80的黄度指数。
3.权利要求2的用途，其中该涂布的聚酯膜的性能为：
-＜30％的透明性，
-＞80％的伯杰白度，
-在20°的测量角下测量的涂布侧的光泽度＞20，
-在150℃在15分钟内在机器方向和横向的收缩低于1.5％，
-涂层的耐机械性，通过纳米压痕法测定其＞0.25GPa，
-膜中聚酯的SV值大于650，
-在涂布的表面上膜的平均粗糙度Ra＞25nm，
-低于70的黄度指数。
4.权利要求3的用途，其中该涂布的聚酯膜的性能为：
-涂层的耐机械性，通过纳米压痕法测定，其＞0.3GPa，
-在涂布的表面上膜的平均粗糙度Ra＞30nm。
5.权利要求1的用途，其中交联剂是水可混溶的或水分散性组分，其带有能进入交联反应的反应性基团。
6.权利要求5的用途，其中交联剂是带有下述基团中至少一种的聚合物：噁唑啉基、碳二亚胺基、环氧基、异氰酸酯基或蜜胺基。
7.权利要求6的用途，其中交联剂是带有噁唑啉或碳二亚胺基团的聚合物。
8.权利要求7的用途，其中所述包含噁唑啉基团的聚合物是通过下述物质的加成聚合形成的大分子化合物：
a)至少一种根据结构式(I)和(II)之一的噁唑啉衍生物与
b)至少一种进一步的共聚单体，
其中结构式(I)到(II)中的R1、R2、R3和R4基分别独立表示氢原子、卤原子、烷基、芳烷基、苯基或取代的苯基，以及R5是带有可聚合双键的非环基。
9.权利要求8的用途，其中共聚单体b)选自下述化合物的一种或多种：甲基丙烯酸酯类、不饱和羧酸类、不饱和腈类、不饱和酰胺类、乙烯基酯类、乙烯基醚类、α-烯烃类、卤代α，β-不饱和化合物以及α，β-不饱和芳族化合物。
10.权利要求1的用途，其中所述涂层另外包含一种或多种选自下述构成的组的聚合物：聚酯类、丙烯酸酯类、甲基丙烯酸酯类、聚乙烯基吡咯烷酮和烷氧基硅烷类的缩合产物。
11.权利要求1的用途，其中所述涂层另外包含一种或多种选自下述构成的组的添加剂：防粘连剂、表面活性剂、抗静电剂、抗氧化剂和泡沫调节剂。
12.权利要求1的用途，其中在所述涂布的聚酯膜上的干涂层具有5—500纳米的厚度。
13.权利要求12的用途，其中在所述涂布的聚酯膜上的干涂层具有10—250纳米的厚度。
14.权利要求1的用途，用于太阳能组件的背面盖或者用于太阳能组件的背面盖的层合体中。
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2009
- 2009-02-20 DE DE200910009791 patent/DE102009009791A1/de not_active Withdrawn
- 2009-04-02 US US12/384,294 patent/US9206295B2/en not_active Expired - Fee Related
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2010
- 2010-02-15 KR KR1020117021720A patent/KR20110118170A/ko active Search and Examination
- 2010-02-15 JP JP2011550461A patent/JP5686745B2/ja not_active Expired - Fee Related
- 2010-02-15 CN CN201080008685.4A patent/CN102325831B/zh not_active Expired - Fee Related
- 2010-02-15 PL PL10708902T patent/PL2398849T3/pl unknown
- 2010-02-15 EP EP10708902.1A patent/EP2398849B1/en active Active
- 2010-02-15 WO PCT/EP2010/000912 patent/WO2010094443A1/en active Application Filing
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| US6348267B1 (en) * | 1998-11-10 | 2002-02-19 | Sharp Kabuhsiki Kaisha | Coated film |
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| Title |
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| JP特開2008-4691A 2008.01.10 |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2012518691A (ja) | 2012-08-16 |
| DE102009009791A1 (de) | 2010-08-26 |
| KR20110118170A (ko) | 2011-10-28 |
| WO2010094443A1 (en) | 2010-08-26 |
| US20100215902A1 (en) | 2010-08-26 |
| EP2398849A1 (en) | 2011-12-28 |
| EP2398849B1 (en) | 2017-11-08 |
| JP5686745B2 (ja) | 2015-03-18 |
| CN102325831A (zh) | 2012-01-18 |
| US9206295B2 (en) | 2015-12-08 |
| PL2398849T3 (pl) | 2019-01-31 |
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