CN101115617B - 导电层合薄膜 - Google Patents
导电层合薄膜 Download PDFInfo
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- CN101115617B CN101115617B CN2006800041486A CN200680004148A CN101115617B CN 101115617 B CN101115617 B CN 101115617B CN 2006800041486 A CN2006800041486 A CN 2006800041486A CN 200680004148 A CN200680004148 A CN 200680004148A CN 101115617 B CN101115617 B CN 101115617B
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- electrically conducting
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Abstract
本发明公开了一种导电薄膜,其是在基材薄膜的至少一面上将锚固层及透明导电涂膜层按此顺序进行层合而得到的,所述锚固层含有聚酯树脂和具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂作为构成成分,该导电薄膜的总透光率为60%以上且表面电阻值为1×101~1×104Ω/□。该导电薄膜具有优异的透明性和导电性,而且由于基材与透明导电涂膜层的贴合好,因此即使在施加外力时也可以保持充分的导电性能,可适合用作液晶显示器(LCD)、透明触控式面板、有机电致发光元件、无机电致发光灯等的透明电极或电磁波屏蔽材料。
Description
技术领域
本发明涉及一种导电薄膜。更详细而言,涉及透明性和导电性及其耐久性均优异,可适合用作液晶显示器(LCD)、透明触控式面板、有机电致发光元件、无机电致发光灯等的透明电极或电磁波屏蔽材料的透明导电薄膜。
背景技术
以往,透明导电薄膜适合用作液晶显示器、透明触控式面板等的透明电极或电磁波屏蔽材料。众所周知,所述透明导电薄膜是通过真空蒸镀法、溅射法、离子喷镀法等干法将氧化铟(In2O3)、氧化锡(SnO2)、In2O3与SnO2的混合烧结物(ITO)等设置在聚对苯二甲酸乙二醇酯(PET)、三乙酰纤维素(TAC)等的透明薄膜表面的至少一面上而得到的薄膜。
但是,通常当将透明导电薄膜用作透明电极或电磁波屏蔽材料时,在成网状下对其进行连续加工或冲孔加工,在表面加工中也以弯曲状态进行使用以及保管。因此,上述通过干法得到的透明导电薄膜在该工艺过程或保管期间有时会产生裂纹,表面电阻增大。
当将ITO等金属氧化物用作透明导电性材料时,例如由于ITO的折射率高达1.8左右,因此表面反射率增高,得不到充分的透过率。因此有人提出了下面的方法,即在ITO层和基材薄膜之间设置二氧化硅等低折射层,并根据需要进一步组合设置氧化钛等高折射层,从而显示出防反射的效果,得到透过率高的导电薄膜(参照日本特开2000-207128号公报)。
另一方面,通过在透明基材薄膜上涂布导电性高分子(湿法)而形成的透明导电涂膜层,其膜本身具有柔软性,不易产生裂纹等问题。通过涂布导电性高分子而得到透明导电薄膜的方法与干法不同,制造成本较低,而且涂布速度也普遍较快,因此还具有生产率优异的优点。通过涂布导电性高分子而得到的透明导电薄膜,迄今为止一般使用的是聚噻吩、聚苯胺、聚吡咯等,在开发的初期阶段因得不到高导电性而使其在防静电用途等中的使用受到限制,导电涂膜层本身的色调也成了问题。但是最近通过改进制造方法等上述问题也得到了改善。例如,在聚阴离子存在下将3,4-二烷氧基噻吩氧化聚合而得到的包括聚(3,4-二烷氧基噻吩)和聚阴离子的导电性高分子(参照日本特开平1-313521号公报),近年来通过制造方法的改进(参照日本特开2002-193972号公报和日本特开2003-286336号公报)等保持着高的光线透过率并显示出非常低的表面电阻。
但是,当将上述使用导电性高分子作为透明导电涂膜层的导电薄膜用于各种用途时,存在着因施加外力而引起的透明导电涂膜层和基材薄膜之间发生剥离,从而导致性能下降的问题。将使用导电性高分子的导电薄膜用于积极施加外力的用途的代表例可列举出触控式面板,虽然已在日本特开2002-109998号公报中提出,但并未触及上述问题点。
并且,由于上述使用导电性高分子作为透明导电涂膜层的导电薄膜的透明导电涂膜层的折射率低至1.5左右,因此难以将折射率低于该值的层设置在导电涂膜层和基材薄膜之间来改善防反射的性能并进一步提高光线透过率。另外在通过与折射率高的物质组合来体现防反射的效果时,也没有发现生产率高的方法。实际情况是还无人提出表面反射性得到充分抑制、实用性也优异的导电薄膜。
发明内容
本发明鉴于上述背景技术而进行,其目的在于提供具有优异的透明性和导电性,而且基材和透明导电涂膜层的贴合好,即使在施加外力时也可以充分地保持导电性能的导电薄膜。
本发明的另一目的在于提供表面反射得到抑制、显示出优异的透明性的导电薄膜。
本发明的其它目的和优点从下面的说明中可以明确。
根据本发明,本发明的上述目的和优点可以通过一种导电层合薄膜来实现,该导电层合薄膜包括基材薄膜、中间层及位于上述中间层上的透明导电涂膜层,所述中间层由含有聚酯树脂和具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂而形成的树脂组合物形成、且位于上述基材薄膜的一面上或两面上,
该导电层合薄膜的特征在于:
透明导电涂膜层是含有由下式(1)表示的重复单元形成的聚噻吩的聚阳离子和聚阴离子形成的导电性高分子而形成的,
其中,R1和R2相互独立表示氢原子或碳原子数为1~4的烷基,或者相互结合表示可以被取代的碳原子数为1~12的亚烷基,
透明导电涂膜层的厚度为0.01~0.30μm的范围,
中间层的折射率为1.53~1.63且厚度为0.01~0.10μm,
总透光率为60%以上且表面电阻值为1×101~1×104Ω/□,
其中,上述形成中间层的聚酯树脂在中间层中的含有比例为5~95%重量,
上述形成中间层的具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂在中间层中的含有比例为5~90%重量,并且
在上述中间层中,以使脂肪族蜡的含量为30%重量以下和微粒的含量为20%重量以下的比例含有脂肪族蜡和微粒。
附图简述
图1是本发明的导电层合薄膜的一个例子的截面说明图。
发明的实施方式
首先用附图来说明本发明的导电层合薄膜。图1是本发明的导电层合薄膜的截面说明图。图1表示层构成的一个例子。图1中,1表示基材薄膜,2表示中间层,3表示透明导电涂膜层,而4表示硬质涂层。由图1可知,本发明的导电层合薄膜是在基材薄膜的至少一面上层合中间层,在该中间层之上再层合透明导电涂膜层而得到的薄膜。只要是具有上述构成的薄膜,就可以在不损害本发明目的的限度内形成例如硬质涂层等其它功能层。图1(b)表示在与形成有透明导电涂膜层的面相反一侧上设置了中间层和硬质涂层的例子。
这样,本发明的导电层合薄膜可以如下形成,在基材薄膜的至少一面上将含有聚酯树脂和具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂作为构成成分的中间层以及透明导电涂膜层按此顺序进行层合。例如若中间层仅位于基材薄膜的相反面上,则无法体现基于中间层对透明导电涂膜层的贴合效果,因此不优选。
并且,具有上述层合结构的本发明的导电层合薄膜的总透光率必需在60%以上。若总透光率不足60%,则将层合薄膜用作液晶显示器、透明触控式面板等的透明电极或电磁波屏蔽材料时,难以得到充分的透明性。总透光率优选65%以上,特别优选为70%以上。上述总透光率可以通过选定后述的基材薄膜、透明导电涂膜层来适当调整。
本发明的导电层合薄膜的透明导电涂膜层的表面电阻在1×101~1×104Ω/□的范围。若该表面电阻超过上限,则在用作液晶显示器、透明触控式面板等的透明电极或电磁波屏蔽材料时,作为电极不能充分地发挥功能,得不到充分的电磁波屏蔽特性。另一方面,若低于下限,则制造工序容易变得不稳定,因此不优选。优选的表面电阻为1×101~5×103Ω/□的范围,特别优选的表面电阻为1×101~1×103Ω/□的范围。
下面,对形成本发明的导电层合薄膜的各层进一步详述。
对本发明中的透明导电涂膜层没有特别限定,只要是表面电阻降低而且还具备透明性的涂膜层即可。
透明导电涂膜层含有包括由下式(1)表示的重复单元形成的聚噻吩的聚阳离子(下面有时称作“聚(3,4-二取代噻吩)”)和聚阴离子的导电性高分子。即,该导电性高分子优选为聚(3,4-二取代噻吩)与聚阴离子的复合化合物。
其中,R1和R2相互独立表示氢原子或碳原子数为1~4的烷基,或者相互结合表示可被取代的碳原子数为1~12的亚烷基。
构成该导电性高分子的聚(3,4-二取代噻吩)的R1和R2相互独立,表示氢原子或碳原子数为1~4的烷基,或者一起表示可被任意取代的碳原子数为1~12的亚烷基。R1和R2一起形成的可具有取代基的碳原子数为1~12的亚烷基的代表例可以列举出:1,2-亚烷基,如1,2-亚环己基和2,3-亚丁基等。R1和R2一起形成的碳原子数为1~12的亚烷基的优选例子可以列举出:亚甲基、1,2-亚乙基和1,3-亚丙基。其中特别优选1,2-亚乙基。具体例子可以列举出:可被烷基取代的亚甲基;可被碳原子数为1~12的烷基或苯基取代的1,2-亚乙基、1,3-亚丙基。
另一方面,构成导电性高分子的聚阴离子可以列举如:高分子状羧酸,如聚丙烯酸、聚甲基丙烯酸、聚马来酸等;和高分子状磺酸,如聚苯乙烯磺酸、聚乙烯基磺酸等。上述高分子状羧酸或磺酸可以是乙烯基羧酸或乙烯基磺酸与其它可聚合的低分子化合物例如丙烯酸酯类、苯乙烯等的共聚物。上述聚阴离子中,优选使用聚苯乙烯磺酸和其全部或一部分为金属盐的聚阴离子。
用于形成透明导电涂膜层的涂料组合物使用将上述导电性高分子作为主要成分分散在水中的分散液,但根据需要可以添加聚酯、聚丙烯酸酯类、聚氨酯、聚乙酸乙烯酯、聚乙烯醇缩丁醛等适当的有机高分子材料作为粘合剂。
并且,根据需要可以在涂料组合物中添加与水具有相容性的适当的溶剂,用于使粘合剂溶解或改善对基材薄膜的湿润性或调整固体成分的浓度。例如优选使用:醇类,如甲醇、乙醇、丙醇、异丙醇等;酰胺类,如甲酰胺、N,N-二甲基甲酰胺、乙酰胺、N-甲基乙酰胺、N,N-二甲基乙酰胺、N-甲基丙酰胺等。
另外,为了提高所得透明导电涂膜层的涂膜强度,在涂料组合物中还可以进一步添加烷氧基硅烷或酰氧基硅烷。上述硅烷化合物以水解、并进一步发生缩合反应的反应产物的形式存在于透明导电涂膜层中。上述硅烷化合物例如可以列举出:甲基三乙酰氧基硅烷、二甲基二乙酰氧基硅烷、三甲基乙酰氧基硅烷、四乙酰氧基硅烷、 四甲氧基硅烷、四乙氧基硅烷、四异丙氧基硅烷、四异丁氧基硅烷、甲基三乙氧基硅烷、二甲基二乙氧基硅烷、三甲基乙氧基硅烷、苯基三乙氧基硅烷等或γ-缩水甘油氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷等具有除烷氧基以外的反应性官能团的三烷氧基硅烷。其中优选:四甲氧基硅烷、四乙氧基硅烷、四异丙氧基硅烷、四异丁氧基硅烷等四烷氧基硅烷和γ-缩水甘油氧基丙基三甲氧基硅烷、乙烯基三乙氧基硅烷等具有除烷氧基以外的反应性官能团的三烷氧基硅烷,特别优选具有缩水甘油氧基的三烷氧基硅烷。所述硅烷化合物的添加量以导电性高分子的重量为基准,优选为50%重量以下、特别优选为10~40%重量的范围。
优选并用催化剂以使上述硅烷化合物的水解/缩合高效率地进行。催化剂可以使用酸性催化剂也可以使用碱性催化剂。作为酸性催化剂,优选例如硫酸、盐酸、硝酸等无机酸,乙酸、枸橼酸、丙酸、草酸、对甲苯磺酸等有机酸。而作为碱性催化剂,优选例如氨、三乙胺、三丙胺等有机胺化合物,甲醇钠、甲醇钾、乙醇钾、氢氧化钠、氢氧化钾等碱金属化合物等。
并且,在上述用于形成透明导电涂膜层的涂料组合物中还可以添加少量表面活性剂,用于提高对基材薄膜的湿润性。优选的表面活性剂例如可以列举:非离子性表面活性剂,如聚氧乙烯烷基苯基醚、聚氧乙烯烷基醚、脱水山梨糖醇脂肪酸酯等;和氟系表面活性剂,如含氟烷基羧酸盐、全氟烷基苯磺酸盐、全氟烷基季铵盐、全氟烷基聚氧乙烯乙醇等。
形成透明导电涂膜层时的涂布方法可以采用自身公知的方法。例如可以优选:lip direct法、comma涂布机法、狭缝逆涂法、模头涂布机法、凹版辊式涂布机法、刮刀涂布机法、喷涂机法、气刀涂布法、浸涂法、刮棒涂布机法等。当并用热固性树脂作为粘合剂时,透明导电涂膜层的涂设通过在基材薄膜上涂布含有形成各透明导电涂膜层的成分的涂布液,进行加热干燥来形成涂膜。加热条件优选 为在80~160℃下加热10~120秒钟,特别优选为在100~150℃下加热20~60秒钟。当并用紫外线(UV)固化性树脂或电子射线(EB)固化性树脂作为粘合剂时,通常在进行预干燥后进行紫外线照射或电子射线照射。
另外,在后述的中间层上涂布用于形成该透明导电涂膜层的涂布液时,根据需要可以在该中间层表面施行电晕放电处理、等离子体放电处理等物理性表面处理,作为用于进一步提高贴合性、涂布性的预处理。
透明导电涂膜层的厚度优选为0.01~0.30μm的范围,特别优选为0.02~0.25μm的范围。若该涂膜的厚度太薄,则有时得不到充分的导电性;反之若太厚,则有时总透光率不足,发生阻隔。
本发明中,为了提高上述透明导电涂膜层与基材薄膜的贴合性,在它们之间必需设置中间层,即用于将透明导电涂膜层固定在基材薄膜上的中间层。该中间层的厚度优选为0.01~0.3μm,更优选为0.02~0.25μm的范围。若其厚度太薄,则贴合力下降;反之若太厚,则有可能发生阻隔、雾度值增高。并且,从防反射效果方面考虑,优选该中间层的折射率为1.53~1.63、优选为1.55~1.62的范围;其厚度为0.01~0.10μm、优选为0.02~0.10μm的范围。当该折射率在上述范围以外时,通过与透明导电涂膜层组合,由光学干涉产生的防反射效果容易变得不充分;当该厚度在上述范围以外时,难以显现出光学干涉的效果。该中间层含有聚酯树脂和具有噁唑啉基和聚环氧乙烷链的丙烯酸酯类树脂两者作为构成成分。
这里对使用的聚酯树脂没有特别限定,可以列举由以下所示的多元酸和多元醇形成的聚酯。特别优选在水或含有一些有机溶剂的水中具有可溶性或分散性的聚酯。
聚酯树脂的多元酸成分可以列举如:对苯二甲酸、间苯二甲酸、邻苯二甲酸、邻苯二甲酸酐、2,6-萘二甲酸、1,4-环己烷二甲酸、己二酸、癸二酸、偏苯三酸、苯均四酸、二聚酸、5-钠磺基间苯二甲酸 等。其中,优选含有2种以上上述酸成分的共聚聚酯。应说明的是,可以含有少量的马来酸、衣康酸等不饱和多元酸成分或如对羟基苯甲酸等羟基羧酸成分。
另一方面,多元醇成分可以列举如:乙二醇、1,4-丁二醇、二甘醇、双丙甘醇、1,6-己二醇、1,4-环己烷二甲醇、苯二甲醇、二羟甲基丙烷等或聚(环氧乙烷)二醇、聚(环氧丁烷)二醇。
另一方面,中间层中使用的具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂优选在水或含有一些有机溶剂的水中具有可溶性或分散性的丙烯酸酯类树脂。所述具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂可以列举如含有下面所示的单体作为共聚成分的丙烯酸酯类树脂。
首先,具有噁唑啉基的单体可以列举如: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、2-异丙烯基-5-甲基-2-噁唑啉等,可以使用它们中的一种或多种的混合物。其中2-异丙烯基-2-噁唑啉在工业上容易获取,优选。通过使用所述具有噁唑啉基的丙烯酸酯类树脂,中间层的凝聚力提高,与透明导电涂膜层的贴合性变得更牢固。并且可以使基材薄膜表面在薄膜制膜工序内或透明导电涂膜层加工工序中具有对金属轧辊的耐擦伤性能。应说明的是,含有噁唑啉基的单体的含量,作为该丙烯酸酯类树脂中的含量优选为2~40%重量,更优选为3~35%重量,进一步优选为5~30%重量。
具有聚环氧烷链的单体可以列举如:使聚环氧烷加成在丙烯酸、甲基丙烯酸的羧基上而得到的酯。聚环氧烷链可以列举如:聚环氧甲烷、聚环氧乙烷、聚环氧丙烷、聚环氧丁烷等。聚环氧烷链的重复单元优选为3~100。通过使用所述具有聚环氧烷链的丙烯酸酯类树脂,与使用不含有聚环氧烷链的丙烯酸酯类树脂相比,中间层中的聚酯树脂与丙烯酸酯类树脂的相容性变好,可以提高中间层的透明性。其中,若聚环氧烷链的重复单元小于3,则聚酯树脂与丙烯酸树 脂的相容性降低,中间层的透明性容易变差;反之若大于100,则中间层的耐湿热性下降,在高湿度、高温下与透明导电涂膜层的贴合性容易下降。应说明的是,具有聚环氧烷链的单体的含量,作为该丙烯酸树脂中的含量优选为3~40%重量,更优选为4~35%重量,进一步优选为5~30%重量。
丙烯酸酯类树脂的其它共聚成分可以列举如下面的单体。即丙烯酸烷基酯、甲基丙烯酸烷基酯(烷基例如甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、2-乙基己基、环己基);丙烯酸-2-羟乙基酯、甲基丙烯酸-2-羟乙基酯、丙烯酸-2-羟丙基酯、甲基丙烯酸-2-羟丙基酯等含羟基的单体;丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、烯丙基缩水甘油醚等含环氧基的单体;丙烯酸、甲基丙烯酸、衣康酸、马来酸、富马酸、丁烯酸、苯乙烯磺酸及其盐(钠盐、钾盐、铵盐、叔胺盐等)等具有羧基、磺酸基或其盐的单体;丙烯酰胺、甲基丙烯酰胺、N-烷基丙烯酰胺、N-烷基甲基丙烯酰胺、N,N-二烷基丙烯酰胺、N,N-二烷基甲基丙烯酰胺(烷基例如甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、2-乙基己基、环己基)、丙烯酰吗啉、N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、N-苯基丙烯酰胺、N-苯基甲基丙烯酰胺等具有酰胺基的单体;马来酸酐、衣康酸酐等酸酐的单体;乙烯基异氰酸酯、烯丙基异氰酸酯、苯乙烯、乙烯基甲基醚、乙烯基乙基醚、乙烯基三烷氧基硅烷、烷基马来酸单酯、烷基富马酸单酯、烷基衣康酸单酯、丙烯腈、甲基丙烯腈、偏氯乙烯、乙烯、丙烯、氯乙烯、乙酸乙烯、丁二烯等。
形成中间层的聚酯树脂在中间层中的含有比例优选为5~95%重量,特别优选为50~90%重量。形成中间层的具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂在中间层中的含有比例优选为5~90%重量,特别优选为10~50%重量。若聚酯树脂超过95%重量或具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂不足5%重量,则中间层的凝聚力下降,透明导电涂膜层的贴合性有时变得不充分。另外,当聚酯树脂不足5% 重量或具有噁唑啉基和聚环氧烷基的丙烯酸酯类树脂超过90%重量时,透明导电涂膜层的贴合性有时变得不充分。
本发明中,优选上述中间层中含有0.5~30%重量的脂肪族蜡,特别优选含有1~10%重量。若该比例少于0.5%重量,则有时不能断定薄膜表面的润滑性提高效果。另一方面若超过30%重量,则有时对基材薄膜的贴合或将透明导电涂膜层固定在基材上的性能不足。
作为优选使用的脂肪族蜡,具体可以列举出:巴西棕榈蜡、小烛树蜡、米糠蜡、木蜡、霍霍巴油、棕榈蜡、松香改性蜡、オウリキユリ-蜡、甘蔗蜡、西班牙草蜡、树皮蜡等植物蜡;蜂蜡、羊毛脂、鲸蜡、虫胶蜡等动物蜡;褐煤蜡、地蜡、纯地蜡等矿物蜡;石蜡、微晶蜡、矿脂等石油蜡;费-托蜡、聚乙烯蜡、聚丙烯蜡等合成烃蜡等。其中从透明导电涂膜层和润滑性良好的角度考虑,优选巴西棕榈蜡、石蜡、聚乙烯蜡。从环境问题和容易处理的角度考虑,上述蜡类特别优选使用水分散的蜡类。
并且,优选在上述中间层中含有0.1~20%重量的平均粒径在0.005~0.5μm范围的微粒。若中间层中的微粒含量不足0.1%重量,则有时薄膜的润滑性下降,难以卷取成卷筒状;反之若超过20%重量,有时中间层的透明性下降,不能用于显示器/触控式面板等用途。作为优选使用的微粒,可以列举如:碳酸钙、碳酸镁、氧化钙、氧化锌、氧化镁、二氧化硅、硅酸钠、氢氧化铝、氧化铁、氧化锆、硫酸钡、氧化钛、氧化锡、氧化锑、炭黑、二硫化钼等无机微粒;由二氧化硅和氧化钛形成的复合无机微粒;丙烯酸酯类交联聚合物、苯乙烯类交联聚合物、硅树脂、氟树脂、苯并胍胺树脂、酚醛树脂、尼龙树脂、聚乙烯蜡等有机微粒。其中,优选由二氧化硅和氧化钛形成的复合无机微粒。并且,从防反射效果和雾度的角度考虑,形成中间层的高分子粘合剂与微粒的折射率差优选为0.02以下,若折射率差变大超过该值,则所得导电薄膜的透明性有时会下降。
为了在基材薄膜上形成上述中间层(下面有时称作“涂膜”),优 选将上述成分以水溶液、水分散液或乳液等水性涂布液的形式使用。为了形成涂膜,根据需要还可以添加除了上述成分以外的其它成分,例如防静电剂、着色剂、表面活性剂、紫外线吸收剂等。特别是通过添加润滑剂可以使耐粘连性更好。
中间层的涂布中所用水性涂布液的固体成分浓度优选为20%重量以下,更优选为1~10%重量。若该比例不足1%重量,则对基材薄膜的湿润性有时会不足;另一方面,若超过20%重量,则涂布液的贮藏稳定性或中间层的外观有时会恶化。
对本发明中的基材薄膜没有特别限定,但优选含有下述成分的薄膜:(甲基)丙烯酸酯类树脂、聚苯乙烯、聚乙酸乙烯、聚乙烯或聚丙烯等聚烯烃、聚氯乙烯、聚偏氯乙烯、聚酰亚胺、聚酰胺、聚砜、聚碳酸酯、聚对苯二甲酸乙二醇酯(下面有时称作PET)、聚萘二甲酸乙二醇酯(下面有时称作PEN)等聚酯(可以是将少量例如以总酸成分为基准20%摩尔以下、优选10%摩尔以下的第3成分共聚的聚酯)或用氨基、环氧基、羟基、羰基等官能团进行部分改性的树脂、三乙酰纤维素(TAC)等。上述基材薄膜中,从机械特性或透明性、生产成本方面考虑,特别优选含有聚酯尤其是PET、PEN和它们的共聚物的薄膜。对基材薄膜的厚度没有特别限定,优选500μm以下。若比500μm厚,则刚性太强,将所得薄膜贴在显示器等上时操作性容易降低。
当使用聚酯薄膜作为基材薄膜时,用于设置中间层的上述水性涂料的涂布可以在任意阶段实施,但优选在聚酯薄膜的制造过程中实施,更优选在取向结晶结束前的聚酯薄膜上涂布。
这里取向结晶结束前的聚酯薄膜包括:未拉伸薄膜、使未拉伸薄膜在纵向或横向中任一方向上取向的单轴取向薄膜、进一步在纵向和横向这两个方向上低倍率拉伸取向的薄膜(最终在纵向和/或横向再拉伸,结束取向结晶前的双轴拉伸薄膜)等。
其中优选在未拉伸薄膜或单向取向的单轴拉伸薄膜上涂布用于形成中间层的水性涂布液,并直接施行纵拉伸和/或横拉伸及热固定。
在基材薄膜上涂布用于形成中间层的水性涂布液时,作为用于提高涂布性的预处理,优选在薄膜表面施行电晕处理、火焰处理、等离子体处理等物理处理,或者将其和组合物一起与化学惰性表面活性剂并用。
所述表面活性剂是促进形成上述中间层的水性涂布液对基材薄膜的湿润性的物质,可以列举如:聚氧乙烯烷基苯基醚、聚氧乙烯-脂肪酸酯、脱水山梨糖醇脂肪族酯、甘油脂肪酸酯、脂肪酸金属皂、烷基硫酸盐、烷基磺酸盐、烷基磺基琥珀酸盐等阴离子型、非离子型表面活性剂。表面活性剂在形成涂膜的组合物中优选含有0.1~10%重量。
形成中间层时的涂布方法可以采用自身公知的方法。可列举如:lip direct法、comma涂布机法、狭缝逆涂法、模头涂布机法、凹版辊式涂布机法、刮刀涂布机法、喷涂机法、气刀涂布法、浸涂法、刮棒涂布机法等,可以单独或组合使用上述方法。应说明的是,涂膜根据需要可以仅在薄膜的一面形成,也可以在两面形成。
如上所述,本发明的导电薄膜需要在基材薄膜的至少一面上将中间层和透明导电涂膜层按此顺序进行层合,但根据需要还可以在与形成有透明导电涂膜层一侧相反的面上设置中间层、硬质涂层等涂膜。
从透明性的角度考虑,本发明的导电薄膜优选在波长550nm处的表面反射率为3%以下,雾度值不足1.5%。
实施例
下面,列举实施例更具体地说明本发明。应说明的是,实施例中的各项评价按下述方法进行。
(1)反射率、膜厚和涂膜的折射率
关于反射率,使用反射分光膜厚计(大冢电子制,商品名“FE-3000”)测定试样导电薄膜的透明导电涂膜层侧在波长300~800nm处 的反射率。
另一方面,中间层和透明导电涂膜层的膜厚和折射率如下求出,即,作为具代表性的折射率的波长分散近似式,引用了n-k Cauchy的分散式,使上述反射率测定值与光谱的实测值拟合。
硬质涂层的厚度通过冲点式计算膜厚来测定,使用任选3点的平均值。
<反射率>
550nm处的反射率为3%以下 …表面反射足够低
550nm处的反射率高于3% …表面反射高
(2)微粒的折射率
将在90℃下干燥的微粒悬浮在折射率不同的各种25℃的液体中,使用阿贝折射率计(D线589nm)测定悬浮液中最透明的液体的折射率。
(3)玻璃化转变温度
将约10mg样品封入测定用的铝盘中,将此盘装在差示量热计(杜邦公司制V4.OB2000型DSC)上,以20℃/分钟的速度从25℃升温至300℃,在300℃下保持5分钟后取出,立即移至冰上骤冷。将此盘再次装在差示量热计上,以20℃/分钟的速度从25℃升温至300℃,测定玻璃化转变温度(Tg:℃)。
(4)特性粘度
特性粘度(〔η〕dl/g)用25℃的邻氯苯酚溶液进行测定。
(5)雾度值
按照JIS K7150,用スガ试验机(株)制的雾度仪HCM-2B进行测定,按下述标准进行评价。
雾度<1.5% …浊度足够低
雾度≥1.5% …浊度高
(6)总透光率
按照JIS K7150,用スガ试验机(株)制的雾度仪HCM-2B进行测 定,按下述标准进行评价。
总透光率≥60% …透明性良好
总透光率<60% …透明性不好
(7)贴合性
按照实施例和比较例中记载的方法,在形成有中间层的基材薄膜的中间层形成面上形成透明导电涂膜层,实施棋盘状的横切试验(横切出100个1mm2的网格),在其上贴附宽24mm的玻璃纸胶粘带(ニチバン公司制),以180°的剥离角度急剧剥离后观察剥离面,按下面的基准进行评价。
5:剥离面积不足10% …粘合力极好
4:剥离面积10%以上、不足20% …粘合力良好
3:剥离面积20%以上、不足30% …粘合力略好
2:剥离面积30%以上、不足40% …粘合力不好
1:剥离面积40%以上 …粘合力极其不好
(8)笔输入擦动耐久性
作为对导电薄膜施加外力时导电性劣化程度的标准,制作模拟触控式面板,进行笔输入擦动耐久试验。在笔输入擦动耐久试验中,切出100mm×100mm大小的试样导电薄膜,在透明导电涂膜层形成面的两端涂布银糊,作成宽5mm的电极。通过恒压电源向该电极间施加5V电压,测定样品中心部分50mm×50mm范围内纵横1mm间隔的(x1,y1)~(x50,y50)这2,500点的电压Vi,j(i,j=1~50)。以Δi,j=(Vi,j-Ui,j)/Ui,j定义各电压测定点处的与理论电压Ui,j=V1,1+(V50,50-V1,1)/50×(j-1)的偏差,将该Δi,j的绝对值的最大值定义为线性。
使用测定了笔输入试验前的线性的薄膜,如实施例和比较例中记载的那样进行操作,制作触控式面板。从由导电薄膜构成的面板一侧开始,在使用由聚缩醛树脂制成的笔尖半径为0.8mm的触摸笔进行线性测定的部位,通过绘图仪来进行边长为2cm大小的片假名 ア~ン的文字记录,进行笔输入试验。此时笔载荷250gf,文字记录速度为2,000字/小时。从记录完毕的触控式面板上取下导电薄膜,按与上述相同的方法测定笔输入试验后的导电薄膜的线性。针对各记录文字数进行此项评价,将线性超过3%时的文字数作为耐笔输入文字数,按下述基准进行评价。
10万字<耐笔输入文字数 …对外力的耐性极好
5万字≤耐笔输入文字数≤10万字 …对外力的耐性良好
耐笔输入文字数<5万字 …对外力的耐性不好
(9)表面电阻
使用三菱化学公司制Lorester MCP-T600,根据JIS K7194进行测定。对任意位置进行5次测定,取其平均值。
实施例1
<基材薄膜和中间层的形成>
将熔融聚对苯二甲酸乙二醇酯(〔η=0.62dl/g,Tg=78℃)从模头挤出,按照常规方法用冷却鼓冷却,作成未拉伸薄膜,接着纵向拉伸3.4倍,然后用辊式涂布机在其两面均匀涂布表1所示涂布液1的浓度为8%的水性涂布液。接着在涂布后将该薄膜在125℃下横向拉伸3.6倍,在220℃下使其宽度方向收缩3%进行热固定,形成了中间层,得到厚度为188μm的基材薄膜。应说明的是,涂膜的厚度为0.15μm。
表1
聚酯1:酸成分由65%摩尔2,6-萘二甲酸/30%摩尔间苯二甲酸/5%摩尔5-钠磺基间苯二甲酸构成;二醇成分由90%摩尔乙二醇/10%摩尔二甘醇构成。Tg=80℃。平均分子量13,000。
聚酯1根据日本特开平6-116487号公报的实施例1中记载的方法如下制造。即,将44份2,6-萘二甲酸二甲酯、16份间苯二甲酸二甲酯、4份5-钠磺基间苯二甲酸二甲酯、34份乙二醇和2份二甘醇装入反应器中,向其中添加0.05份四丁氧基钛,在氮气氛下将温度控制在230℃进行加热,使生成的甲醇馏去,进行酯交换反应。接着将反应体系的温度缓慢升至255℃,使体系内处于1mmHg的减压来进行缩聚反应,得到聚酯1。
聚酯2:酸成分由60%摩尔对苯二甲酸/35%摩尔间苯二甲酸/5%摩尔5-钠磺基间苯二甲酸构成;二醇成分由90%摩尔乙二醇/10%摩尔二甘醇构成。Tg=45℃。平均分子量14,000。
聚酯2根据日本特开平6-116487号公报的实施例1中记载的方法如下制造。即,将36份对苯二甲酸二甲酯、21份间苯二甲酸二甲酯、5份5-钠磺基间苯二甲酸二甲酯、36份乙二醇和2份二甘醇装入反应器中,向其中添加0.05份四丁氧基钛,在氮气氛下将温度控制在230℃进行加热,使生成的甲醇馏去,进行酯交换反应。接着,将反应体系的温度缓慢升至255℃,使体系内处于1mmHg的减压来进行聚合反应,得到聚酯2。
丙烯酸酯1:由30%摩尔甲基丙烯酸甲酯/30%摩尔2-异丙烯基-2-噁唑啉/10%摩尔聚环氧乙烷(n=10)甲基丙烯酸酯/30%摩尔丙烯酰胺构成。Tg=50℃。
丙烯酸酯1根据日本特开昭63-37167号公报的制造例1~3中记载的方法如下制造。即,向四颈烧瓶中装入3份作为表面活性剂的十二烷基磺酸钠和181份离子交换水,在氮气流中升温至60℃,接着添加0.5份过硫酸铵、0.2份亚硝酸氢钠作为聚合引发剂,再一边将液温调整至60~70℃,一边用3小时滴加作为单体的23.3份甲基 丙烯酸甲酯、22.6份2-异丙烯基-2-噁唑啉、40.7份聚环氧乙烷(n=10)甲基丙烯酸酯和13.3份丙烯酰胺的混合物。滴加完毕后仍保持相同温度范围2小时,同时在搅拌下继续反应,接下来进行冷却,得到固体成分为35%的丙烯酸酯1的水分散体。
丙烯酸酯2:由30%摩尔甲基丙烯酸甲酯/40%摩尔2-异丙烯基-2-噁唑啉/30%摩尔丙烯酰胺构成。Tg=80℃。
丙烯酸酯2根据日本特开昭63-37167号公报的制造例1~3中记载的方法如下制造。即,向四颈烧瓶中装入3份作为表面活性剂的十二烷基磺酸钠和181份离子交换水,在氮气流中升温至60℃,接着添加0.5份过硫酸铵和0.2份亚硝酸氢钠作为聚合引发剂,再一边将液温调整至60~70℃,一边用3小时滴加作为单体的34.9份甲基丙烯酸甲酯、45.2份2-异丙烯基-2-噁唑啉和19.9份丙烯酰胺的混合物。滴加完毕后仍保持相同温度范围2小时,同时在搅拌下继续反应,接下来进行冷却,得到固体成分为35%的丙烯酸酯2的水分散体。
丙烯酸酯3:由45%摩尔甲基丙烯酸甲酯/45%摩尔丙烯酸丁酯/5%摩尔甲基丙烯酸缩水甘油酯/5%摩尔甲基丙烯酸-2-羟乙基酯构成。Tg=50℃。
丙烯酸酯3根据日本特开昭63-37167号公报的制造例1~3中记载的方法如下制造。即,向四颈烧瓶中装入3份作为表面活性剂的十二烷基磺酸钠和181份离子交换水,在氮气流中升温至60℃,接着添加0.5份过硫酸铵和0.2份亚硝酸氢钠作为聚合引发剂,再一边将液温调整至60~70℃,一边用3小时滴加作为单体的38.7份甲基丙烯酸甲酯、49.6份丙烯酸丁酯、6.1份甲基丙烯酸缩水甘油酯和5.6份甲基丙烯酸-2-羟乙基酯的混合物。滴加完毕后仍保持相同温度范围2小时,同时在搅拌下继续反应,接下来进行冷却,得到固体成分为35%的丙烯酸酯3的水分散体。
添加剂1:二氧化硅填料(平均粒径100nm)(日产化学株式会社 制:商品名スノ-テツクスZL)
添加剂2:巴西棕榈蜡(中京油脂株式会社制,商品名セロゾ-ル524)
湿润剂:聚氧乙烯(n=7)十二烷基醚(三洋化成株式会社制,商品名ナロアクテイ-N-70)
<透明导电涂膜层的形成>
导电性聚合物:将99.6份含有0.5%重量聚(3,4-亚乙基二氧基噻吩)和0.8%重量聚苯乙烯磺酸(分子量Mn=150,000)的聚合物的水分散体(Baytron P:バイエルAG制)与0.4份硅烷化合物γ-缩水甘油氧基丙基三甲氧基硅烷(TSL-8350:东芝シリコ-ン制)混合后,搅拌1小时得到涂布液,使用迈耶绕线棒涂布器将所得涂布液涂布在上述设置了中间层的基材薄膜上,在140℃下干燥1分钟,得到透明导电涂膜层。透明导电涂膜层的厚度为0.15μm。
<硬质涂层的形成>
进行笔输入擦动耐久试验时,使用迈耶绕线棒涂布器在上述导电薄膜的与透明导电涂膜层相反的面上涂布丙烯酸酯类硬质涂层涂料(荒川化学工业株式会社制,商品名ビ-ムセツト700),用于消除由薄膜本身产生不可逆的凹陷而造成的影响,进行60℃×30秒钟的预干燥后,以1,000mJ的能量照射UV,得到硬质涂层。硬质涂层的膜厚为8μm。得到的导电层合薄膜的特性如表2所示。
实施例2
除了将形成中间层的水性涂布液的成分作为涂布液2、透明导电涂膜层的厚度为0.18μm以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
实施例3
除了将形成中间层的水性涂布液的成分作为涂布液3以外,重 复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
实施例4
除了将形成中间层的水性涂布液的成分作为涂布液4以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
实施例5
将作为形成基材薄膜的材料的熔融聚2,6-萘二甲酸乙二醇酯(〔η〕=0.65dl/g,Tg=121℃)从模头挤出,按照常规方法用冷却鼓冷却,作成未拉伸薄膜,接着纵向拉伸3.4倍,然后用辊式涂布机在其两面均匀涂布表1所示涂布液1的浓度为8%的水性涂布液。接着在涂布后将该薄膜在125℃下横向拉伸3.6倍,在220℃下使其宽度方向收缩3%进行热固定,形成了中间层,得到厚度188μm的基材薄膜。应说明的是,涂膜的厚度为0.15μm。透明导电涂膜层与实施例1同样地形成。所得导电薄膜的特性如表2所示。
比较例1
除了没有形成中间层以外,重复与实施例1相同的操作。所得导电薄膜的特性如表2所示。
比较例2
除了将形成中间层的水性涂布液的成分作为涂布液5以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
比较例3
除了将形成中间层的水性涂布液的成分作为涂布液6以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
比较例4
除了使透明导电涂膜层的厚度达到0.005μm以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
比较例5
除了使透明导电涂膜层的厚度达到0.9μm以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
实施例6
除了使透明导电涂膜层的厚度达到0.07μm以外,重复与实施例1相同的操作。所得导电层合薄膜的特性如表2所示。
表2
涂剂 | 透明导电涂 膜层厚度 (μm) | 表面电阻 (Ω/□) | 总光线 透过率 (%) | 贴合 性 | 笔输入擦动耐久性 (耐记录次数) | |
实施例1 | 涂布液1 | 0.15 | 2500 | 87 | 5 | 20万次 |
实施例2 | 涂布液2 | 0.18 | 1500 | 83 | 5 | 15万次 |
实施例3 | 涂布液3 | 0.15 | 2500 | 87 | 5 | 15万次 |
实施例4 | 涂布液4 | 0.15 | 2500 | 87 | 5 | 14万次 |
实施例5 | 涂布液1 | 0.15 | 2500 | 87 | 5 | 18万次 |
比较例1 | - | 0.15 | 2500 | 87 | 2 | 1万次 |
比较例2 | 涂布液5 | 0.15 | 2500 | 87 | 2 | 3万次 |
比较例3 | 涂布液6 | 0.15 | 2500 | 87 | 2 | 3万次 |
比较例4 | 涂布液1 | 0.005 | 53000 | 89 | 5 | 17万次 |
比较例5 | 涂布液1 | 0.9 | 450 | 55 | 5 | 16万次 |
实施例6 | 涂布液1 | 0.07 | 6000 | 88 | 5 | 16万次 |
实施例7~8和比较例6
<基材薄膜和锚固层的形成>
将熔融聚对苯二甲酸乙二醇酯(〔η〕=0.63dl/g,Tg=79℃)从模头挤出,按照常规方法用冷却鼓冷却,作成未拉伸薄膜,接着纵向拉伸3.4倍,然后通过辊式涂布机在其两面均匀涂布表3所示的水性 涂布液。接着在涂布后将该薄膜在125℃下横向拉伸3.6倍,在220℃下使其宽度方向收缩3%进行热固定,形成了中间层,得到厚度为188μm的基材薄膜。应说明的是,涂膜厚度通过调整各涂布液的浓度使其如表4所示。
表3
聚酯1、聚酯2、丙烯酸酯1、添加剂2和湿润剂与表1相同。
微粒1:二氧化硅和氧化钛的复合无机微粒(平均粒径100nm)。微粒1根据日本特开平7-2520号公报的制造例和实施例中记载的方法如下制造。即,向带有搅拌桨的容积为4升的玻璃制反应容器中装入140g甲醇、260g异丙醇和100g氨水(25%重量),调整反应液,将反应液的温度保持在40℃同时进行搅拌。接着向3升的三角烧瓶中装入550g四甲氧基硅(Si(OMe)4,コルコ-ト株式会社制,商品名:メチルシリケ-ト39),边搅拌边加入195g甲醇和28g 0.1%重量盐酸水溶液(将和光纯药工业株式会社制的35%盐酸用水稀释至1/1000),搅拌约10分钟。随后加入将300g四异丙氧基钛(Ti(O-iPr)4,日本曹达株式会社制,商品名:A-1(TPT))用634g异丙醇稀释的溶液,得到透明的均匀溶液(四烷氧基硅与四烷氧基钛的共缩合物)。用2小时将1699g上述均匀溶液和480g氨水(25%重量)分别滴加到上述反应液中,最初滴加速度慢,一直到最后阶段逐渐加快速度。滴加完毕后过滤所得共水解物,在50℃下干燥有机溶剂,然后将其分散在水中,得到浓度为10%重量、折射率为1.57的微粒1。
微粒2:丙烯酸酯类填料(平均粒径:100nm,折射率1.50)(日本ペイント株式会社制,商品名マイクロジエルE1002)。
微粒3:丙烯酸酯类填料(平均粒径:30nm,折射率1.50)(日本ペイント株式会社制,商品名マイクロジエルE2002)。
<透明导电涂膜层的形成>
导电性聚合物:使用迈耶绕线棒涂布器,将含有0.5%重量聚(3,4-亚乙基二氧基噻吩)和0.8%重量聚苯乙烯磺酸(分子量Mn=150,000)的聚合物的水分散体(Baytron P:バイエルAG制)涂布在上述设有中间层的基材薄膜上,在140℃下干燥1分钟,得到透明导电涂膜层。透明导电涂膜层的厚度为0.15μm。表面电阻为1,200Ω/□。
<硬质涂层的形成>
进行笔输入擦动耐久试验时,使用迈耶绕线棒涂布器在上述导电薄膜的与透明导电涂膜层相反面上涂布丙烯酸酯类硬质涂层涂料(荒川化学工业株式会社制,商品名ビ-ムセツト700),用于消除由膜本身产生不可逆的凹陷而造成的影响,进行60℃×30秒钟的预干燥后,以1,000mJ的能量照射UV得到硬质涂层。硬质涂层的膜厚为8μm。所得导电薄膜的特性如表4所示。
由表2可知:本发明的导电层合薄膜的透明导电涂膜层的贴合性好,即使在反复施加外力时也可以保持充分的导电性。
由表4可知:本发明的导电薄膜的表面反射率低,可作为实用性高的导电薄膜获得。
本发明的导电层合薄膜在维持优异的透明性、导电性的同时,由于透明导电涂膜层的贴合性好,即使在反复施加外力时也可以保持充分的导电性,可适合用作透明触控式面板、液晶显示器(LCD)、有机电致发光元件、无机电致发光元件等的透明电极或电磁波屏蔽材料。
Claims (9)
1.一种导电层合薄膜,其包括基材薄膜、中间层及位于上述中间层上的透明导电涂膜层,所述中间层由含有聚酯树脂和具有噁唑啉基和聚环氧烷链的丙烯酸树脂而形成的树脂组合物形成、且位于上述基材薄膜的一面上或两面上,
该导电层合薄膜的特征在于:
透明导电涂膜层是含有由下式(1)表示的重复单元形成的聚噻吩的聚阳离子和聚阴离子形成的导电性高分子而形成的,
其中,R1和R2相互独立表示氢原子或碳原子数为1~4的烷基,或者相互结合表示可以被取代的碳原子数为1~12的亚烷基,
透明导电涂膜层的厚度为0.01~0.30μm的范围,
中间层的折射率为1.53~1.63且厚度为0.01~0.10μm,
总透光率为60%以上且表面电阻值为1×101~1×104Ω/□,
其中,上述形成中间层的聚酯树脂在中间层中的含有比例为5~95%重量,
上述形成中间层的具有噁唑啉基和聚环氧烷链的丙烯酸酯类树脂在中间层中的含有比例为5~90%重量,并且
在上述中间层中,以使脂肪族蜡的含量为30%重量以下和微粒的含量为20%重量以下的比例含有脂肪族蜡和微粒。
2.权利要求1的导电层合薄膜,其中透明导电涂膜层是含有由上式(1)表示的重复单元形成的聚噻吩的聚阳离子和聚阴离子形成的导电性高分子和至少一种选自四烷氧基硅烷和具有烷氧基以外的反应性官能团的三烷氧基硅烷的硅烷化合物的反应产物而形成的。
3.权利要求2的导电层合薄膜,其中具有除烷氧基以外的反应性官能团的三烷氧基硅烷为具有缩水甘油氧基的三烷氧基硅烷。
4.权利要求1的导电层合薄膜,其中基材薄膜是由聚对苯二甲酸乙二醇酯或聚2,6-萘二甲酸乙二醇酯形成的。
5.权利要求1的导电层合薄膜,其中中间层的树脂组合物还含有微粒,并且该微粒的折射率与构成该树脂组合物的树脂的折射率之差为0.02以下。
6.权利要求5的导电层合薄膜,其中微粒含有二氧化硅与氧化钛的复合氧化物。
7.权利要求1的导电层合薄膜,其中中间层是在基材薄膜的制膜时同时形成的。
8.权利要求1的导电层合薄膜,其中波长550nm处的表面反射率为3%以下。
9.权利要求1的导电层合薄膜,其中雾度值为不足1.5%。
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DE60126353T2 (de) * | 2001-08-07 | 2007-10-18 | Teijin Dupont Films Japan Ltd. | Biaxial orientierte schichtförmige polyesterfolie und folie mit harter überzugsschicht |
JP2003292655A (ja) | 2002-04-04 | 2003-10-15 | Teijin Dupont Films Japan Ltd | 帯電防止性積層ポリエステルフィルム |
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2006
- 2006-01-30 JP JP2007501654A patent/JP4852526B2/ja active Active
- 2006-01-30 KR KR1020077018001A patent/KR101297443B1/ko active IP Right Grant
- 2006-01-30 US US11/795,565 patent/US7527853B2/en active Active
- 2006-01-30 WO PCT/JP2006/301909 patent/WO2006082944A1/ja active Application Filing
- 2006-01-30 EP EP20060713052 patent/EP1847386B1/en not_active Expired - Fee Related
- 2006-01-30 CN CN2006800041486A patent/CN101115617B/zh not_active Expired - Fee Related
- 2006-02-07 TW TW095104071A patent/TW200635768A/zh not_active IP Right Cessation
-
2008
- 2008-01-22 HK HK08100817A patent/HK1110548A1/xx not_active IP Right Cessation
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CN1175610A (zh) * | 1996-08-19 | 1998-03-11 | 拜尔公司 | 抗划伤导电涂料 |
JP2003286336A (ja) * | 2002-02-15 | 2003-10-10 | Bayer Ag | 透明の導電性層の製造方法、こうして得られる層並びにその使用 |
JP2003321561A (ja) * | 2002-03-01 | 2003-11-14 | Teijin Dupont Films Japan Ltd | 高透明易接着ポリエステルフィルム |
JP2003334912A (ja) * | 2002-03-13 | 2003-11-25 | Teijin Dupont Films Japan Ltd | 高透明易接着性ポリエステルフィルム |
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US20040265539A1 (en) * | 2002-06-04 | 2004-12-30 | Teijin Dupont Films Japan Limited | Laminated polyester film and laminated film |
Also Published As
Publication number | Publication date |
---|---|
WO2006082944A1 (ja) | 2006-08-10 |
JP4852526B2 (ja) | 2012-01-11 |
HK1110548A1 (en) | 2008-07-18 |
EP1847386B1 (en) | 2013-10-23 |
KR101297443B1 (ko) | 2013-08-30 |
CN101115617A (zh) | 2008-01-30 |
JPWO2006082944A1 (ja) | 2008-06-26 |
US20080138597A1 (en) | 2008-06-12 |
EP1847386A4 (en) | 2011-10-26 |
KR20070106710A (ko) | 2007-11-05 |
EP1847386A1 (en) | 2007-10-24 |
US7527853B2 (en) | 2009-05-05 |
TW200635768A (en) | 2006-10-16 |
TWI377130B (zh) | 2012-11-21 |
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