CN102123859B - 与腐蚀敏感层相容的粘合剂 - Google Patents

与腐蚀敏感层相容的粘合剂 Download PDF

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CN102123859B
CN102123859B CN200980131507.8A CN200980131507A CN102123859B CN 102123859 B CN102123859 B CN 102123859B CN 200980131507 A CN200980131507 A CN 200980131507A CN 102123859 B CN102123859 B CN 102123859B
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binding agent
base material
goods
sensitive layers
corrosion
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CN102123859A (zh
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艾伯特·I·埃费拉茨
夏剑辉
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3M Innovative Properties Co
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Abstract

本发明提供一种包括粘合剂的制品，所述粘合剂具有小于约5的酸值。所述粘合剂选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合。所述粘合剂与选自金属和金属合金的腐蚀敏感层接触。当将所述制品在约60℃和90％相对湿度下调理约21天时，腐蚀敏感层显示出偏离其初始电阻值20％或更小的变化。

Description

与腐蚀敏感层相容的粘合剂
背景技术
粘合剂在光学显示器中得到广泛的应用。这种应用包括(但不限于)在液晶显示器(LCD)的模块上粘结偏光器和在移动手持设备(MHH)的玻璃透镜上附接各种光学膜。偏光器可以与粘合剂直接或间接接触。
近来，在各种显示器应用中引入及结合触摸屏功能出现上升趋势。触摸屏通常包括腐蚀敏感层，如铟锡氧化物层、带涂层的聚对苯二甲酸乙二醇酯膜或带涂层的玻璃。通常用粘合剂将这些带涂层的基材附接于显示器模块。在一些触摸屏设计中，粘合剂接触腐蚀敏感层。在其他显示器应用中，粘合剂也可接触诸如蒸汽涂覆的镜面或电磁干扰屏蔽层之类的腐蚀敏感层。这些层也往往衍生自导电的金属和金属合金。
发明内容
本发明解决了对于与腐蚀敏感层(如金属或金属合金)相容的粘合剂的需求。也就是说，粘合剂与这种层接触时只是最小程度地改变其电阻。在本发明中使用如下的定义：
“变化”用来描述腐蚀敏感层表现出的电阻，通常是指在调理前后所述层的电阻的绝对值差；
“酸值”通常表示聚合物的酸含量，定义为中和一克聚合物中的酸所需的氢氧化钾的量(通常以毫克计)，一般按ASTM D974测定；
“加成固化有机硅”通常涉及通常在铂催化剂存在下进行的乙烯基封端的低聚物/聚合物(如乙烯基封端的聚二甲基硅氧烷(PDMS))与含氢化物的低聚物/聚合物(如含硅烷的PDMS)的反应；
“粘合剂”通常是指具有粘性和弹性组分的粘弹性材料，这样虽然粘合剂在压缩应力下显示出一定程度的回弹性，但它通常并不是像弹簧一样的材料，即，它不是弹性固体；
“腐蚀敏感层”通常是指在暴露于空气和水分的情况下易被氧化的层，且该层在被施加电压时能够传导电流；
“现场固化的粘合剂”通常是指能被传送到所需位置的液体系统，在该位置时，粘合剂组分或者几乎自发地相互反应，或者当暴露于能量源(如热或辐射)时相互反应；
“热活化粘合剂”通常是指在室温下利用手指压力的情况下，在干形式时基本上不呈现粘性的粘合剂，但在暴露于高温时粘合剂会发粘，良好地润湿基材表面，并且在冷却到室温后粘附于多种不同的表面上；
用于描述任何一般层或基材的“微结构”通常是指含有从所述层的主表面伸出的重复结构的层或基材，所述结构可为多种形式，包括(但不限于)峰和锥；
“光学透明的”通常是指按在下面实例部分中所述的方式对25微米厚的样品进行测量时，材料显示出约5％或更小的雾度；和
“压敏粘合剂”通常是指粘合剂在室温下在干形式下强力且永久地发粘，并牢固地粘附于多种不同的表面。
在一个方面，本发明涉及包含粘合剂的制品，所述粘合剂具有小于约5的酸值，并选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合，其与选自金属和金属合金的腐蚀敏感层接触，其中当将所述制品在约60℃和90％相对湿度下调理约21天时，腐蚀敏感层显示出偏离其初始电阻值20％或更小的变化。在一个实施例中，将粘合剂和腐蚀敏感层设置在基材的第一主表面上，使得腐蚀敏感层和任选粘合剂与基材的第一主表面接触。
优选地，本发明涉及一种包含粘合剂的制品，所述粘合剂是粘弹性的，具有小于约5的酸值，并选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合，其与选自金属和金属合金的腐蚀敏感层接触，其中当将所述制品在约60℃和90％相对湿度下调理约21天时，所述腐蚀敏感层显示出偏离其初始电阻值20％或更小的变化，其中所述粘合剂不是现场固化粘合剂。
在另一方面，本发明涉及制备制品的方法，该方法包括以下步骤：(i)提供基材，所述基材具有设置在其至少一部分上的腐蚀敏感层；(ii)提供条带，所述条带包括(a)具有相对的第一和第二主表面的背衬，(b)具有小于约5的酸值的粘合剂，并且其选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合；和(iii)将条带层合至基材，使得粘合剂接触腐蚀敏感层。本文中公开的腐蚀敏感层为基本上平的；即，它们不含微结构。在其他实施例中，背衬(如果使用条带的话)或基材为基本上平的。
优选地，本发明涉及一种制备制品的方法，该方法包括以下步骤：
提供基材，所述基材具有设置在其至少一部分上的腐蚀敏感层；
提供条带，所述条带包括(i)具有相对的第一和第二主表面的背衬，(ii)具有小于约5的酸值的粘合剂，并且其选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合，其中所述粘合剂是粘弹性的，并且所述粘合剂不是现场固化粘合剂；和
将所述条带层合至所述基材，使得所述粘合剂接触所述腐蚀敏感层。
在一个示例性应用中，可将本发明所述的制品及制品的制造方法结合到电子设备当中，所述电子设备例如(但不限于)液晶显示面板、电容式触摸屏、移动电话、手持装置和膝上型计算机。
由以下的具体实施方式和权利要求书可显而易见本发明的其他特征及优点。以上发明内容并非意图描述本公开的每个图示实施例或每种实施方式。以下的具体实施方式更具体地例示某些目前优选的利用本文中公开的原理的实施例。
附图说明
参考附图可以更好地对本发明进行描述，其中：
图1是根据本发明的示例性制品的俯视平面图；
图2是根据本发明的另一个示例性制品的截面图；
图3是制备根据本发明的制品的示例性方法的示意图；
图4A和4B是制备根据本发明的制品的另一个示例性方法的示意图；
图5是根据本发明的另一个示例性制品的截面图；和
图6显示在调理的各阶段期间，实例1至5和对照样品的电阻变化与时间的关系。
附图是理想化的，并非按比例绘制，并且只用于说明的目的。
具体实施方式
本文中的所有数值均假定由术语“约”来修饰。通过端点叙述的数值范围包括该范围内包含的所有数值(例如1至5包括1、1.5、2、2.75、3、3.80、4和5)。除另指出外，本文中叙述的所有份数均按重量计。
现在转向附图，图1显示可用在电子设备中的制品1的俯视平面图。该制品包括具有多根腐蚀敏感迹线5的基材4，所述腐蚀敏感迹线呈网格形式设置在基材的第一主表面上。连接片6与腐蚀敏感迹线的每个末端邻接。当电流施加于连接片时，它们与腐蚀敏感迹线电气连通。本文中公开的粘合剂通常会被施加于基材，使得它与腐蚀敏感层和基材的第一主表面直接接触。
图2示出具有多个交替的粘合剂层18与基材层14的示例性制品10的截面图，所述基材14具有设置在基材的第一表面14a上的腐蚀敏感层15。连接片16与基材的边缘邻接。连接片与腐蚀敏感层连通，使得当电流经过层15时，焊盘与腐蚀敏感层彼此电气连通。虽然只显示了基材与粘合剂的两组交替层，但使用更多数目的交替层或者使用一组基材与粘合剂均在本发明的范围内。
图3示出制备制品的示例性方法的示意图。该方法包括提供第一基材24的步骤，所述第一基材24具有设置在基材的第一表面24a上的不连续的腐蚀敏感层25。如图1所示，连接片26与基材邻接。条带卷20具有涂布在背衬21上的粘合剂28。任选地，背衬包括有助于该条带卷展开的防粘涂层。条带层合至第一基材24的第一表面24a，使得粘合剂28与腐蚀敏感层以及第一表面24a的暴露部分(即，不被腐蚀敏感层覆盖的部分)接触。在一个实施例中，背衬21用作第二基材并成为制品的一部分。在另一个实施例中，可以移除背衬并丢弃，并且可以将第二基材层合到粘合剂28的当前暴露的表面上。虽然图3示出的是使用条带卷，但所述方法也可使用条带切段来实施。
图4A和4B示出制备根据本发明的制品的另一个示例性方法的示意图。该方法包括提供由第一和第二基材44a和44b形成的腔43的步骤，所述第一和第二基材44a和44b可为基本上彼此共面的。腐蚀敏感层45设置在第一和第二基材中的至少一个上。电连接片46与两个基材中的一个邻接，并与腐蚀敏感层连通。为了进行示意性的说明，图中显示腐蚀敏感层设置在第二基材44b上。递送装置(如多腔注射器50)包括第一腔50a和第二腔50b，其中分别储存着粘合剂的组分。在使用时可以压下注射器中的柱塞，组分将在第三腔中混合，该第三腔装有搅拌器，且粘合剂组合物58可在其中进行混合。按这种方式，可以在稳定的条件下储存组分直至准备使用。在图4b中，粘合剂组合物58已经混入，从注射器中分送并充满腔。混合后，各组分可充分地具有反应性以使它们聚合并产生最终的粘合剂。任选地，可以使用能量源60(如来自烘箱或红外光源的热)来固化粘合剂组合物。这种具体方法具有的优点在于，粘合剂组合物在处于液态形式的时候可更好地适应第一与第二基材(基材是粗糙的)之间的不均匀厚度。本方法特别适合于第一与第二基材是玻璃或透明、基本上刚性的聚合物材料的情况。
图5显示多层制品30的截面图。该制品包括具有相对的第一和第二主表面(分别为34a和34b)的中间基材34。第一和第二表面的每个上敷设有腐蚀敏感的导电层35。虽然图5显示两个连续层35，但只有一个层35也在本发明的范围内，并且所述层可以是不连续的。任选地，电连接片(未显示)附接于基材，并且焊盘可以与层35连通。覆盖层35的是两个粘合剂层38。并且如果需要，可以用保护衬片39覆盖粘合剂层。
粘合剂
适合用于本发明的粘合剂包括性质为中性或碱性的粘合剂。换句话说，粘合剂优选不含或只含微量的酸官能团，使得粘合剂具有的酸值小于约5。在制品的寿命内，粘合剂中的酸含量对腐蚀敏感层的电性能没有明显的干扰。适合用于本发明的粘合剂可以是压敏粘合剂(PSA)、热活化粘合剂(HAA)或现场固化粘合剂(CIPA)。在一个实施例中，粘合剂是光学透明的。因此，粘合剂可以是以下中的一种：光学透明的PSA或非光学透明的PSA、光学透明的HAA或非光学透明的HAA或者光学透明的CIPA或非光学透明的CIPA。
示例性的粘合剂包括聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合。粘合剂具有的酸值小于约5，优选小于3，更优选小于1。本文中公开的聚合物通常衍生自用多官能异氰酸酯扩链(以制备聚氨酯、聚脲或它们的组合)或用多官能酯扩链(以制备聚酰胺、聚酯或它们的组合)的多元醇或多胺。聚酰胺还可以通过开环聚合的方式衍生自环酰胺(内酰胺)，但为了容易引入其他链段，扩链是优选的。聚酯也可衍生自多元醇和多官能酰基氯，前提是满足酸值小于约5的条件。脲、酰胺、酯或氨基甲酸酯基团通常提供聚合物的刚性、增强性链段。这些基团之间的强氢键作用提供内聚强度。在一些情况中，短链增长剂(通常是低分子量多胺或多元醇)可用于提供额外的硬链段。任选地，聚合物可用端固化基团或结构侧固化基团(如硅烷、丙烯酸酯、甲基丙烯酸酯、异氰酸酯残基、环氧化物等)封端。为促进粘合剂的热活化或为使它们内在发粘，衍生自具有较低模量和/或较低Tg的多元醇和多胺的软链段通常是优选的。这些多胺或多元醇的例子包括氨丙基官能化聚二甲基硅氧烷、羟丙基官能化聚二甲基硅氧烷、聚丁二烯二醇、聚乙烯丁二醇、聚醚二醇(如聚四氢呋喃二醇)、聚醚二胺(如JeffamineTM)、低Tg聚酯等。如需要，本发明的粘合剂可进一步配以增粘剂和用于所述固化基团的任选催化剂。
优选的是，压敏粘合剂在室温下具有的剪切弹性模量为3×105帕斯卡或更低，玻璃化转变温度(Tg)为约10℃或更低。热活化粘合剂在热活化温度下通常具有的剪切弹性模量为5×105帕斯卡或更低，Tg小于热活化温度。所有这三种类型的粘合剂即PSA、HAA和CIPA，无论是光学透明的还是非光学透明的，通常在它们的模量中都兼有弹性分量和粘性分量，即，材料的变形(应变)不与所施加的应力成正比，存在着一些粘性耗散。可以采用溶剂型溶液聚合或采用本体聚合来制备粘合剂。
在溶液聚合中，把溶剂型粘合剂、各组分和添加剂在有机溶剂中混合，由溶液涂布，然后干燥。当期望进行粘合剂的溶剂涂布时，反应可以在合适的溶剂(即，溶剂不干扰聚合反应)中进行，或者反应可以本体进行，然后把所得聚合物溶解在合适的溶剂中用于涂布。聚合物变化中的硬链段与软链段的相分离经常产生物理交联的网络。这一网络对聚合物和涂层提供高的内聚强度。在一些情况中，溶剂型粘合剂在干燥处理期间可另外地交联，或者在一些情况中可以在干燥步骤之后交联。这种交联剂包括热交联剂或UV交联剂，它们在制备溶剂涂布的粘合剂的干燥步骤期间或之后活化。也可以采用诸如电子束之类的辐射诱导交联。此外，本发明的聚合物也可以包含一种或多种可固化基团。这些可固化基团的例子包括通常通过水分固化的硅烷或端异氰酸酯、可以用热或辐射固化(任选在催化剂或引发剂的存在下)的环氧化物和烯键式不饱和基团(如丙烯酸酯)。可以通过任何已知的涂布技术将溶剂型粘合剂涂布在合适的柔性背衬材料上，从而制备涂布有粘合剂的片材。
在本体聚合中，使用静态搅拌器、挤出机或机械搅拌器混合包含粘合剂各组分的单体预混物，从而促进试剂的相互间紧密接触。任选地，还可以向混合物添加诸如二月桂酸二丁基锡之类的催化剂。本文中所述的本体聚合很好地适合于制备用于刚性对刚性的层合应用的厚(例如，0.005英寸至0.040英寸)粘合剂膜。例如，这种厚粘合剂膜可层合至玻璃片上，或者可用于将两片玻璃层合在一起。
在又一种方法中，使粘合剂的各组分与任选的添加剂(例如，增粘剂、热稳定剂、填料)和任选的交联剂混合。单体或单体混合物可用于填补间隙的应用，例如填充两基材之间(如两个玻璃基材之间)的空间。在一种应用中，使用注射器把粘合剂组分递送到间隙里，并利用热辐射固化试剂。这种方法和递送装置很适合具有变化厚度的间隙或其中基材具有基本上不平的表面的间隙。
柔性背衬材料可以是常规用作条带背衬、光学膜、剥离衬片或任何其他柔性材料的任何材料。当最终产品应用要求粘合剂与腐蚀敏感表面接触但在光路以外时，背衬无须是光学透明的。用作可用于粘合剂组合物的条带背衬的柔性背衬材料的典型例子包括由塑料膜(如聚丙烯、聚乙烯、聚氨酯、聚氯乙烯、聚酯(例如聚对苯二甲酸乙二醇酯)、醋酸纤维素和乙基纤维素)制成的那些。一些柔性背衬可以具有涂层。例如剥离衬片可涂有低粘附组分，如有机硅。示例性涂布技术包括辊涂、喷涂、刮涂、模具涂布、印刷等。本文中所述的溶液处理很好地适合于制备用作传送带的薄粘合剂膜，例如25微米至75微米(0.001英寸至0.003英寸)。所得条带经烘干后具有低挥发性的残余物。
实例
这些实例仅用于示例性目的，并且无意于限制所附权利要求书的范围。除非另外指明，否则实例以及说明书其余部分中的所有份数、百分比、比率等均按重量计。除另指明外，所用溶剂和其他试剂均购自Sigma-Aldrich Chemical Company(Milwaukee,Wisconsin)。
雾度及透射度测试
把25微米厚的粘合剂样品层合至25微米厚的聚酯膜454(得自DuPontCompany(Wilmington,DE))，层合的方式应确保膜与粘合剂层之间没有气泡截留。使用手压辊把已用异丙醇擦拭三遍的75mm×50mm的平显微载玻片(得自Dow Corning(Midland,MI)的载玻片)层合至粘合剂样品，确保粘合剂与载玻片之间没有气泡截留。使用9970 BYKGardner TCS Plus型分光光度计(得自BYK Gardner(Columbia,MD))测量透射度百分比(％)和雾度。用聚酯膜454和载玻片的夹层物进行背景测量。然后在分光光度计中直接对膜/粘合剂/玻璃层合体获得粘合剂样品的％透射度和雾度。
实例1至5的每一粘合剂具有的透光度值大于90％，雾度值低于5％。
腐蚀敏感层的ITO相容性研究
粘合剂与作为腐蚀敏感层的铟锡氧化物(ITO)层的相容性试验如下。把粘合剂样品传送至0.0015英寸厚的涂底漆的聚酯(PET)背衬以形成条带。然后把条带层合至主表面涂有ITO层的PET膜，使得粘合剂与迹线直接接触以形成层合体。使用欧姆表在ITO迹线上测量初始表面电阻，其中将表的电引线放在连接片上。将所得层合体在设定为60℃和90％相对湿度的烘箱中进行调理。在28天期间使用欧姆表定期测量每一样品的表面电阻。记录五次表面电阻测量值的平均值。
对照样品包括暴露于环境条件的ITO迹线，即，在具有含ITO的迹线的PET基材上没有层合粘合剂。
与其他腐蚀敏感表面的相容性测试
粘合剂与作为腐蚀敏感材料的镍或铝蒸汽金属化PET的相容性试验如下。把粘合剂样品传送至0.0015英寸厚的涂底漆的聚酯(PET)背衬上以形成条带。然后把条带层合至金属化PET膜，使得粘合剂与镍或铝直接接触。使用9970 BYK Gardner TCS Plus分光光度计(得自BYK Gardner(Columbia,MD))测量层合体的初始透光度和Δ(E)。将所得层合体在设定为60℃和90％相对湿度的烘箱中进行调理，在25天期间定期测量每一样品的透光度和Δ(E)。Δ(E)用于(在数学上)描述两种颜色之间的距离。其定义为(L1-L2)2、(a1-a2)2和(b1-b2)2之和的平方根，其中L、a和b是色指数。
实例1
往反应器里装入800克D-2000聚醚胺(得自Huntsman Corp.(TheWoodlands,Texas))、800克异丙醇、22.35克A二胺(得自DuPont(Wilmington,Delaware))和溶解于600克异丙醇中的151.36克W单体环脂族二异氰酸酯(得自Bayer Material Science AG(Leverkusen,德国))。在室温下将所得混合物在机械辊上放置48小时。然后把溶液涂在硅化聚酯剥离衬片上，并在70℃干燥10分钟，至最终的压敏聚酰胺基粘合剂的厚度为25微米(0.001英寸)。
实例2
往反应器里装入86克数均分子量为2,800的羟基官能化聚丁二烯(CAS号69102-90-5，得自Aldrich(Milwaukee,Wisconsin))与9.15克异佛尔酮二异氰酸酯(0.08当量)。让所得混合物在干燥氮气氛下于80℃下反应2小时。此后加入5.3克氨丙基三甲氧基硅烷(0.21当量)。搅拌混合物10分钟，然后加入66.7克甲苯以制备硅烷封端的氨基甲酸酯的60％固体含量的溶液。把溶液涂在衬片上并在70℃干燥15分钟，至最终的压敏厚度为48微米(0.0019英寸)。由于三甲氧基硅烷端基的存在，此干燥的聚合物涂层可在水分的存在下继续固化，从而产生交联的聚合物涂层。诸如二月桂酸二丁基锡之类的催化剂的存在可促进湿固化。
实例3
往反应器里装入150克3192、半结晶性聚酯多元醇(1020羟基当量重量，0.147当量，得自Uniqema(New Castle,Delaware))和27.7克异佛尔酮二异氰酸酯(0.25当量)。让所得混合物在干燥氮气氛下于80℃下反应2小时。此后加入22.3克氨丙基三甲氧基硅烷(0.10当量)。搅拌混合物10分钟，然后加入66.7克甲苯以制备硅烷封端的氨基甲酸酯的75％固体含量的溶液。把溶液涂在衬片上并在70℃干燥15分钟，至最终的压敏厚度为38微米(0.0015英寸)。如同实例2的材料一样，此聚合物也可在水分的存在下进行交联。
表1
实例4和5的组分
制备例A：有机硅聚脲(SPU)弹性体的合成
在反应容器中按1:1:2的摩尔比装入PDMS二胺33,000、DYTEK A和H12MDI到足量的2-丙醇中，得到所述试剂的20％固体含量的溶液。搅拌混合物2小时以得到20％固体含量的有机硅聚脲弹性体。
制备例B
将14K PDMS二胺样品(830.00克)加入到2升的3颈树脂烧瓶中，所述烧瓶配备有机械搅拌器、加热套、氮气入口管(带有旋塞阀)和出口管。用氮气将烧瓶吹扫15分钟，然后在剧烈搅拌下，滴加草酸二乙酯(33.56克)。将此反应混合物在室温下搅拌约一小时，然后在80℃下搅拌75分钟。反应烧瓶配有蒸馏接头和接收器。将反应混合物在120℃下真空加热2小时(133帕斯卡，1托)，然后在130℃下加热30分钟，直到不再收集到馏出物。将反应混合物冷却至室温，从而得到草酰氨基酯封端的有机硅产物(即，有机硅二胺在两端用单乙基草酰胺酯基封端)。对透明的可流动的液体进行气相色谱分析显示，不残余可检测量的草酸二乙酯。通过滴定确定用于制备例C的此前体的酯当量重量(当量重量＝8,272克/当量)。
确定当量重量的滴定方法
将大约10克制备例B的前体化合物加入广口瓶。加入大约50克THF溶剂。用磁力搅拌棒混合广口瓶内容物直至混合物均匀。计算前体的理论当量重量，然后加入此当量数的3至4倍量的N-己胺。将反应混合物搅拌最少4小时。加入溴酚兰(10-20滴)，并将内容物混合直至均匀。用1.0N(或0.1N)的盐酸滴定混合物至黄色滴定终点。前体的当量数等于加入到样品中的N-己胺的当量数减去滴定期间加入的盐酸的当量数。所述当量重量(克/当量)等于前体的样品重量除以前体的当量数。
制备例C
往广口瓶里称入制备例B的前体(98.13克)和乙二胺(0.36克)。将广口瓶密封，并且快速搅拌混合物，直至内容物变得过于粘稠而无法流动。在环境温度下，将广口瓶放置在辊磨机上过夜。收集固体产物。
实例4
对于实例4，有机硅聚脲弹性体粘合剂的制备方式是，利用常规的溶剂方法，将制备例A所得的有机硅聚脲弹性体(80份)与添加剂油(20份)在30重量％IPA(120.00份)和70重量％甲苯(280.00份)的溶剂共混物中混合(固体含量为20％)。将这些样品从溶剂混合物中涂到涂底漆的PET上并干燥到最终厚度为25微米。
实例5
将制备例C的共聚物(18.50克)溶解在THF(45.60克)中。将MQ树脂(30.83克，60.0％固体含量)加到该聚合物溶液。将所得混合物在环境条件下混合过夜，然后刮涂到PET上。将被涂覆的膜在环境温度下干燥约15分钟，然后在130℃烘箱中干燥10分钟，从而产生干燥厚度为25微米的涂层。
图5显示以上述测试方法所述的28天里实例1至5和对照样品的粘合剂相容性研究结果。数据显示，在暴露于60℃和90％相对湿度(RH)下28天后，所有五个样品都显示出20％或更小的电阻增加，完全处于经21天暴露中电阻变化小于20％的目标范围内。虽然与实例相比对照样品显示出最小的电阻增加，但在本文所设想的产品设备的应用中将需要粘合剂。
实例6
把实例5的粘合剂(25微米)层合到聚烯烃(ExxonMobil EXACT 8210)载体膜(125密耳)的两侧，产生具有聚烯烃芯和有机硅粘合剂表面的粘合剂转移带。
表2和3显示实例6的粘合剂在镍和铝蒸汽金属化PET膜上的相容性研究结果。数据显示，由透光度和Δ(E)的增加相似表明，粘合剂对金属表面的腐蚀极小。
表2
涂金属的PET膜暴露于60℃/90％RH后的透光度测量值
表3
涂金属的PET膜暴露于60℃/90％RH后的Δ(E)测量值
实例7
将两种有机硅粘合剂Dow Corning 7657和Dow Corning 7658(70/30干重比)与Dow Corning Syl-Off 7678交联剂(0.16份)和Dow Corning Syl-Off 4000催化剂混合。在130℃烘箱中将混合溶液在氟硅氧烷衬片上干燥约15分钟，产生干燥厚度为36微米的涂层。然后将干燥的粘合剂层合到聚烯烃(ExxonMobil EXACT 8210)载体膜(100密耳)的两侧，产生粘合剂转移带。
表4显示当把实例7的粘合剂放在ITO表面上时的表面电阻变化。数据显示，由电阻的小幅增加表明ITO腐蚀极小。
表4
ITO膜暴露于60℃/90％RH后的表面电阻变化
4天 14天 20天
对照-裸电路 -1.50％ 0.95％ 1.99％
实例7 -0.60％ 2.40％ 3.22％

Claims (20)

1.一种包含粘合剂的制品，所述粘合剂是粘弹性的，具有小于约5的酸值，并选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合，其与选自金属和金属合金的腐蚀敏感层接触，其中当将所述制品在约60℃和90％相对湿度下调理约21天时，所述腐蚀敏感层显示出偏离其初始电阻值20％或更小的变化，其中所述粘合剂不是现场固化粘合剂。
2.根据权利要求1所述的制品，其中所述腐蚀敏感层设置在基材的第一主表面上。
3.根据权利要求2所述的制品，其中所述粘合剂和所述基材中的至少一者是光学透明的。
4.根据权利要求2所述的制品，其中所述基材选自玻璃和聚合物膜。
5.根据权利要求2所述的制品，其中所述腐蚀敏感层覆盖所述基材的第一主表面的基本上全部或覆盖所述基材的第一主表面的一部分。
6.根据权利要求5所述的制品，其中当所述腐蚀敏感层覆盖所述基材的第一主表面的一部分时，所述层具有规则图案。
7.根据权利要求1所述的制品，其中所述腐蚀敏感层选自铜、铜合金、银、银合金、铟锡氧化物、镍，铝和锑锡氧化物。
8.根据权利要求1所述的制品，其中所述腐蚀敏感层是基本上平的。
9.根据权利要求2所述的制品，其包括多个交替的粘合剂层与基材层，所述基材具有在该基材上设置的腐蚀敏感层。
10.根据权利要求2所述的制品，其还包括设置成与所述基材的边缘邻接并与所述腐蚀敏感层连接的连接片。
11.根据权利要求2所述的制品，其中所述基材具有与所述第一主表面相对的第二主表面，每个表面具有设置在其至少一部分上的所述腐蚀敏感层，且所述粘合剂设置在所述腐蚀敏感层上。
12.根据权利要求1所述的制品，其中所述粘合剂是压敏粘合剂或热活化粘合剂。
13.根据权利要求1所述的制品，其中所述粘合剂是具有相对的第一和第二主表面的膜，且所述腐蚀敏感层设置在所述粘合剂膜的所述第一和所述第二表面的每一者上。
14.一种制备制品的方法，该方法包括以下步骤：
提供基材，所述基材具有设置在其至少一部分上的腐蚀敏感层；
提供条带，所述条带包括(i)具有相对的第一和第二主表面的背衬，(ii)具有小于约5的酸值的粘合剂，并且其选自聚脲、聚酰胺、聚氨酯、聚酯、加成固化有机硅以及它们的组合，其中所述粘合剂是粘弹性的，并且所述粘合剂不是现场固化粘合剂；和
将所述条带层合至所述基材，使得所述粘合剂接触所述腐蚀敏感层。
15.根据权利要求14所述的方法，其中所述粘合剂和所述基材中的至少一者是光学透明的。
16.根据权利要求14所述的方法，其中所述基材选自玻璃和聚合物膜。
17.根据权利要求14所述的方法，其中当所述腐蚀敏感层以规则图案覆盖。
18.根据权利要求14所述的方法，其中所述腐蚀敏感层选自铜、铜合金、银、银合金、铟锡氧化物、镍，铝和锑锡氧化物。
19.根据权利要求14所述的方法，其中所述腐蚀敏感层是基本上平的。
20.根据权利要求14所述的方法，其还包括设置成与所述基材的边缘邻接并与所述腐蚀敏感层接触的连接片。
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JP2011530438A (ja) 2011-12-22
US20100040842A1 (en) 2010-02-18
KR20110041565A (ko) 2011-04-21
TW201012655A (en) 2010-04-01
WO2010019528A3 (en) 2010-05-14
KR101701522B1 (ko) 2017-02-01
TWI468296B (zh) 2015-01-11
JP5499031B2 (ja) 2014-05-21
EP2315663A2 (en) 2011-05-04
WO2010019528A2 (en) 2010-02-18
EP2315663A4 (en) 2015-06-24
EP2315663B1 (en) 2020-09-23
CN102123859A (zh) 2011-07-13

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