CN106133062A - 剥离层形成用组合物 - Google Patents
剥离层形成用组合物 Download PDFInfo
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Abstract
本发明提供用于形成具有下述剥离层的组合物,所述剥离层可维持与设置该剥离层的玻璃基板的密合性从而不在与玻璃基板之间的界面处产生剥离,同时也可实现将形成于剥离层上部的层或层组从该剥离层简易地剥离。本发明提供一种组合物,其为用于形成在紧邻于玻璃基板的上方设置的剥离层的组合物,所述组合物含有(A)芳香族聚酰亚胺及/或芳香族聚酰亚胺前体;和(B)酰胺类溶剂,并且来自上述(A)的芳香族聚酰亚胺满足下述条件(1)~(4):(1)加热时的重量变化中的1%重量减少的温度为500℃以上;(2)波长1000nm处的折射率为1.7以上;(3)波长1000nm处的折射率与双折射率之差为0.15以上;及(4)表面能为40dyne/cm以上。
Description
技术领域
本发明涉及用于形成在紧邻于玻璃基板的上方(ガラス基板直上)设置的剥离层的组合物。
背景技术
近年来,对于电子器件而言,赋予其可弯曲的功能、薄型化及轻量化的性能是令人期望的。鉴于此,期望使用轻量的柔性塑料基板,来代替以往的沉重且脆弱而不能弯曲的玻璃基板。此外,对于新一代显示器而言,期望使用轻量的柔性塑料基板来开发有源式全彩(active full-color)TFT显示面板。
因此,已在开始对以树脂膜作为基板的电子器件的制造方法进行各种研究,正在对能够将现有的TFT设备转用于制造新一代显示器的工艺进行研究。
专利文献1、2及3公开了下述方法:在玻璃基板上形成非晶硅薄膜层,在该薄膜层上形成塑料基板后,从玻璃面侧照射激光,利用伴随非晶硅的结晶化产生的氢气而将塑料基板从玻璃基板剥离。
此外,专利文献4公开了使用专利文献1~3所公开的技术将被剥离层(专利文献4中记载为“被转印层(被転写層)”)贴附于塑料膜从而制成液晶显示装置的方法。
然而,专利文献1~4公开的方法(尤其是专利文献4公开的方法)必须使用透光性高的基板,存在下述问题:为了施予足以使激光通过基板、进而使非晶硅中含有的氢放出的能量,较大程度的激光的照射被认为是必要的,其将对被剥离层造成损伤。此外,由于激光处理需要较长时间,并且将具有较大面积的被剥离层剥离是困难的,因此还存在难以提高器件制作的生产率的问题。
现有技术文献
专利文献
专利文献1:日本特开平10-125929号公报。
专利文献2:日本特开平10-125931号公报。
专利文献3:WO2005/050754号小册子。
专利文献4:日本特开平10-125930号公报。
发明内容
发明所要解决的课题
因此,本发明的目的在于解决上述课题。
具体而言,本发明的目的在于提供用于形成下述剥离层的组合物,所述剥离层用于实现在不对适用于柔性电子器件的基板造成损伤的情况下将该剥离层剥离。
另外,除了上述目的之外,或者在上述目的以外,本发明的目的还在于提供用于形成下述剥离层的组合物,所述剥离层可维持与设置该剥离层的玻璃基板的密合性从而不在与玻璃基板之间的界面处产生剥离,同时也可实现将形成于剥离层上部的层或层组从该剥离层简易地剥离。
用于解决课题的手段
本申请的发明人做出了以下发明。
<1>组合物,其为用于形成在紧邻于玻璃基板的上方设置的剥离层的组合物,所述组合物含有:
(A)芳香族聚酰亚胺及/或芳香族聚酰亚胺前体;和
(B)酰胺类溶剂,
上述组合物中,来自(A)的芳香族聚酰亚胺满足下述条件(1)~(4):
(1)加热时的重量变化中的1%重量减少的温度为500℃以上;
(2)波长1000nm处的折射率为1.7以上;
(3)波长1000nm处的折射率与双折射率之差为0.15以上;及
(4)表面能为40dyne/cm以上。
<2>上述<1>中,(A)成分优选为使用选自由对苯二胺及三联苯二胺(terphenyl diamine)组成的组中的至少一种二胺成分制造的。
<3>上述<2>中,对苯二胺及/或三联苯二胺的量优选为全部二胺成分100摩尔%中的70摩尔%以上。
<4>上述<1>~<3>中的任一项中,(A)成分优选为使用具有第一骨架的芳香族二胺制造的,所述第一骨架为选自由联苯骨架、咪唑骨架及噁唑骨架组成的组中的至少一种。
<5>上述<1>~<4>中的任一项中,(A)成分优选为使用具有第二骨架的酸二酐制造的,所述第二骨架为选自由苯骨架、萘骨架及联苯骨架组成的组中的至少一种。
<6>上述<1>~<3>中的任一项中,(B)成分优选为下述式(I)表示的溶剂、及/或式(II)(式(I)及(II)中,R1及R2各自独立地表示碳原子数1~4的烷基,h表示自然数)表示的溶剂。
<7>剥离层,其被设置在紧邻于玻璃基板的上方,且是利用上述<1>~<6>中任一项所述的组合物形成的。
<8>被剥离体的制造方法,所述方法通过具有下述工序而得到被剥离体,所述工序为:
a)将上述<1>~<6>中任一项所述的组合物涂布于玻璃基板上后,形成剥离层的工序;
b)在该剥离层上形成被剥离体的工序;及
c)在剥离层与被剥离体的界面处将被剥离体剥离的工序。
发明的效果
通过本发明,可以解决上述课题。
具体而言,通过本发明,能够提供用于形成下述剥离层的组合物,所述剥离层用于实现在不对适用于柔性电子器件的基板造成损伤的情况下将该剥离层剥离。
另外,除了上述效果之外,或者在上述效果以外,通过本发明还能够提供用于形成下述剥离层的组合物,所述剥离层可维持与设置该剥离层的玻璃基板的密合性从而不在与玻璃基板之间的界面处产生剥离,同时也可实现将形成于剥离层上部的层或层组从该剥离层简易地剥离。
具体实施方式
本申请提供用于形成在紧邻于玻璃基板的上方设置的剥离层的组合物。
以下,对该组合物进行详细说明。
<组合物>
本发明的组合物含有:(A)芳香族聚酰亚胺及/或芳香族聚酰亚胺前体;及(B)酰胺类溶剂。
<<(A)成分>>
(A)成分为芳香族聚酰亚胺及/或芳香族聚酰亚胺前体。
此处,所谓“芳香族聚酰亚胺”是指,由于构成聚酰亚胺的二胺成分及酸二酐成分中的双方均具有芳香族基团,所以由其得到的聚酰亚胺主要在主链上具有芳香族基团。
此外,所谓“芳香族聚酰亚胺前体”是指,上述的芳香族聚酰亚胺的前体,典型地,可以举出聚酰胺酸、聚酰胺酸酯、聚异酰亚胺,优选聚酰胺酸。
具体而言,作为芳香族聚酰亚胺,可分为构成该聚酰亚胺的二胺成分及酸二酐成分而举出下述的成分,但并不限定于此。
<二胺成分>
作为具有芳香族基团的二胺成分,可以举出1,4-二氨基苯(对苯二胺)、1,3-二氨基苯(间苯二胺)、1,2-二氨基苯(邻苯二胺)、2,4-二氨基甲苯、2,5-二氨基甲苯、2,6-二氨基甲苯、4,6-二甲基-间苯二胺、2,5-二甲基-对苯二胺、2,6-二甲基-对苯二胺、2,4-双(氨基叔丁基)甲苯、2,4,6-三甲基-1,3-苯二胺、2,3,5,6-四甲基-对苯二胺、间苯二甲胺、对苯二甲胺、5-三氟甲基苯-1,3-二胺、5-三氟甲基苯-1,2-二胺、3,5-双(三氟甲基)苯-1,2-二胺等具有1个苯核的二胺;4,4’-二氨基二苯基醚、3,4’-二氨基二苯基醚、4,4’-二氨基二苯基甲烷、3,3’-二甲基-4,4’-二氨基联苯、2,2’-二甲基-4,4’-二氨基联苯、2,2’-双(三氟甲基)-4,4’-二氨基联苯、3,3’-二甲基-4,4’-二氨基二苯基甲烷、3,3’-二羧基-4,4’-二氨基二苯基甲烷、3,3’,5,5’-四甲基-4,4’-二氨基二苯基甲烷、双(4-氨基苯基)硫醚、4,4’-二氨基苯甲酰苯胺、3,3’-二氯联苯胺、3,3’-二甲基联苯胺、2,2’-二甲基联苯胺、3,3’-二甲氧基联苯胺、2,2’-二甲氧基联苯胺、3,3’-二氨基二苯基醚、3,4’-二氨基二苯基醚、4,4’-二氨基二苯基醚、3,3’-二氨基二苯硫醚、3,4’-二氨基二苯硫醚、4,4’-二氨基二苯硫醚、3,3’-二氨基二苯砜、3,4’-二氨基二苯砜、4,4’-二氨基二苯砜、3,3’-二氨基二苯甲酮、3,3’-二氨基-4,4’-二氯二苯甲酮、3,3’-二氨基-4,4’-二甲氧基二苯甲酮、3,3’-二氨基二苯基甲烷、3,4’-二氨基二苯基甲烷、4,4’-二氨基二苯基甲烷、2,2-双(3-氨基苯基)丙烷、2,2-双(4-氨基苯基)丙烷、2,2-双(3-氨基苯基)-1,1,1,3,3,3-六氟丙烷、2,2-双(4-氨基苯基)-1,1,1,3,3,3-六氟丙烷、3,3’-二氨基二苯亚砜、3,4’-二氨基二苯亚砜、4,4’-二氨基二苯亚砜、2,2’-双(三氟甲基)联苯-4,4’-二胺、3,3’-双(三氟甲基)联苯-4,4’-二胺、3,3’,5,5’-四氟联苯-4,4’-二胺、4,4’-二氨基八氟联苯等具有2个苯核的二胺;1,3-双(3-氨基苯基)苯、1,3-双(4-氨基苯基)苯、1,4-双(3-氨基苯基)苯、1,4-双(4-氨基苯基)苯、1,3-双(4-氨基苯氧基)苯、1,4-双(3-氨基苯氧基)苯、1,4-双(4-氨基苯氧基)苯、1,3-双(3-氨基苯氧基)-4-三氟甲基苯、3,3’-二氨基-4-(4-苯基)苯氧基二苯甲酮、3,3’-二氨基-4,4’-二(4-苯基苯氧基)二苯甲酮、1,3-双(3-氨基苯基硫醚)苯(1,3-bis(3-aminophenylsulfide)benzene)、1,3-双(4-氨基苯基硫醚)苯、1,4-双(4-氨基苯基硫醚)苯、1,3-双(3-氨基苯砜)苯、1,3-双(4-氨基苯砜)苯、1,4-双(4-氨基苯砜)苯、1,3-双〔2-(4-氨基苯基)异丙基〕苯、1,4-双〔2-(3-氨基苯基)异丙基〕苯、1,4-双〔2-(4-氨基苯基)异丙基〕苯等具有3个苯核的二胺;3,3’-双(3-氨基苯氧基)联苯、3,3’-双(4-氨基苯氧基)联苯、4,4’-双(3-氨基苯氧基)联苯、4,4’-双(4-氨基苯氧基)联苯、双〔3-(3-氨基苯氧基)苯基〕醚、双〔3-(4-氨基苯氧基)苯基〕醚、双〔4-(3-氨基苯氧基)苯基〕醚、双〔4-(4-氨基苯氧基)苯基〕醚、双〔3-(3-氨基苯氧基)苯基〕酮、双〔3-(4-氨基苯氧基)苯基〕酮、双〔4-(3-氨基苯氧基)苯基〕酮、双〔4-(4-氨基苯氧基)苯基〕酮(双(4-氨基苯氧基)二苯甲酮)、双〔3-(3-氨基苯氧基)苯基〕硫醚、双〔3-(4-氨基苯氧基)苯基〕硫醚、双〔4-(3-氨基苯氧基)苯基〕硫醚、双〔4-(4-氨基苯氧基)苯基〕硫醚、双〔3-(3-氨基苯氧基)苯基〕砜、双〔3-(4-氨基苯氧基)苯基〕砜、双〔4-(3-氨基苯氧基)苯基〕砜、双〔4-(4-氨基苯氧基)苯基〕砜、双〔3-(3-氨基苯氧基)苯基〕甲烷、双〔3-(4-氨基苯氧基)苯基〕甲烷、双〔4-(3-氨基苯氧基)苯基〕甲烷、双〔4-(4-氨基苯氧基)苯基〕甲烷、2,2-双〔3-(3-氨基苯氧基)苯基〕丙烷、2,2-双〔3-(4-氨基苯氧基)苯基〕丙烷、2,2-双〔4-(3-氨基苯氧基)苯基〕丙烷、2,2-双〔4-(4-氨基苯氧基)苯基〕丙烷、2,2-双〔3-(3-氨基苯氧基)苯基〕-1,1,1,3,3,3-六氟丙烷、2,2-双〔3-(4-氨基苯氧基)苯基〕-1,1,1,3,3,3-六氟丙烷、2,2-双〔4-(3-氨基苯氧基)苯基〕-1,1,1,3,3,3-六氟丙烷、2,2-双〔4-(4-氨基苯氧基)苯基〕-1,1,1,3,3,3-六氟丙烷、9,9-双(4-氨基苯基)芴、9,9-双(4-氨基苯基)芴、9,9’-双(4-氨基苯氧基苯基)芴等具有4个以上的苯核的二胺;5-氨基-2-(对氨基苯基)苯并噁唑、5-氨基-2-(间氨基苯基)苯并噁唑、6-氨基-2-(对氨基苯基)苯并噁唑、6-氨基-2-(间氨基苯基)苯并噁唑、2,2’-对-苯撑双(5-氨基苯并噁唑)、2,2’-对苯撑双(6-氨基苯并噁唑)、1-(5-氨基苯并噁唑(benzoxazolo))-4-(6-氨基苯并噁唑)苯、2,6-(4,4’-二氨基二苯基)苯并〔1,2-d:5,4-d’〕二噁唑、2,6-(4,4’-二氨基二苯基)苯并〔1,2-d:4,5-d’〕二噁唑、2,6-(3,4’-二氨基二苯基)苯并〔1,2-d:5,4-d’〕二噁唑、2,6-(3,4’-二氨基二苯基)苯并〔1,2-d:4,5-d’〕二噁唑、2,6-(3,3’-二氨基二苯基)苯并〔1,2-d:5,4-d’〕二噁唑、2,6-(3,3’-二氨基二苯基)苯并〔1,2-d:4,5-d’〕二噁唑、2,4-二氨基吡啶、2,6-二氨基吡啶、2,5-二氨基吡啶等具有苯并噁唑结构的二胺等,但并不限定于此。它们可单独使用,或者也可混合2种以上而使用。
对于二胺成分而言,在某个方面,优选使用选自由对苯二胺及三联苯二胺组成的组中的至少1种二胺成分。
该情况下,对苯二胺及/或三联苯二胺的量在全部二胺成分100摩尔%中为70摩尔%以上,优选为80摩尔%以上,更优选为90摩尔%以上。
对于二胺成分而言,在另一方面,优选为具有选自由联苯骨架、咪唑骨架及噁唑骨架组成的组中的至少1种第一骨架的芳香族二胺。
<酸二酐成分>
作为具有芳香族基团的酸二酐成分,可以举出具有苯骨架的酸二酐、具有萘骨架的酸二酐、具有联苯骨架的酸二酐等,但并不限定于此。
具体而言,可以举出均苯四甲酸二酐、3,3’,4,4’-联苯四甲酸二酐、2,2’,3,3’-联苯四甲酸二酐、2,3,3’,4’-联苯四甲酸二酐、氧双邻苯二甲酸二酐、3,4,3’,4’-二苯基砜四甲酸二酐、双(3,4-二羧基苯基)硫醚二酐、2,2-双(3,4-二羧基苯基)-1,1,1,3,3,3-六氟丙烷二酐、2,3,3’,4’-二苯甲酮四甲酸二酐、3,3’,4,4’-二苯甲酮四甲酸二酐、双(3,4-二羧基苯基)甲烷二酐、2,2-双(3,4-二羧基苯基)丙烷二酐、对-苯撑双(偏苯三酸单酯酸酐)、对-甲基苯撑双(偏苯三酸单酯酸酐)、对-(2,3-二甲基苯撑)双(偏苯三酸单酯酸酐)、4,4’-联苯撑双(偏苯三酸单酯酸酐)、1,4-萘双(偏苯三酸单酯酸酐)、2,6-萘双(偏苯三酸单酯酸酐)、2,2-双(4-羟基苯基)丙烷二苯甲酸酯-3,3’,4,4’-四甲酸二酐、间三联苯-3,4,3’,4’-四甲酸二酐、对三联苯-3,4,3’,4’-四甲酸二酐、1,3-双(3,4-二羧基苯氧基)苯二酐、1,4-双(3,4-二羧基苯氧基)苯二酐、1,4-双(3,4-二羧基苯氧基)联苯二酐、2,2-双〔(3,4-二羧基苯氧基)苯基〕丙烷二酐、2,3,6,7-萘四甲酸二酐、1,4,5,8-萘四甲酸二酐、4,4’-(2,2-六氟异亚丙基)双邻苯二甲酸二酐、N,N’-(2,2’-双{三氟甲基}-[1,1’-联苯]-4,4’-二基)双(1,3-二氧代-1,3-二羟基苯并呋喃-5-甲酰胺)等,但并不限定于此。它们可单独使用,或者也可混合2种以上而使用。
<来自(A)的芳香族聚酰亚胺的特性>
本申请的组合物中的来自于(A)的芳香族聚酰亚胺具有下述(1)~(4)的特性。
<<(1)~(4)的特性>>
(1)加热时的重量变化中的1%重量减少的温度为500℃以上,优选为520℃以上,更优选为550℃以上;
(2)波长1000nm处的折射率为1.7以上;
(3)波长1000nm处的折射率与双折射率之差为0.15以上,优选为0.16以上;及
(4)表面能为40dyne/cm以上,优选为45~70dyne/cm,更优选为45~60dyne/cm。
需要说明的是,所谓“来自于(A)的芳香族聚酰亚胺”或“来自(A)的芳香族聚酰亚胺”,在(A)成分仅由“芳香族聚酰亚胺”组成的情况下,是指该“芳香族聚酰亚胺”。此外,在(A)成分仅由“芳香族聚酰亚胺前体”组成的情况下,是指该前体全部变为“芳香族聚酰亚胺”时的该“芳香族聚酰亚胺”。在(A)成分含有“芳香族聚酰亚胺A”及“芳香族聚酰亚胺前体B”的情况下,是指由“芳香族聚酰亚胺前体B”形成的“芳香族聚酰亚胺B’”和“芳香族聚酰亚胺A”的整体。
通过具有上述特性,从而在由组合物形成剥离层时,该剥离层与玻璃基板的密合性变得良好,且另一方面,在剥离层上形成被剥离体时,该被剥离体可通过用刀具(cutter)等刻上切口而容易地被剥离。
<(B)成分>
本申请的组合物含有酰胺类溶剂作为(B)成分。
所谓酰胺类溶剂,是指具有酰胺基、烷基酰胺基的液体。
作为酰胺类溶剂,例如,可以举出N-甲基吡咯烷酮、N-乙基吡咯烷酮、DMAc、DMF、Ekuamido M、Ekuamido B(出光兴产(株)制)等,但并不限定于此。
作为酰胺类溶剂,优选为下述式(I)表示的溶剂、及/或式(II)(式(I)及(II)中,R1及R2各自独立地表示碳原子数1~4的烷基,h表示自然数。)表示的溶剂。
本发明的组合物除了含有上述(A)成分及(B)成分之外,还可以含有各种成分。例如,可以举出交联剂(以下,也称为交联性化合物。),但并不限定于此。
作为上述交联性化合物,例如可以举出含有2个以上环氧基的化合物、具有氨基的氢原子被羟甲基、烷氧基甲基或这两者取代而得的基团的三聚氰胺衍生物、苯胍胺衍生物或甘脲等,但并不限定于此。
以下举出交联性化合物的具体例,但并不限定于此。
作为含有2个以上环氧基的化合物,可以举出Epolead GT-401、Epolead GT-403、Epolead GT-301、Epolead GT-302、Celloxide 2021、Celloxide 3000(以上为(株)Daicel制)等具有环己烯结构的环氧化合物;Epikote1001、Epikote 1002、Epikote 1003、Epikote1004、Epikote 1007、Epikote 1009、Epikote 1010、Epikote 828(以上为Japan EpoxyResin(株)制(现:三菱化学(株)制,jER(注册商标)系列))等双酚A型环氧化合物;Epikote807(Japan Epoxy Resin(株)制)等双酚F型环氧化合物;Epikote 152、Epikote 154(以上为Japan Epoxy Resin(株)制(现:三菱化学(株)制,jER(注册商标)系列))、EPPN 201、EPPN202(以上为日本化药(株)制)等苯酚Novolacs型环氧化合物;ECON-102、ECON-103S、ECON-104S、ECON-1020、ECON-1025、ECON-1027(以上为日本化药(株)制)、Epikote 180S75(JapanEpoxy Resin(株)(现:三菱化学(株)制,jER(注册商标)系列)制)等甲酚Novolacs型环氧化合物;V8000-C7(DIC(株)制)等萘型环氧化合物;Denacol EX-252(Nagase ChemteX(株)制)、CY175、CY177、CY179、Araldite CY-182、Araldite CY-192、Araldite CY-184(以上为BASF公司制)、Epiclon 200、Epiclon 400(以上为DIC(株)制)、Epikote 871、Epikote 872(以上为Japan Epoxy Resin(株)制(现:三菱化学(株)制,jER(注册商标)系列))、ED-5661、ED-5662(以上为Celanese Coating(株)制)等脂环式环氧化合物;Denacol EX-611、Denacol EX-612、Denacol EX-614、Denacol EX-622、Denacol EX-411、Denacol EX-512、Denacol EX-522、Denacol EX-421、Denacol EX-313、Denacol EX-314、Denacol EX-312(以上为Nagase ChemteX(株)制)等脂肪族聚缩水甘油醚化合物等。
作为具有氨基的氢原子被羟甲基、烷氧基甲基或这两者取代而得的基团的三聚氰胺衍生物、苯胍胺衍生物或甘脲,可以举出每1个三嗪环被平均3.7个甲氧基甲基取代的MX-750、每1个三嗪环被平均5.8个甲氧基甲基取代的MW-30((以上为(株)三和化学制);Cymel300、Cymel 301、Cymel 303、Cymel 350、Cymel 370、Cymel 771、Cymel 325、Cymel 327、Cymel 703、Cymel 712等甲氧基甲基化三聚氰胺;Cymel 235、Cymel 236、Cymel 238、Cymel212、Cymel 253、Cymel 254等甲氧基甲基化丁氧基甲基化三聚氰胺;Cymel 506、Cymel 508等丁氧基甲基化三聚氰胺;Cymel 1141这样的含有羧基的甲氧基甲基化异丁氧基甲基化三聚氰胺;Cymel 1123这样的甲氧基甲基化乙氧基甲基化苯胍胺;Cymel 1123-10这样的甲氧基甲基化丁氧基甲基化苯胍胺;Cymel 1128这样的丁氧基甲基化苯胍胺;Cymel 1125-80这样的含有羧基的甲氧基甲基化乙氧基甲基化苯胍胺;Cymel 1170这样的丁氧基甲基化甘脲;Cymel 1172这样的羟甲基化甘脲(以上为Mitsui Cyanamid(株)制(现:Nihon CytecIndustries(株))等。
通过本申请的组合物,能够形成可设置在紧邻于玻璃基板的上方的剥离层。
例如,可以利用以往已知的方法将本申请的组合物涂布于玻璃基板上,并以规定的温度对得到的涂布膜进行加热,由此形成剥离层。
此外,被剥离体层可以形成于剥离层上。被剥离体层可以为单层,也可以为多层。对于各种器件的制作而言,实际中为多层。
对于被剥离体层中的位于紧邻于剥离层的上方的层而言,虽然取决于采用的剥离层,但优选使用与该剥离层的剥离性良好的层,换言之,优选使用与采用的剥离层的密合性不高的层。
作为本申请的其他方面,提供被剥离体的制造方法。
该方法通过具有下述a)~c)的工序,从而可以得到被剥离体。
a)将本申请的组合物涂布于玻璃基板上后,形成剥离层的工序;
b)在该剥离层上形成被剥离体的工序;及
c)在剥离层与被剥离体的界面处将被剥离体剥离的工序;
在b)工序中,“被剥离体”可以为单层,也可以为多层。需要说明的是,对于“被剥离体”中的位于紧邻于剥离层的上方的层而言,虽然取决于采用的剥离层,但优选使用与该剥离层的剥离性良好的层,换言之,优选使用与采用的剥离层的密合性不高的层。
以下,根据实施例对本发明进行说明,但本发明不受该实施例的限制。
实施例
对于本实施例中使用的缩写,以下进行列举说明。
<溶剂>
NMP:N-甲基吡咯烷酮。
<胺类>
PDA:对苯二胺。
APAB:2-(3-氨基苯基)-5-氨基苯并咪唑。
DATP:4,4’-二氨基对三联苯。
6FAP:2,2-双(3-氨基-4-羟基苯基)六氟丙烷。
<酸二酐>
BPDA:3,3’,4,4’-联苯四甲酸二酐。
BA-TME:4,4’-联苯撑双(偏苯三酸单酯酸酐)。
PMDA:均苯四甲酸二酐。
<醛>
IPHA:间苯二甲醛。
[数均分子量及重均分子量的测定]
对于聚合物的重均分子量(以下简称为“Mw”)和分子量分布而言,使用日本分光株式会社制GPC装置(Shodex(商标)柱KF803L及KF805L),在使作为洗脱溶剂的二甲基甲酰胺的流量为1ml/分钟、柱温为50℃的条件下进行测定。需要说明的是,Mw为聚苯乙烯换算值。
<合成例>
<合成例1聚酰亚胺前体P1的合成>
将17.8g(0.164摩尔)PDA、2.38g(0.009摩尔)DATP及2.05g(0.009摩尔)APAB溶解于425g的NMP中,同时添加52.8g(0.179摩尔)BPDA,然后,再次添加7.4g的NMP,在氮气气氛下,于23℃进行24小时反应。得到的聚酰亚胺前体P1的Mw为63000,分子量分布为9.9。
<合成例2聚酰亚胺前体P2的合成>
将30.8g(0.118摩尔)的DATP溶解于425g的NMP中,同时添加34.1g(0.116摩尔)BPDA,然后,再次添加10g的NMP,在氮气气氛下,于23℃进行24小时反应。得到的聚酰亚胺前体P2的Mw为70700,分子量分布为9.7。
<合成例3聚酰亚胺前体P3的合成>
将20.261g(0.1875摩尔)PDA和12.206g(0.0469摩尔)TPDA溶解于617.4g的NMP中,于15℃冷却后,添加50.112g(0.2298摩尔)PMDA,在氮气气氛下,于50℃进行48小时反应。得到的聚酰亚胺前体P3的Mw为82,100,分子量分布为2.7。
<合成例4聚酰亚胺前体P4的合成>
将9.66g(0.089摩尔)PDA和1.05g(0.005摩尔)APAB溶解于440g的NMP中,添加49.2g(0.092摩尔)BP-TME,在氮气气氛下,于室温进行24小时反应。得到的聚酰亚胺前体P4的Mw为57000,分子量分布为9.3。
<合成例5聚酰亚胺前体P5的合成>
将3.176g(0.02937摩尔)PDA溶解于88.2g的NMP中,添加8.624g(0.02931摩尔)BPDA后,在氮气气氛下,于23℃进行24小时反应。得到的聚酰亚胺前体P5的Mw为107,300,分子量分布为4.6。
<合成例6聚苯并噁唑前体(P6)的合成>
将3.18g(0.059摩尔)6FAP溶解于70g的NMP中,添加7.92g(0.060摩尔)IPHA后,在氮气气氛下,于23℃进行24小时反应。得到的聚合物的Mw为107,300,分子量分布为4.6。
<合成例7聚酰亚胺前体P7的合成>
PMDA(98)//p-PDA(100)
将10.078g(93mmol)p-PDA溶解于220.0g的NMP中。向得到的溶液中添加19.922g(91mmol)PMDA,在氮气气氛下,于23℃进行24小时反应。得到的聚合物的Mw为55,900,分子量分布为3.1。
<剥离层基板的制作>
将上述合成例1~7中得到的P1~P7用NMP稀释至4wt%,使用旋转涂布机将其涂布于100mm×100mm玻璃基板(OA-10G无碱玻璃)或硅晶片上后,按照固化条件A~C中的任意一项,利用烘箱进行烧成从而制作剥离层。
固化条件A:120℃维持30分钟→升温→300℃维持60分钟→升温→400℃维持60分钟。需要说明的是,升温速度为10℃/分钟。
固化条件B:120℃维持30分钟→升温→180℃维持20分钟→升温→240℃维持20分钟→升温→300℃维持20分钟→升温→400℃维持20分钟→升温→450℃维持60分钟。需要说明的是,升温速度为10℃/分钟。
固化条件C:80℃维持10分钟→升温→300℃维持30分钟→升温→400℃维持30分钟。需要说明的是,升温速度为10℃/分钟。
使用接触式膜厚测定仪(株式会社ULVAC制Dektak 3ST),测定所得到的涂布膜的膜厚。
将使用的P1~P7的前体、涂布基板、固化条件、及制作的剥离层的膜厚示于表1。
表1
前体 | 基板 | 固化条件 | 膜厚(μm) | |
实施例1 | P1 | 玻璃 | A | 0.165 |
实施例2 | P2 | 玻璃 | B | 0.857 |
实施例3 | P3 | 玻璃 | B | 0.162 |
实施例4 | P4 | 玻璃 | A | 0.172 |
实施例5 | P7 | 玻璃 | C | 0.125 |
比较例1 | P5 | 硅晶片 | A | 0.167 |
比较例2 | P6 | 玻璃 | A | 0.181 |
比较例3 | P6 | 硅晶片 | A | 0.166 |
<交叉切割试验I>
针对表1所示的实施例1~5及比较例1~3的具备剥离层的基板,通过交叉切割试验I确认基板(玻璃或硅晶片)/剥离层的密合力。
交叉切割试验I如下所述地进行。
(1)在剥离层上制作100个1mm见方的正方形。
(2)然后,用粘贴胶带(Cellotape(注册商标))贴附上述的正方形并进行剥离工序。
(3)计数在剥离工序后残留于基板上的上述正方形的个数。
<交叉切割试验I的结果的指标>
作为交叉切割试验的结果,用以下的指标表示剥离的程度。
5B:未剥离。
4B:5%以下的剥离。
3B:5~15%的剥离。
2B:15~35%的剥离。
1B:35~65%的剥离。
0B:65%~80%的剥离。
B:80%~95%的剥离。
A:95%至不足100%的剥离。
AA:100%的剥离。
与上述交叉切割试验I分开地,针对表1所示的实施例1~5及比较例1~3的具备剥离层的基板,测定了构成该剥离层的成分的特性,即(1)显示出加热时的重量变化中的1%重量减少的温度,(2)波长1000nm处的折射率,(3)波长1000nm处的双折射率,及(4)表面能。需要说明的是,各特性的测定条件等如下所示。
<(1)显示出加热时的重量变化中的1%重量减少的温度>
使用Bruker(株)制TD-DTA2000ST,在氮气气氛下进行热重(TG)测定,求出重量减少1%的温度。
<(2)波长1000nm处的折射率及(3)双折射率>
使用高速光谱型椭圆偏振仪M-2000(J.A.Woolam Japan株式会社制),测定折射率及双折射率。需要说明的是,折射率为1000nm处的数值中的面内折射率,双折射率为面内折射率与面外折射率之差。
<(4)表面能>
使用全自动接触角计DM-701(共和界面科学(株)制),测定利用上述合成例1~7中得到的P1~P7而得的剥离层的表面能。需要说明的是,测定中使用的溶剂为水和二碘甲烷,从这些溶剂的接触角算出表面能。
<被剥离体的形成及其剥离试验(交叉切割试验II)>
在实施例1~5及比较例1~3的具备剥离层的基板上形成被剥离体,通过交叉切割试验II确认其剥离的程度。
<<被剥离体层的制作>>
在具备剥离层的基板的该剥离层上,形成作为被剥离体的聚酰亚胺层。
具体而言,使用棒涂机,将上述合成例5或合成例1中得到的前体P5或P1,涂布于表1所示的实施例1~5及比较例1~3的具备剥离层的基板的剥离层上。然后,利用烘箱按照下述条件进行固化,制作由聚酰亚胺形成的膜厚为15μm的被剥离体层,所述条件为:120℃维持30分钟→升温→180℃维持20分钟→升温→240℃维持20分钟→升温→300℃维持20分钟→升温→400℃维持20分钟→升温→450℃维持60分钟(在任意升温中,升温速度均为10℃/分钟)。
<<交叉切割试验II>>
针对上述所得的具备被剥离体层及剥离层的基板,通过交叉切割试验II确认被剥离体层/剥离层之间的密合力。
与交叉切割试验I同样地进行交叉切割试验II。
将(1)显示出加热时的重量变化中的1%重量减少的温度(表2中,用“(1)”标注)、(2)波长1000nm处的折射率(表2中,用“(2)”标注)、(3)该(2)的折射率与双折射率之差(表2中,用“(3)”标注)、(4)表面能(表2中,用“(4)”标注。其中,单位为dyne/cm)、被剥离体层中使用的聚酰亚胺前体、以及交叉切割试验I和II的结果示于表2。
表2
(1) | (2) | (3) | (4) | 聚酰亚胺 | 试验I | 试验II | |
实施例1 | 530℃ | 1.80 | 0.21 | 52.1 | P5 | 5B | AA |
实施例2 | 550℃ | 1.79 | 0.20 | 50.6 | P5 | 5B | AA |
实施例3 | 570℃ | 1.78 | 0.23 | 52.5 | P5 | 5B | AA |
实施例4 | 500℃ | 1.76 | 0.19 | 50.9 | P5 | 5B | AA |
实施例5 | 530℃ | 1.75 | 0.22 | 53.8 | P5 | 5B | AA |
比较例1 | 560℃ | 1.81 | 0.21 | 48.8 | P5 | AA | -** |
比较例2 | 440℃ | 1.59 | -* | 36.2 | P5 | 5B | 5B |
比较例3 | 560℃ | 1.81 | 0.21 | 48.8 | P1 | AA | -** |
*:比较例2的双折射率无法测定。
**:比较例1及比较例3的交叉切割试验II由于剥离层与基板的密合性低,所以无法测定。
由表2可得知下述结论。对于实施例1~5的剥离层而言,根据试验I的结果为5B,可知剥离层未从基板剥落,而另一方面,根据试验II的结果为AA,可知仅被剥离体层从剥离层剥离。总而言之,可知由本发明的剥离层用组合物形成的剥离层可带来所期望的剥离结果。
另一方面,对于比较例1及比较例3而言,由于试验I的结果为AA,所以可知剥离层从基板上剥离。总而言之,可知比较例1及比较例3不能得到所期望的剥离结果。另外,对于比较例2而言,根据试验I及试验II均为5B,可知在剥离层与基板的界面处、及剥离层与被剥离体层的界面处均未发生剥离,不能得到所期望的剥离结果。
Claims (6)
1.组合物,其为用于形成在紧邻于玻璃基板的上方设置的剥离层的组合物,所述组合物含有:
(A)芳香族聚酰亚胺及/或芳香族聚酰亚胺前体;和
(B)酰胺类溶剂,
所述组合物中,来自所述(A)的芳香族聚酰亚胺满足下述条件(1)~(4):
(1)加热时的重量变化中的1%重量减少的温度为500℃以上;
(2)波长1000nm处的折射率为1.7以上;
(3)波长1000nm处的折射率与双折射率之差为0.15以上;及
(4)表面能为40dyne/cm以上。
2.如权利要求1所述的组合物,其中,所述(A)成分是使用选自由对苯二胺及三联苯二胺组成的组中的至少一种二胺成分制造的。
3.如权利要求2所述的组合物,其中,对苯二胺及/或三联苯二胺的量为全部二胺成分100摩尔%中的70摩尔%以上。
4.如权利要求1~3中任一项所述的组合物,其中,所述(A)成分是使用具有第一骨架的芳香族二胺制造的,所述第一骨架为选自由联苯骨架、咪唑骨架及噁唑骨架组成的组中的至少一种。
5.如权利要求1~4中任一项所述的组合物,其中,所述(A)成分是使用具有第二骨架的酸二酐制造的,所述第二骨架为选自由苯骨架、萘骨架及联苯骨架组成的组中的至少一种。
6.如权利要求1~5中任一项所述的组合物,其中,所述(B)成分为下述式(I)表示的溶剂、及/或式(II)表示的溶剂,式(I)及(II)中,R1及R2各自独立地表示碳原子数1~4的烷基,h表示自然数,
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WO2015152121A1 (ja) | 2015-10-08 |
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