CN104540884A - 透明聚酰亚胺基底以及制备该基底的方法 - Google Patents
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Abstract
本发明公开了一种透明聚酰亚胺基底,包括:透明聚酰亚胺膜;和氧化硅层,该氧化硅层形成于所述透明聚酰亚胺膜的一面或两面上,且包含氧化硅。
Description
技术领域
本发明涉及一种透明聚酰亚胺基底及其制备方法,所述基底可以用作柔性显示器基底。
背景技术
近来,电子设备如柔性OLED、彩色EPD、塑料LCD、TSP和OPV等,已经作为可以容易地扭曲和弯曲的下一代显示器而吸引了大量注意。为了制备这种可以容易地进行扭曲和弯曲的柔性显示器,需要新型的基底来替代传统的玻璃基底。这种新型基底必须具有足够的耐化学性、耐热性和透光性以保护显示器的部件。另外,这种新型基底必须耐用于在制备显示器过程中所进行的清洗、剥离和蚀刻等中使用的溶剂,而且需要耐高温。
多种塑料基底正在被考虑作为柔性显示器基底的备选项。在这些塑料基底中,透明聚酰亚胺膜被认为是主要的备选项。
为了改善被考虑作为柔性显示器基底的透明聚酰亚胺膜的耐溶剂性,通常,采用在透明聚酰亚胺膜上形成丙烯酸类或环氧类有机固化膜的方法。然而,这种有机固化膜的问题在于,其耐热性在超过200℃的高温或在300℃以上的高温下会发生劣化。
发明内容
技术问题
因此,本发明已完成以解决上述问题,本发明的一个目的是提供一种具有优异的耐溶剂性和高耐热性的透明聚酰亚胺基底。
本发明的另一个目的是提供一种制备具有优异的耐溶剂性和高耐热性的透明聚酰亚胺基底的方法。
技术方案
为了实现上述目的,本发明的一方面提供一种透明聚酰亚胺基底,包括:透明聚酰亚胺膜;和氧化硅层,该氧化硅层形成于所述透明聚酰亚胺膜的一面或两面上,并且该氧化硅层包含具有由下式1表示的单元结构的氧化硅:
[式1]
其中,m和n各自独立地为0至10的整数。
本发明的另一方面提供一种制备透明聚酰亚胺基底的方法,包括如下步骤:将含有聚硅氮烷的溶液涂布在透明聚酰亚胺膜的一面或两面上,然后干燥该溶液,形成聚硅氮烷层;以及使所述聚硅氮烷层固化。
有益效果
本发明提供了一种具有优异的耐溶剂性和高耐热性的透明聚酰亚胺基底。
并且,本发明提供了一种制备具有优异的耐溶剂性和高耐热性的透明聚酰亚胺基底的方法。
具体实施方式
本发明提供一种透明聚酰亚胺基底,包括:透明聚酰亚胺膜;和氧化硅层,该氧化硅层形成于所述透明聚酰亚胺膜的一面或两面上,并且该氧化硅层包含具有由下式1表示的单元结构的氧化硅:
[式1]
其中,m和n各自独立地为0至10的整数。
也就是说,在透明聚酰亚胺膜的一面或两面上形成氧化硅层,由此改善透明聚酰亚胺膜的耐溶剂性和耐热性。在式1中,当n或m为0时,氧化硅层为纯无机材料,从而使得透明聚酰亚胺膜的耐溶剂性和耐热性最大化。如有必要,为了改善透明聚酰亚胺基底的柔性,优选式1中的n或m为1以上的自然数,使得氧化硅具有合适的烷基链长度。然而,当n或m为10以上时,氧化硅具有疏水性,因而造成涂布溶液的结块。
此处,所述氧化硅层的厚度可以为0.3~2.0μm。为了赋予透明聚酰亚胺膜以合适的耐溶剂性,优选氧化硅层的厚度为0.3μm以上;而为了防止透明基底的柔性劣化,优选其厚度为2.0μm以下。
就此而言,根据本发明提供的含有氧化硅层的透明聚酰亚胺基底具有达到如下程度的优异耐溶剂性:即使在显示器的制备中,将所述基底在室温下浸渍于用于蚀刻工艺等的有机溶剂(例如TMAH(四甲基氢氧化铵)、KOH(氢氧化钾)、NMP(N-甲基吡咯烷酮)、MEK(甲基乙基酮)或MASO2(含有16.9~20.3%HCL的溶剂,由Dongwoo Finechem Co.,Ltd.生产)等)中约30分钟时,通过肉眼也不会观察到其外观的改变。
并且,本发明的透明聚酰亚胺基底在其表面上含有氧化硅层,使得其表面粗糙度(RMS)可以降低至5nm以下,从而带来了使透明聚酰亚胺基底平整的益处。由于这种益处,在形成电极或TFT的过程中,载流子可以容易地进行迁移。
另外,本发明提供一种制备透明聚酰亚胺基底的方法,包括如下步骤:将含有聚硅氮烷的溶液涂布在透明聚酰亚胺膜的一面或两面上,然后干燥该溶液,形成聚硅氮烷层;以及使所述聚硅氮烷层固化。
也就是说,根据本发明的制备透明聚酰亚胺基底的方法的特征在于,将透明聚酰亚胺膜用聚硅氮烷进行涂布然后固化,使得式2的单元结构中存在的-NH-基团被转化为式1的单元结构中存在的-O-基团,由此形成氧化硅层。
作为常规的在膜上形成无机层的沉积方法,PECVD或溅射的不利之处在于,由于真空设备的局限而使沉积面积受到了限制。然而,根据本发明的用溶液涂布膜然后固化该溶液而形成无机层的方法的有利之处在于,该方法可以采用简单的浇铸过程来进行,因此在大面积和连续的工艺中非常有效。
此处,所述聚硅氮烷可以包含由下式2表示的单元结构:
[式2]
其中,m和n各自独立地为0至10的整数。
并且,所述聚硅氮烷的重均分子量可以为1,000~5,000。
在式1中,m和n可以根据最终形成的氧化硅层的特性来合适地选择。并且,当聚硅氮烷的重均分子量为1,000以上时,可以确保更高的耐溶剂性和耐热性;而当其重均分子量为5,000以下时,可以确保均匀的涂布性能。
所述将含有聚硅氮烷的溶液涂布在透明聚酰亚胺膜的一面或两面上的过程,可以采用选自喷涂、棒涂、旋涂和浸涂等中的任一种来进行。
此处,通过将式2的单元结构中存在的-NH-基团转化为式1的单元结构中存在的-O-基团而形成氧化硅层的过程,可以采用热固化或UV固化来进行。
此处,热固化的有利之处在于,可以容易地形成使聚硅氮烷易于转化为氧化硅膜所必需的网络结构,因而能够增强氧化硅膜的薄膜特性,从而极大地改善透明聚酰亚胺基底的耐化学性和耐热性,但不利之处在于加工温度必须提高至200~300℃。同时,UV固化的有利之处在于可以通过用UV照射聚硅氮烷而在短时间内将聚硅氮烷转化为氧化硅膜,但不利之处在于,由于与热固化相比网络结构只是部分形成,因而不能使氧化硅膜的薄膜特性得到增强。因此,热固化和UV固化可以根据最终产品的物理性质或工艺的优势与劣势来选择性地采用。
当选择热固化时,可以在200~300℃的温度下对聚硅氮烷进行热处理。在这种情况下,当热处理温度为200℃以上时,可以减少使聚硅氮烷形成氧化硅层所需的固化时间;而当热处理温度为300℃以下时,可以防止由透明聚酰亚胺膜与氧化硅层之间的热膨胀系数差异所导致的翘曲。
当选择UV固化时,在涂布含有聚硅氮烷的溶液的步骤中,所述含有聚硅氮烷的溶液还可以包含UV固化剂;以及,在使聚硅氮烷层固化的步骤中,可以通过用具有312nm或365nm的短波长的UV,以1500~4000J/m2的辐射强度照射所述聚硅氮烷层而使该聚硅氮烷层固化。
此处,所述UV固化剂可以包括选自安息香醚(benzoin ether)光引发剂、二苯甲酮光引发剂以及它们的混合物的任一种。
下文中,将参照以下实施例详细地描述本发明。
<比较例1>
提供表面完全未经处理的透明聚酰亚胺膜作为比较例1。
<实施例1>
将由式2表示(其中m和n为0)且分子量为约2,000的聚硅氮烷以2wt%的浓度溶解在DBE(二丁基醚)中,制得含有聚硅氮烷的溶液。接着,将该含有聚硅氮烷的溶液通过金属线(wire)涂布在比较例1的透明聚酰亚胺膜的一面上,然后在约80℃的温度下干燥,形成厚度为1μm的聚硅氮烷膜。
其后,将上述制备的聚硅氮烷膜在室温下放置约5分钟,然后在约250℃的温度下热固化,形成氧化硅层。
<实施例2>
以与实施例1中所述的相同方式形成氧化硅层,不同之处在于:使用由式2表示(其中m为0且n为1,或者m和n为1)且分子量为约3,000的聚硅氮烷。
<实施例3>
以与实施例1中所述的相同方式形成氧化硅层,不同之处在于:将含有聚硅氮烷的溶液涂布在所述透明聚酰亚胺膜的两面上。
<实施例4>
以与实施例2中所述的相同方式形成氧化硅层,不同之处在于:将含有聚硅氮烷的溶液涂布在所述透明聚酰亚胺膜的两面上。
<实施例5>
将由式2表示(其中m和n为0)且分子量为约2,000的聚硅氮烷以2wt%的浓度溶解在DBE(二丁基醚)中,制得第一溶液。接着,将UV固化剂加入然后溶解在所述第一溶液中,制得第二溶液。然后,将该第二溶液通过金属线涂布在比较例1的透明聚酰亚胺膜的一面上,然后在约80℃的温度下干燥,形成厚度为1μm的聚硅氮烷膜。
其后,使用UV固化单元,用具有312nm或365nm的短波长的UV以27W/m2的辐射强度照射上述制备的聚硅氮烷膜60秒,制得含有氧化硅层的无色透明聚酰亚胺膜。
如下进行实施例1至4和比较例1中制备的无色透明聚酰亚胺膜的耐溶剂性和其它物理性质的测量。
[物理性质的测量]
采用以下方法测量上述聚酰亚胺膜的物理性质,其结果在下表1中给出。
耐溶剂性
在室温下将各个透明聚酰亚胺膜分别浸渍在表1中给出的有机溶剂中30分钟后,对它们的耐溶剂性进行评价。在用肉眼观察各个透明聚酰亚胺膜的情况下,当其外观不改变且在浸渍试验前与浸渍试验后的RMS之差小于1nm时,其耐溶剂性由◎表示。此外,在用肉眼观察各个透明聚酰亚胺膜的情况下,当其外观不改变且在浸渍试验前与浸渍试验后的RMS之差为1nm以上时,其耐溶剂性由○表示。并且,在用肉眼观察各个透明聚酰亚胺膜的情况下,当各个透明聚酰亚胺膜变白和浑浊或者出现斑点时,其耐溶剂性由×表示。其结果示于下表1中。
平均光学透射率(%)
使用分光计(CU-3700D,由Konica Minolta Corp.制造),测量各个透明聚酰亚胺膜在350~700nm波长下的平均光学透射率。
黄度指数
使用分光计(CU-3700D,由Konica Minolta Corp.制造),测量各个透明聚酰亚胺膜的黄度指数。
热膨胀系数(CTE)(ppm/℃)
使用热分析仪(TA Instrument Q-400),测量各个透明聚酰亚胺膜在50~250℃下的热膨胀系数(CTE)(ppm/℃)。
透氧率(毫升/平方厘米*天)
使用氧气渗透仪(MOCON/US/Ox-Tran 2-61),测量各个透明聚酰亚胺膜的透氧率。
表面粗糙度(RMS)(nm)
使用XE100AFM,测量各个透明聚酰亚胺膜在20×20μm中的表面粗糙度。
粘合性
按照ASTM D3359,通过用胶带贴膜100次来测量各个透明聚酰亚胺膜的粘合性。
耐热性
将各个透明聚酰亚胺膜充分干燥以去除水分,在300℃的氮气气氛下放置于热风烘箱中24小时,然后测量其重量变化率。在这种情况下,当其重量变化率小于1%时,其耐热性表示为优异。并且,当其重量变化率为1%以上时,其耐热性表示为较差。
[表1]
类别 | IPA | TMAH | KOH | NMP | MEK | MASO2 |
实施例1 | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ |
实施例2 | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ |
实施例3 | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ |
实施例4 | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ |
比较例1 | ◎ | ○ | × | × | × | ○ |
[表2]
如上表1中所给出的,实施例1至4和比较例1的透明聚酰亚胺膜的耐溶剂性试验显示,实施例1至4的透明聚酰亚胺膜对全部溶剂的耐溶剂性均表示为◎,也就是说,评价表明,当用肉眼观察各个透明聚酰亚胺膜时,其外观不改变,并且在浸渍试验前后的RMS之差小于1nm。然而,除一些溶剂外,比较例1的透明聚酰亚胺膜对各种溶剂的耐溶剂性被评价为较差。
另外,由于实施例1至4的各个透明聚酰亚胺膜在其表面上含有氧化硅层,因此其平均光学透射率、黄度指数、CTE、透氧率、表面粗糙度(RMS)和粘合性与表面完全未经处理的比较例1的透明聚酰亚胺膜的这些性质相比,获得了改善。
虽然已经出于示例性的目的而公开了本发明的优选实施方案,但本领域的技术人员将会理解,在不背离如所附权利要求公开的本发明的范围和精神的情况下,可以进行各种修改、添加和替换。
Claims (10)
1.一种透明聚酰亚胺基底,包括:
透明聚酰亚胺膜;和
氧化硅层,该氧化硅层形成于所述透明聚酰亚胺膜的一面或两面上,并且该氧化硅层包含具有由下式1表示的单元结构的氧化硅:
其中,m和n各自独立地为0至10的整数。
2.根据权利要求1所述的透明聚酰亚胺基底,其中,所述氧化硅层的厚度为0.3~2.0μm。
3.根据权利要求1所述的透明聚酰亚胺基底,其中,所述氧化硅层的表面粗糙度(RMS)为5nm以下。
4.一种制备透明聚酰亚胺基底的方法,包括如下步骤:
将含有聚硅氮烷的溶液涂布在透明聚酰亚胺膜的一面或两面上,然后干燥该溶液,形成聚硅氮烷层;以及
使所述聚硅氮烷层固化。
5.根据权利要求4所述的方法,其中,所述聚硅氮烷包含由下式2表示的单元结构:
其中,m和n各自独立地为0至10的整数。
6.根据权利要求5所述的方法,其中,所述聚硅氮烷的重均分子量为1,000~5,000。
7.根据权利要求4所述的方法,其中,所述聚硅氮烷层的厚度为0.3~2.0μm。
8.根据权利要求4所述的方法,其中,在所述使聚硅氮烷层固化的步骤中,所述聚硅氮烷层通过在200~300℃的温度下进行热处理而被热固化。
9.根据权利要求4所述的方法,其中,在所述涂布含有聚硅氮烷的溶液的步骤中,所述含有聚硅氮烷的溶液还包含UV固化剂,
并且,在所述使聚硅氮烷层固化的步骤中,所述聚硅氮烷层通过用具有312nm或365nm的短波长的UV,以1500~4000J/m2的辐射强度照射而被固化。
10.根据权利要求9所述的方法,其中,所述UV固化剂包括选自安息香醚光引发剂、二苯甲酮光引发剂以及它们的混合物的任一种。
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JP5768652B2 (ja) * | 2011-10-24 | 2015-08-26 | コニカミノルタ株式会社 | バリアーフィルムの製造方法 |
CN103917364A (zh) * | 2011-11-11 | 2014-07-09 | 三菱瓦斯化学株式会社 | 透明耐热阻气性薄膜的制造方法 |
-
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Non-Patent Citations (1)
Title |
---|
LONGFEI HU ET AL.: "A polysilazane coating peotecting polyimide from atomic oxygen and vacuum ultraviolet radiation erosion", 《SURFACE & COATINGS TECHNOLOGY》 * |
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