CN111148811B - 用于可折叠显示器的粘合剂组合物以及包含其的可折叠显示器 - Google Patents
用于可折叠显示器的粘合剂组合物以及包含其的可折叠显示器 Download PDFInfo
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- CN111148811B CN111148811B CN201880061987.4A CN201880061987A CN111148811B CN 111148811 B CN111148811 B CN 111148811B CN 201880061987 A CN201880061987 A CN 201880061987A CN 111148811 B CN111148811 B CN 111148811B
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Abstract
本说明书提供了用于可折叠显示器的粘合剂组合物。
Description
技术领域
本申请要求于2017年12月11日向韩国知识产权局提交的韩国专利申请第10-2017-0169351号的优先权和权益,其全部内容通过引用并入本文。
本申请涉及用于可折叠显示器的粘合剂组合物、以及包含其的可折叠显示器。
背景技术
随着显示器相关技术的最新发展,已经研究和开发了在使用阶段可变形(例如折叠、卷成卷状或如同橡胶带一样拉伸)的显示装置。这些显示器可以变形成不同形状,因此,可以满足对于使用阶段的较大显示器和为了便携性的较小显示器的两者的需求。
可以响应于用户需求或者根据使用显示装置的情况的需要将可变形的显示装置变形成不同形状,以及将其变形成预先设定的形状。因此,需要识别显示器的变形形状,并且需要响应于所识别的形状来控制显示装置。
同时,可变形的显示装置具有以下问题:显示装置的各构造均可能由于变形而受到损坏,因此,这样的显示装置的各构造均需要满足折叠可靠性和稳定性。
此外,用于可折叠显示器的粘合剂需要满足折叠可靠性和现有的粘合剂特性,并且需要在-40℃至60℃的全球温度变化条件下满足驱动条件。
另外,为了满足折叠可靠性条件,需要满足粘合剂的流变行为条件,并且在粘合剂的流变特性中,储能模量值需要大于或等于104Pa且小于或等于106Pa,在室温和高温下折叠100,000次之后不应存在分层。
然而,现有的用于可折叠显示器的粘合剂组合物具有的问题在于,即使在满足这样的折叠可靠性条件时,也会当在-20℃下(这是允许实际折叠测试的条件中最严苛的条件)进行动态折叠测试时发生分层和面板破裂。
发明内容
技术问题
本说明书旨在提供用于可折叠显示器的粘合剂组合物、以及包含其的可折叠显示器。
技术方案
本说明书的一个实施方案提供了用于可折叠显示器的粘合剂组合物,其包含:包含(甲基)丙烯酸烷基酯和具有可交联官能团的单体的聚合物、和交联剂,
其中固化之后粘合剂组合物与聚酰亚胺膜的粘合强度在室温下大于或等于500gf/in且小于或等于5,000gf/in,
在-20℃和1%应变的条件下测量的固化之后的粘合剂组合物的储能模量大于或等于50,000Pa且小于或等于250,000Pa,
在-20℃和12%应变的条件下开始应变时的初始应力大于或等于5,000Pa且小于或等于20,000Pa,
在-20℃和12%应变的条件下应变10分钟之后测量的最终应力大于或等于1,000Pa且小于或等于10,000Pa,
由(最终应变)/(最初施加的应变)×100%定义的应变恢复大于或等于70%且小于或等于90%,
最初施加的应变为12%应变,以及
最终应变是基于移除最初施加的应变的时间在20分钟之后的恢复的应变。
本说明书的另一个实施方案提供了包含上述用于可折叠显示器的粘合剂组合物或其固化材料的粘合剂层。
本说明书的又一个实施方案提供了可折叠显示器,其包括:背板基底;设置在背板基底的一个表面上的根据本申请的粘合剂层;和设置在粘合剂层的与背板基底接触的表面的相反的表面上的显示面板。
有益效果
根据本说明书的一个实施方案的用于可折叠显示器的粘合剂组合物具有如下优点:在保持现有的用于可折叠显示器的粘合剂组合物的特性例如在室温和高温下的可靠性条件和粘附特性的同时,满足在进行折叠测试时即使在-20℃下也不引起例如分层和破裂的问题的可靠性条件。
使用根据本申请的一个实施方案的用于可折叠显示器的粘合剂组合物制备的粘合剂层可以用于可折叠显示器中,并且包括根据本申请的粘合剂层的可折叠显示器具有优异的耐久性的特性,原因是即使在极低的温度(-20℃)下也不会在折叠和恢复期间发生粘合剂的分层和破裂。
附图说明
图1示出了根据本说明书的一个实施方案的应力松弛测试中的应变和应力变化和恢复的速率。
具体实施方式
在本说明书中,一个构件被放置在另一构件“上”的描述不仅包括一个构件邻接另一构件的情况,而且还包括在这两个构件之间存在另一构件的情况。
在本说明书中,特定部分“包括”某些构成要素的描述意指能够进一步包括其他构成要素,并且除非特别相反地说明,否则不排除其他构成要素。
在下文中,将更详细地描述本说明书。
本申请涉及用于可折叠显示器的粘合剂组合物和包含其的可折叠显示器。
本说明书的一个实施方案提供了用于可折叠显示器的粘合剂组合物,其包含:包含(甲基)丙烯酸烷基酯和具有可交联官能团的单体的聚合物、和交联剂,其中固化之后粘合剂组合物与聚酰亚胺膜的粘合强度在室温下大于或等于500gf/in且小于或等于5,000gf/in,在-20℃和1%应变的条件下测量的固化之后的粘合剂组合物的储能模量大于或等于50,000Pa且小于或等于250,000Pa,在-20℃和12%应变的条件下开始应变时的初始应力大于或等于5,000Pa且小于或等于20,000Pa,在-20℃和12%应变的条件下应变10分钟之后测量的最终应力大于或等于1,000Pa且小于或等于10,000Pa,由(最终应变)/(最初施加的应变)×100%定义的应变恢复大于或等于70%且小于或等于90%,最初施加的应变为12%应变,以及最终应变是基于移除最初施加的应变的时间在20分钟之后的恢复的应变。
本说明书的另一个实施方案提供了包含上述用于可折叠显示器的粘合剂组合物或其固化材料的粘合剂层。
这样的粘合剂组合物可以例如被固化以形成粘合剂层,并且粘合剂层可以包括在可折叠显示器内以用于例如附接显示面板与覆盖玻璃的应用中。
在本说明书中,术语“可折叠显示器”可以意指设计成如同纸一样重复折叠和展开并且具有曲率半径为5mm或更小的折叠部分的柔性显示器。
与现有的粘合剂不同,用于可折叠显示器的粘合剂需要满足弯曲可靠性,并且为了具有这样的优异的弯曲可靠性,需要在宽的温度范围内满足可靠性。
当在低温(例如,-20℃)下以及在室温和高温范围内进行折叠测试时,根据本说明书的一个实施方案的粘合剂组合物不会引起例如分层和破裂的问题,并因此具有用于可折叠显示器中的适当的特性。
根据本说明书的一个实施方案,固化之后粘合剂组合物与聚酰亚胺膜的粘合强度在室温下可以大于或等于500gf/in且小于或等于5,000gf/in,更优选地大于或等于800gf/in且小于或等于2,000gf/in,以及甚至更优选地大于或等于950gf/in且小于或等于1800gf/in。
通过使固化之后粘合剂组合物与聚酰亚胺膜的粘合强度在室温下满足上述范围,在随后折叠包括包含粘合剂组合物的粘合剂层的可折叠显示器时,在粘合剂层与可折叠显示装置的界面处不会发生分层。
根据本说明书的一个实施方案,粘合剂组合物的固化可以包括在120℃的温度条件下干燥和固化3分钟之后在40℃下老化3天。
根据本说明书的一个实施方案,室温可以意指25℃。
根据本说明书的一个实施方案,聚酰亚胺膜可以使用可商购的产品,并且可以具体地为GF200(SKC-Kolon PI),然而,聚酰亚胺膜不限于此。
根据本说明书的一个实施方案,粘合强度是测量180°剥离粘合强度的值,并且可以通过将粘合剂层合在被粘物上并使所得物静置一天来测量。作为测量装置,使用质构分析仪(Stable Micro Systems),并且可以以0.3mpm的剥离速率和1英寸的样品宽度来测量粘合剂的粘合强度。
在本说明书中,术语“储能模量”意指公知的“动态储能模量”。换言之,在向弹性体施加正弦型剪切应变时,在粘弹性材料中应力似乎以中间形式延迟,并且在数学上表示时,这意指一个构成要素处于同一相位,而另一构成要素则延迟了π/2,并且在本文中,可以将处于同一相位的部分,即,由于弹性而无损失地存储的能量称为“动态储能模量”或“储能模量”。
根据本说明书的一个实施方案,可以例如使用先进的流变膨胀系统(TAInstruments Inc.)根据手册在1%应变条件下测量储能模量值。
在本说明书的一个实施方案中,在-20℃和1%应变的条件下测量的固化之后的粘合剂组合物的储能模量可以大于或等于50,000Pa且小于或等于250,000Pa,优选地大于或等于70,000Pa且小于或等于250,000Pa,以及更优选地大于或等于150,000Pa且小于或等于250,000Pa。
通过满足上述范围,包含粘合剂组合物的粘合剂层的硬度是适当的,并且因此,粘合剂层的特性优异,并且在折叠时可能产生的应力可以被释放,并且因此,使与粘合剂层粘合的层上的损坏最小化。另外,通过具有上述范围的储能模量,通过具有反复折叠和展开时的优异回弹性而获得不留下膜折叠痕迹的特性。
换言之,当在-20℃和1%应变的条件下测量的固化之后的粘合剂组合物的储能模量大于上述范围时,粘合剂变得太硬而损害了粘合剂的特性,这可能因无法释放折叠时产生的应力而使粘附层损坏。当储能模量小于上述范围时,由于回弹性不足而在折叠之后出现可见的膜折叠痕迹的问题。
在本说明书中,术语应变恢复由(最终恢复应变%)/(最初施加的应变12%)×100%定义,并且可以通过设计粘合剂的分子量、交联度和组成来调节应变恢复。
在本说明书中,使用DMA(TA Instruments Inc.)作为测量应力和应变的装置,并在-20℃,12%应变600秒,并恢复1200秒的条件下使用尺寸为约宽度:6mm,厚度:1mm和长度:10mm至15mm的样品进行测量。
在将样品在较长边的方向上通过应变拉伸12%并保持特定的一段时间时,通过拉伸应变而增加的应力缓慢地降低。
换言之,当拉伸了12%时看到的最大应力意指初始应力,并且应力开始减小,并在特定的一段时间(600秒)之后保持而没有较大变化。如上保持的应力意指最终应力。
图1示出了应变和应力随时间的变化。如图1中所示,当以12%应变拉伸样品试样时的初始的最大应力为初始应力,并且特定的一段时间之后的应力意指最终应力。
当随后移除施加的应力时,经拉伸的样品缩小并开始恢复至其原始状态,并且在使样品静置足够的一段时间(1,200秒)以避免进一步缩小之后测量最终应变。
在本申请的一个实施方案中的由(最终应变)/(最初施加的应变)×100%定义的应变恢复中,最初施加的应变为12%应变,并且最终应变意指基于移除最初施加的应变的时间在20分钟之后的恢复的应变。
基于移除最初施加的应变的时间在20分钟之后的恢复的应变意指,在将移除最初施加的应变12%的时间调节为零点之后,在20分钟之后的恢复的应变。
例如,当粘合剂组合物的固化材料以12%应变变化并且从移除外力的时间起恢复20分钟之后测量的应变为10%时,最初施加的应变为12%,并且最终应变为10%,并且在本文中,应变恢复可以意指约83.33%。
在本说明书的一个实施方案中,最初施加的应变可以为12%,并且可以满足±5%的范围。
在本说明书的一个实施方案中,最终应变可以大于或等于5%且小于或等于11%,优选地大于或等于7%且小于或等于11%,以及更优选地大于或等于8%且小于或等于10%。
另外,评估当以2.5R折叠时产生的应变为约12%的情况下进行测量,并且将在折叠之后立即存在于粘合剂中的应力、和折叠时在存储时保留的应力模拟为初始应力和最终应力。将展开时粘合剂对整个折叠结构的恢复作出贡献的程度模拟为恢复率。
根据本说明书的一个实施方案,初始应力可以大于或等于5,000Pa且小于或等于20,000Pa,以及更优选地大于或等于10,000Pa且小于或等于18,000Pa。
根据本说明书的一个实施方案,在-20℃和12%应变的条件下应变10分钟之后测量的最终应力可以大于或等于1,000Pa且小于或等于10,000Pa,以及更优选地大于或等于5,000Pa且小于或等于8,000Pa。
在本说明书的一个实施方案中,应变恢复可以为70%至90%,优选地为75%至90%,以及更优选地为80%至90%。
根据本说明书的一个实施方案,当应变恢复满足70%至90%的范围时,折叠时产生的应力被释放并最小化,并且获得了保持粘合强度的内聚强度,因此,在低温、室温和高温下均获得了优异的折叠特性。
另一方面,当应变恢复为90%或更大时,折叠时返回的力较大,这可能在反复地折叠时引起显示面板或者覆盖窗侧的硬涂层上的裂纹,或者由于较大的应力而引起界面分层。
另外,当应变恢复小于70%时,内聚强度太低,因此,粘合强度变得非常低,或者由于粘合剂内聚失败在折叠时在界面处可能出现气泡或分层。
在本申请的一个实施方案中提供的用于可折叠显示器的粘合剂组合物中,基于100重量份的聚合物,(甲基)丙烯酸烷基酯的含量为50重量份至99重量份,以及具有可交联官能团的单体的含量为1重量份至50重量份。
在本说明书的一个实施方案中,基于100重量份的聚合物,(甲基)丙烯酸烷基酯的含量可以为50重量份至99重量份,优选地为60重量份至99重量份,以及更优选地为80重量份至99重量份。
在本说明书的一个实施方案中,基于100重量份的聚合物,具有可交联官能团的单体的含量可以为1重量份至50重量份,优选地为1重量份至25重量份,以及更优选地为1重量份至5重量份。
在本申请的一个实施方案中提供的用于可折叠显示器的粘合剂组合物中,基于100重量份的聚合物,交联剂的含量在0.001重量份至5重量份的范围内。
在另一个实施方案中,基于100重量份的聚合物,交联剂的含量可以为0.001重量份至5重量份,优选地为0.01重量份至1重量份,以及更优选地为0.01重量份至0.4重量份。
通过使交联剂含量满足上述范围,在-20℃的温度下可以获得目标储能模量。
在根据本申请的一个实施方案的用于可折叠显示器的粘合剂组合物中,通过以如上的特定含量包含特定材料可以满足储能模量和应力恢复的范围,并且因为即使在极低的温度(-20℃)下折叠和恢复时也不会发生粘合剂分层和破裂,因此包括粘合剂层的可折叠显示器具有优异耐久性的特性。
在本说明书中,除非另外定义,否则术语“重量份”意指各组分之间的重量比。
根据本说明书的一个实施方案的粘合剂组合物可以为(甲基)丙烯酸烷基酯与具有可交联官能团的单体的聚合物。
根据本说明书的一个实施方案,(甲基)丙烯酸烷基酯可以为具有有1至20个碳原子的烷基的(甲基)丙烯酸烷基酯,并且其实例可以包括(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸2-乙基丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十二烷基酯、(甲基)丙烯酸十三烷基酯、(甲基)丙烯酸十四烷基酯、(甲基)丙烯酸十八烷基酯或(甲基)丙烯酸异冰片酯等,但不限于此。
在本文中,术语“(甲基)丙烯酸酯”意指丙烯酸酯或甲基丙烯酸酯。
根据本说明书的一个实施方案,可以没有特别限制地选择具有可交联官能团的单体,只要其能够向由与(甲基)丙烯酸烷基酯单体的聚合产生的聚合物提供可交联官能团即可。
根据本说明书的一个实施方案,可交联官能团可以为选自羟基、异氰酸酯基、缩水甘油基、环氧基、胺基和羧基中的任一者或更多者。
具有羟基的单体的实例可以包括(甲基)丙烯酸羟烷基酯,例如(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丙酯、(甲基)丙烯酸4-羟丁酯、(甲基)丙烯酸6-羟己酯或(甲基)丙烯酸8-羟辛酯;(甲基)丙烯酸羟基聚亚烷基二醇酯,例如(甲基)丙烯酸羟基聚乙二醇酯或(甲基)丙烯酸羟基聚丙二醇酯;等等,但不限于此。
具有羧基的单体的实例可以包括丙烯酸β-羧基乙酯、(甲基)丙烯酸、2-(甲基)丙烯酰氧基乙酸、3-(甲基)丙烯酰氧基丙酸、4-(甲基)丙烯酰氧基丁酸、丙烯酸二聚体、衣康酸、马来酸、马来酸酐等,但不限于此。
具有胺基的单体的实例可以包括(甲基)丙烯酸2-氨基乙酯、(甲基)丙烯酸3-氨基丙酯、(甲基)丙烯酸N,N-二甲基氨基乙酯、(甲基)丙烯酸N,N-二甲基氨基丙酯等,但是不限于此。
在具有各种可交联官能团的单体中,可以考虑丙烯酸类聚合物的目标玻璃化转变温度或者与稍后描述的交联剂的反应性来选择适当的类型。
根据本说明书的一个实施方案,可交联官能团可以为羧基。
根据本说明书的一个实施方案,可以没有限制地选择可交联官能团,只要其能够例如在约50℃至300℃的范围内的温度下与稍后描述的交联剂产生交联反应即可。
根据本说明书的一个实施方案的粘合剂组合物可以具有在-150℃至0℃的范围内的玻璃化转变温度(Tg)。在这样的玻璃化转变温度(Tg)的范围内,可以提供在宽温度范围内具有低的储能模量变化率的粘合剂组合物。
根据本说明书的一个实施方案,粘合剂组合物可以具有在-150℃至0℃、-100℃至-10℃或-90℃至-20℃的范围内的玻璃化转变温度(Tg)。
在本说明书的一个实施方案中提供的用于可折叠显示器的粘合剂组合物中,用于可折叠显示器的粘合剂组合物的玻璃化转变温度(Tg)高于或等于-50℃且低于或等于-20℃。
在另一个实施方案中,用于可折叠显示器的粘合剂组合物的玻璃化转变温度(Tg)可以高于或等于-50℃且低于或等于-20℃,优选地高于或等于-40℃且低于或等于-25℃,以及更优选地高于或等于-40℃且低于或等于-30℃。
通过使用于可折叠显示器的粘合剂组合物的玻璃化转变温度满足上述范围,随后的包含该粘合剂组合物的粘合剂层具有优异的硬度和粘附性,并且在可折叠显示器的低温驱动下具有优异折叠特性的特性。
作为本说明书中的玻璃化转变温度,使用旋转流变仪ARES-G2测量在-60℃至80℃的温度范围和1Hz的频率下的G’和tanδ值。当以5℃/分钟的升温速率升温时,tanδ在G’迅速降低的部分中形成峰,并且可以将tanδ的最高点出现处的温度识别为Tg值。
用于可折叠显示器的粘合剂组合物的玻璃化转变温度可以意指包含粘合剂组合物中所含的所有单体组分的整个粘合剂组合物的玻璃化转变温度。
根据本说明书的另一个实施方案,聚合物可以具有在5,000至3,000,000的范围内的重均分子量。
在本说明书中,术语重均分子量可以意指通过凝胶渗透色谱法(GPC)测量的对于标准聚苯乙烯的换算因数,并且除非另外特别定义,否则特定聚合物的分子量可以意指该聚合物的重均分子量。在另一个实施方案中,聚合物可以具有在100,000至2,500,000、500,000至2,200,000或1,500,000至2,000,000的范围内的重均分子量。另外,多分散度(PDI)可以为2.0至3.9。
根据本说明书的一个实施方案,粘合剂组合物包含交联剂。
根据本说明书的另一个实施方案,通过包含具有能够与聚合物中包含的可交联官能团反应的官能团的交联剂,可以提供具有用于可折叠显示器的适当的特性的粘合剂组合物。
具体地,交联剂可以包含选自以下中的任一个或更多个官能团:烷氧基硅烷基、羧基、酸酐基、乙烯基醚基、胺基、羰基、异氰酸酯基、环氧基、氮丙啶基、碳二亚胺基和唑啉基。官能团的类型可以根据聚合物中包含的可交联官能团的类型或交联结构的实现机理而变化。
包含羧基的交联剂的实例可以包括芳族二羧酸,例如邻苯二甲酸、间苯二甲酸、对苯二甲酸、1,4-二甲基对苯二甲酸、1,3-二甲基间苯二甲酸、5-磺基-1,3-二甲基间苯二甲酸、4,4-联苯基二羧酸、1,4-萘二羧酸、2,6-萘二羧酸、降冰片烯二羧酸、二苯基甲烷-4,4’-二羧酸或苯基茚满二羧酸;芳族二羧酸酐,例如邻苯二甲酸酐、1,8-萘二羧酸酐或2,3-萘二羧酸酐;脂环族二羧酸,例如六氢邻苯二甲酸;脂环族二羧酸酐,例如六氢邻苯二甲酸酐、3-甲基-六氢邻苯二甲酸酐、4-甲基-六氢邻苯二甲酸酐或1,2-环己烷二羧酸酐;或脂族二羧酸,例如草酸、丙二酸、琥珀酸、己二酸、癸二酸、壬二酸、辛二酸、马来酸、氯代马来酸、富马酸、十二烷二酸、庚二酸、柠康酸、戊二酸或衣康酸。
包含酸酐基团的交联剂的实例可以包括均苯四酸酐、二苯甲酮四羧酸二酐、联苯基四羧酸二酐、氧基二邻苯二甲酸二酐、二苯砜四羧酸二酐、二苯硫醚四羧酸二酐、丁烷四羧酸二酐、苝四羧酸二酐、萘四羧酸二酐等。
包含乙烯基醚基的交联剂的实例可以包括乙二醇二乙烯基醚、二乙二醇二乙烯基醚、三乙二醇二乙烯基醚、四乙二醇二乙烯基醚、季戊四醇二乙烯基醚、丙二醇二乙烯基醚、二丙二醇二乙烯基醚、三丙二醇二乙烯基醚、新戊二醇二乙烯基醚、1,4-丁二醇二乙烯基醚、1,6-己二醇二乙烯基醚、甘油二乙烯基醚、三羟甲基丙烷二乙烯基醚、1,4-二羟基环己烷二乙烯基醚、1,4-二羟基甲基环己烷二乙烯基醚、对苯二酚二乙烯基醚、环氧乙烷改性的对苯二酚二乙烯基醚、环氧乙烷改性的间苯二酚二乙烯基醚、环氧乙烷改性的双酚A二乙烯基醚、环氧乙烷改性的双酚S二乙烯基醚、甘油三乙烯基醚、山梨糖醇四乙烯基醚、三羟甲基丙烷三乙烯基醚、季戊四醇三乙烯基醚、季戊四醇四乙烯基醚、二季戊四醇六乙烯基醚、二季戊四醇聚乙烯基醚、二三羟甲基丙烷四乙烯基醚、二三羟甲基丙烷聚乙烯基醚等。
包含胺基的交联剂的实例可以包括脂族二胺,例如乙二胺或六亚甲基二胺;脂环族二胺,例如4,4’-二氨基-3,3’-二甲基二环己基甲烷、4,4’-二氨基-3,3’-二甲基二环己基、二氨基环己烷或异佛尔酮二胺;芳族二胺,例如二甲苯二胺等。
包含异氰酸酯基的交联剂的实例可以包括芳族多异氰酸酯,例如1,3-亚苯基二异氰酸酯、4,4’-二苯基二异氰酸酯、1,4-亚苯基二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、2,4-亚甲苯基二异氰酸酯、2,6-亚甲苯基二异氰酸酯、4,4’-甲苯胺二异氰酸酯、2,4,6-三异氰酸酯甲苯、1,3,5-三异氰酸酯苯、联茴香胺二异氰酸酯、4,4’-二苯基醚二异氰酸酯、4,4’,4”-三苯基甲烷三异氰酸酯、ω,ω’-二异氰酸酯-1,3-二甲基苯、ω,ω’-二异氰酸酯-1,4-二甲基苯、ω,ω’-二异氰酸酯-1,4-二乙基苯、1,4-四甲基亚二甲苯二异氰酸酯、1,3-四甲基二甲苯二异氰酸酯、亚二甲苯二异氰酸酯;脂族多异氰酸酯,例如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、2,3-亚丁基二异氰酸酯、1,3-亚丁基二异氰酸酯、十二亚甲基二异氰酸酯或2,4,4-三甲基六亚甲基二异氰酸酯;脂环族多异氰酸酯,例如3-异氰酸酯甲基-3,5,5-三甲基环己基异氰酸酯、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、甲基-2,4-环己烷二异氰酸酯、甲基-2,6-环己烷二异氰酸酯、4,4’-亚甲基双(环己基异氰酸酯)或1,4-双(异氰酸酯甲基)环己烷等,或者上述多异氰酸酯中的一者或更多者与多元醇的反应物。
包含环氧基的交联剂的实例可以包括乙二醇二缩水甘油基醚、三缩水甘油基醚、三羟甲基丙烷三缩水甘油基醚、N,N,N’,N’-四缩水甘油基-1,3-二甲苯二胺、甘油二缩水甘油基醚等。
根据本说明书的一个实施方案,粘合剂组合物可以通过包含交联剂与聚合物中包含的可交联官能团进行交联反应。
根据本说明书的一个实施方案,除了如上所述的交联剂和聚合物之外,粘合剂组合物还可以包含已知的另外的组分,例如抗静电剂、粘附提供树脂、固化剂、紫外线稳定剂、抗氧化剂、着色剂、增强剂、填料、消泡剂、表面活性剂或增塑剂。
根据本说明书的一个实施方案,粘合剂组合物具有适用于可折叠显示器的弯曲可靠性,并且例如可以用于例如附接可折叠显示器中的面板、覆盖玻璃等的应用中。
本说明书的另一个实施方案可以提供包含上述用于可折叠显示器的粘合剂组合物或其固化材料的粘合剂层。
在本说明书的一个实施方案中提供的粘合剂层中,在粘合剂层的一个表面或两个表面上还包括离型膜。
离型膜是用于保护非常薄的粘合剂层的层,并且是指附接在粘合剂层的一个表面或两个表面上的透明层,并且可以使用具有优异的机械强度、热稳定性、水分阻挡特性、各向同性等的膜。例如,可以使用基于乙酸酯的(例如三乙酰基纤维素(TAC))、基于聚酯的、基于聚醚砜的、基于聚碳酸酯的、基于聚酰胺的、基于聚酰亚胺的、基于聚烯烃的、基于环烯烃的、基于聚氨酯的和基于丙烯酸类的树脂膜等,然而,离型膜不限于此,只要其是可商购的经有机硅处理的离型膜即可。
本说明书的另一个实施方案可以提供包括上述粘合剂层的可折叠显示器。
可折叠显示器的其他具体构造例如是在韩国专利申请特许公开第2015-0138450号等中已知的,并且本申请可以没有限制地包括这样的已知的可折叠显示器构造。
在本说明书的一个实施方案中,提供了可折叠显示器,其包括:背板基底;设置在背板基底的一个表面上的根据本申请的粘合剂层;和设置在粘合剂层的与背板基底接触的表面的相反的表面上的显示面板。
在本说明书的一个实施方案中提供的可折叠显示器中,背板基底包含选自以下中的任一者或更多者:聚对苯二甲酸乙二醇酯(PET)、聚酯、聚碳酸酯(PC)、聚酰亚胺(PI)、聚萘二甲酸乙二醇酯(PEN)、聚醚醚酮(PEEK)、聚芳酯(PAR)、聚环烯烃(PCO)、聚降冰片烯、聚醚砜(PES)和环烯烃聚合物(COP)。
在另一个实施方案中,背板基底可以是聚酰亚胺(PI)基底。
在本说明书的一个实施方案中提供的可折叠显示器还包括在背板基底的与粘合剂层接触的表面的相反的表面上的支撑体。
支撑体可以通过粘合剂层粘附至背板基底,并且作为粘合剂层,可以使用根据本申请的粘合剂层。
在本说明书的一个实施方案中,还可以在显示面板的与粘合剂层接触的表面的相反的表面上包括偏光板,并且偏光板和显示面板可以通过根据本申请的粘合剂层粘附。
另外,还可以在偏光板的与显示面板接触的表面的相反的表面上包括覆盖窗,并且偏光板和覆盖窗可以通过根据本申请的粘合剂层粘附。
在本说明书中,可折叠显示器包括显示面板、和附接在显示面板的背面上的折叠调节装置,并且折叠调节体可以包括弹性板、设置在弹性板的背面上的链板、以及分别设置在链板的上表面或下表面上的上板和下板。
发明实施方式
在下文中,将参照实施例详细描述本说明书。然而,根据本说明书的实施例可以被修改为各种其他形式,并且本说明书的范围不应被解释为限于以下描述的实施例。提供本说明书的实施例以向本领域普通技术人员更充分地描述本说明书。
在本说明书中,以以下方式评估粘合剂组合物的特性。
储能模量的测量
在将实施例和比较例中制备的各粘合剂组合物涂覆在离型膜之间之后,将所得物切成15cm×25cm的尺寸,并且在除去一个表面上的离型膜之后,将所得物层合数次以具有约1mm的厚度。
随后,将层合体切割成直径为8mm的圆形形状,用玻璃压缩,并静置过夜以增强各层之间的界面处的润湿,并除去在层合期间产生的气泡以制备样品。然后,将样品放置在平行板上,并且在调节间隙之后,将法线&扭矩设定为零,检查法向力稳定,并测量储能模量。
(1)测量装置及测量条件
测量装置:设置有强制对流烘箱的ARES-G2,TA Instruments Inc.
(2)测量条件:
几何:8mm平行板
间距:约1mm
测试类型:动态应变频率扫描
应变=0.1[%]
温度:-20℃
频率:1Hz
实施例1
向其中回流有氮气并配备有冷却装置以易于控制温度的1L反应器中,基于100重量份的(甲基)丙烯酸烷基酯和具有可交联官能团的单体,引入98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)。随后,基于100重量份的(甲基)丙烯酸烷基酯和具有可交联官能团的单体,向其中引入150重量份的乙酸乙酯(EAc)作为溶剂,并且在用氮气吹扫反应器60分钟以除去氧气之后,在将温度保持在60℃的同时,向其中引入0.02重量份的偶氮二异丁腈(AIBN)(反应引发剂)以引发反应。将反应了约1小时的反应材料用乙酸乙酯(EAc)稀释,以制备具有约2,000,000的分子量的丙烯酸类聚合物。相对于100重量份的丙烯酸类聚合物,将0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam YoungInk&Paint MFG.Co.,Ltd.制造)(交联剂)混合以制备粘合剂组合物。
在SKC的有机硅离型膜(RF12N)上,将粘合剂组合物(C1)涂覆至约25μm的厚度并干燥,并且在其上涂覆轻剥离离型膜(RF02N)之后,使所得物在40℃下固化2天以形成粘合剂层。
实施例2
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入59重量份的丙烯酸乙基己酯(EHA)、40重量份的丙烯酸丁酯(BA)和1重量份的丙烯酸β-羧基乙酯(B-CEA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
实施例3
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入97.5重量份的丙烯酸丁酯(BA)和2.5重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
实施例4
以与实施例1中相同的方式形成粘合剂层,不同之处在于,以0.1重量份使用N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)。
比较例1
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物,并且相对于100重量份的丙烯酸类聚合物,以0.3重量份引入交联剂。
比较例2
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入19重量份的丙烯酸乙基己酯(EHA)、80重量份的丙烯酸丁酯(BA)和1重量份的丙烯酸β-羧基乙酯(B-CEA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
比较例3
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物,并且相对于100重量份的丙烯酸类聚合物,以0.5重量份引入交联剂。
比较例4
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入94重量份的丙烯酸乙基己酯(EHA)和6重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
比较例5
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入98重量份的丙烯酸丁酯(BA)和2重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
比较例6
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入60重量份的丙烯酸丁酯(BA)、39重量份的丙烯酸乙基己酯(EHA)和1重量份的B-CEA代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
比较例7
以与比较例6中相同的方式形成粘合剂层,不同之处在于,使用0.1重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由SamYoung Ink&Paint MFG.Co.,Ltd.制造)(交联剂)。
比较例8
以与比较例6中相同的方式形成粘合剂层,不同之处在于,使用0.2重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由SamYoung Ink&Paint MFG.Co.,Ltd.制造)(交联剂)。
比较例9
以与比较例6中相同的方式形成粘合剂层,不同之处在于,使用0.3重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由SamYoung Ink&Paint MFG.Co.,Ltd.制造)(交联剂)。
比较例10
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入98重量份的丙烯酸丁酯(BA)和2重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物,并且使用0.1重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&PaintMFG.Co.,Ltd.制造)(交联剂)。
比较例11
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入99重量份的丙烯酸丁酯(BA)和1重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物,并且使用0.5重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&PaintMFG.Co.,Ltd.制造)(交联剂)。
比较例12
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入99重量份的丙烯酸丁酯(BA)和1重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物,并且使用1重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.03重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)。
比较例13
以与比较例10中相同的方式形成粘合剂层,不同之处在于,使用0.3重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由Sam Young Ink&Paint MFG.Co.,Ltd.制造)(交联剂)代替0.1重量份的N,N,N’,N’-四缩水甘油基-间二甲苯二胺(BXX-5240,由SamYoung Ink&Paint MFG.Co.,Ltd.制造)(交联剂)
比较例14
以与实施例1中相同的方式形成粘合剂层,不同之处在于,通过引入94重量份的丙烯酸丁酯(BA)和6重量份的丙烯酸(AA)代替98重量份的丙烯酸乙基己酯(EHA)和2重量份的丙烯酸(AA)来制备丙烯酸类聚合物。
在使根据实施例和比较例的各组合物固化之后,使用动态机械分析仪(DMA)(TAInstruments Inc.)在-20℃,12%应变600秒并且恢复1200秒的条件下,由尺寸为约宽度:6mm,厚度:1mm并且长度:10mm至15mm的粘合剂层样品测量粘合剂层的初始应力、应变10分钟之后的最终应力、和应变恢复,并使用配备有强制对流烘箱的ARES-G2(TA instruments装置)测量在-20℃下的储能模量。
换言之,在将粘合剂层样品在较长边的方向上以12%应变拉伸并保持特定的一段时间(600秒)时,应力开始降低并且在特定的一段时间(600秒)之后保持而没有较大变化,并且当应力值如上所述保持时测量最终应力。
另外,对于基于移除最初施加的应变(12%)的时间在20分钟(1200秒)之后恢复的应变,在将移除最初施加的应变12%的时间调节为零点之后,测量20分钟之后的恢复的应变(最终应变),并由此计算应变恢复。
另外,初始应力、最终应力、储能模量、应变恢复、粘合强度以及在-20℃下的动态折叠测试期间的面板破裂或分层的次数描述在下表1中。
[表1]
根据表1的比较例1、3、5、8至14看出,当应变恢复太高时,折叠时产生的应力无法适当地释放,并且在面板的每一层中积聚的应力更快地引起问题。相反,确定当应变恢复太低时,内聚强度不足,并且难以作为粘合剂使用。
如表1的比较例2至14中看出的,当初始应力高时,对于每次反复的折叠和展开,应力被传递到每一层,由于积聚的疲劳(fatigue)而在面板上引起问题。
如表1的比较例1中确定的,当折叠之后释放和保留的最终应力较高时,即使在低的初始应力的情况下,积聚在面板上的应力也会在静态折叠测试以及动态折叠测试中引起问题。
根据表1的比较例4、5和10至14看出,当储能模量太高时,在-20℃下在折叠时产生的应力增加,这在折叠中是不利的。
Claims (10)
1.一种用于可折叠显示器的粘合剂组合物,包含:
包含(甲基)丙烯酸烷基酯和具有可交联官能团的单体的聚合物;和
交联剂,
其中所述(甲基)丙烯酸烷基酯包括(甲基)丙烯酸乙基己酯,
其中基于100重量份的所述聚合物,所述(甲基)丙烯酸乙基己酯的含量为50重量份至99重量份,
其中基于100重量份的所述聚合物,所述具有可交联官能团的单体的含量为1重量份至5重量份,
其中基于100重量份的所述聚合物,所述交联剂的含量在0.01重量份至0.1重量份的范围内,其中所述交联剂具有选自以下中的任一个或更多个官能团:烷氧基硅烷基、羧基、酸酐基、乙烯基醚基、胺基、羰基、异氰酸酯基、环氧基、氮丙啶基、碳二亚胺基和唑啉基,
其中所述粘合剂组合物具有高于或等于-50℃且低于或等于-20℃的玻璃化转变温度Tg,
其中所述聚合物具有在500,000至3,000,000的范围内的重均分子量,
其中固化之后所述粘合剂组合物与聚酰亚胺膜的粘合强度在室温下大于或等于500gf/in且小于或等于5,000gf/in;
在-20℃和1%应变的条件下测量的固化之后的所述粘合剂组合物的储能模量大于或等于50,000Pa且小于或等于250,000Pa;
在-20℃和12%应变的条件下开始应变时的初始应力大于或等于5,000Pa且小于或等于20,000Pa;
在-20℃和12%应变的条件下应变10分钟之后测量的最终应力大于或等于1,000Pa且小于或等于10,000Pa;
由(最终应变)/(最初施加的应变)×100%定义的应变恢复大于或等于70%且小于或等于90%;
所述最初施加的应变为12%应变;以及
所述最终应变是基于移除所述最初施加的应变的时间在20分钟之后的恢复的应变。
2.根据权利要求1所述的用于可折叠显示器的粘合剂组合物,其中所述可交联官能团包括选自羟基、异氰酸酯基、缩水甘油基、环氧基、胺基和羧基中的任一者或更多者。
3.根据权利要求1所述的用于可折叠显示器的粘合剂组合物,还包含选自以下中的一者或更多者:抗静电剂、粘附提供树脂、固化剂、紫外线稳定剂、抗氧化剂、着色剂、增强剂、填料、消泡剂、表面活性剂和增塑剂。
4.一种粘合剂层,包含根据权利要求1至3中任一项所述的用于可折叠显示器的粘合剂组合物或其固化材料。
5.根据权利要求4所述的粘合剂层,还包括在所述粘合剂层的一个表面或两个表面上的离型膜。
6.一种可折叠显示器,包括:
背板基底;
设置在所述背板基底的一个表面上的根据权利要求4所述的粘合剂层;和
设置在所述粘合剂层的与所述背板基底接触的表面的相反的表面上的显示面板。
7.根据权利要求6所述的可折叠显示器,还包括在所述背板基底的与所述粘合剂层接触的表面的相反的表面上的支撑体。
8.根据权利要求6所述的可折叠显示器,其中所述背板基底包含选自以下中的任一者或更多者:聚酯、聚碳酸酯PC、聚酰亚胺PI、聚醚醚酮PEEK、聚降冰片烯、聚醚砜PES和环烯烃聚合物COP。
9.根据权利要求6所述的可折叠显示器,其中所述背板基底包含选自以下中的任一者或更多者:聚碳酸酯PC、聚酰亚胺PI、聚醚醚酮PEEK、聚芳酯PAR、聚降冰片烯、聚醚砜PES和环烯烃聚合物COP。
10.根据权利要求6所述的可折叠显示器,其中所述背板基底包含选自以下中的任一者或更多者:聚对苯二甲酸乙二醇酯PET、聚碳酸酯PC、聚酰亚胺PI、聚萘二甲酸乙二醇酯PEN、聚醚醚酮PEEK、聚降冰片烯、聚醚砜PES和环烯烃聚合物COP。
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