CN113372926A - 包含可聚合化合物的液晶组合物和液晶显示器件 - Google Patents
包含可聚合化合物的液晶组合物和液晶显示器件 Download PDFInfo
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- CN113372926A CN113372926A CN202010158210.9A CN202010158210A CN113372926A CN 113372926 A CN113372926 A CN 113372926A CN 202010158210 A CN202010158210 A CN 202010158210A CN 113372926 A CN113372926 A CN 113372926A
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Abstract
本发明提供了一种包含可聚合化合物的液晶组合物及其液晶显示器件,其中所述包含可聚合化合物的液晶组合物包含至少一种通式I的化合物、至少一种通式II的化合物以及至少一种通式M的化合物。与现有技术相比,本发明的液晶组合物具有较高的电压保持率(尤其是UV光照后的电压保持率表现优异),同时还具有较低的聚合物层表面粗糙度、较快的聚合速度、较小的聚合物残留量和较好的预倾斜角稳定性;使得包含其的液晶显示器件在具有较好的电压稳定性和较快的响应速度的情况下,能够有效降低或防止液晶显示器件出现“烧屏”、“图像粘滞”、“碎亮点”、“显示不均”等问题,具有较高的实用价值。
Description
技术领域
本发明涉及液晶领域,具体涉及含有可聚合化合物的液晶组合物以及其液晶显示器件。
背景技术
液晶显示器(Liquid Crystal Display,LCD)因其体积小、重量轻、功耗低且显示质量优异而获得了飞速发展,特别是在便携式电子信息产品中获得广泛的应用。根据显示模式的类型,可以将液晶显示器分为PC(phase change,相变)、TN(twist nematic,扭曲向列)、STN(super twisted nematic,超扭曲向列)、ECB(electrically controlledbirefringence,电控双折射)、OCB(optically compensated bend,光学补偿弯曲)、IPS(in-plane switching,共面转变)、FFS(fringe field switching,边缘场切换)、VA(vertical alignment,垂直配向) 和PSA(polymer stable alignment,聚合物稳定配向)等类型。
PSA模式是将少量(如0.3wt%,较典型<1wt%)的一种或更多种可聚合化合物添加到液晶组合物中,并在将液晶组合物填充入液晶盒之后在电极之间施加电压或不施加电压的情况下,使其在液晶分子具有初始取向的状态下原位聚合或交联(通常通过UV光聚合),从而固定液晶分子的取向。聚合在液晶组合物显示出液晶相的温度下进行(通常在室温下进行)。已证实将可聚合的液晶化合物添加到液晶组合物中是特别适宜的,因为其在单元内形成的聚合物结构可以很好地控制液晶分子的倾斜角,且PSA型液晶显示元件还具有高速响应性和高对比度的效果。
因此,PSA型液晶显示元件被不断开发,并且PSA原理也被用在各种传统的液晶显示器中,诸如已知的PSA-VA、PSA-OCB、PSA-IPS、PSA-FFS和PSA-TN型液晶显示器。在PSA型液晶显示器中,含有可聚合化合物的液晶组合物位于两个基板之间,各基板均配备有电极结构,或者两个电极结构仅置于基板之一上。此外,两个基板中的任意一者或两者可以含有设置于基板或电极结构(若存在)上从而与液晶组合物接触的配向层,以诱发液晶组合物的初始配向。如常规的液晶显示器一样,PSA型液晶显示器能作为有源矩阵或无源矩阵显示器来操作。就有源矩阵显示器的情况而言,各个像素通常通过集成的非线性有源元件(如晶体管)来进行寻址,而就无源矩阵显示器的情况而言,各个像素通常根据现有技术中已知的多路传输方法来进行寻址。
将液晶组合物填充至显示器件中之后,液晶组合物中含有的可聚合化合物通常通过 UV光聚合进行原位聚合或交联,其中UV光聚合通过将液晶组合物暴露于UV辐射而实现,并且优选同时向电极结构施加电压。作为UV暴露的结果,经聚合或经交联的可聚合化合物与液晶组合物中的其他化合物出现相分离,并且在基板表面上形成聚合物层,在此处它们引起液晶分子相对于基板的预倾斜角。对于PSA-VA、PSA-OCB、PSA-FFS和 PSA-TN型液晶显示器,可聚合化合物的聚合优选在施加电压的情况下进行;对于PSA-IPS 型液晶显示器,施加或不施加电压皆可,优选不施加电压。
通常,PSA型液晶显示器的生产方法中的UV光聚合是通过两个步骤实现的。在第一步骤(以下称为“UV1步骤”)中,将液晶组合物暴露于由辐射源(以下称为“光源”)发射的UV辐射,同时向电极结构施加电压,以产生预倾斜角;在第二步骤(以下称为“UV2 步骤”)中,将液晶组合物暴露于UV照射,而不向电极结构施加电压,以确保在UV1步骤中未发生聚合的任何残余的可聚合化合物的能够彻底聚合。如上文所描述,彻底聚合是重要的,这是因为残余的未发生聚合的可聚合化合物可能导致不期望的效应,如显示器中降低的可靠性、降低的倾斜角稳定性或图像粘滞。此外,重要的是确保UV2步骤中的聚合在可接受的时间内完成,以使节拍时间显著地短于2h。此外,相较于UV1步骤,应当减小UV2步骤中的UV辐射强度,以避免或减小负面效应(如降低的可靠性或图像粘滞)。
然而,PSA型液晶显示元件也存在一些显示不良的情况(如图像保留等)。已有的研究显示,此类问题多是由杂质的存在以及液晶分子的取向的变化(预倾斜角的变化)造成的,而液晶分子的取向则是由可聚合化合物聚合后形成的聚合物网络控制的。如果构成聚合物网络的可聚合化合物的结构刚性不够,那么在PSA型液晶显示元件长时间连续显示同一图案时,聚合物网络的结构有可能发生变化,继而导致液晶分子的预倾斜角发生变化。因此,通常需要选取具有刚直结构的可聚合化合物。
现有技术中使用较广的是如下式(a)、式(b)的可聚合化合物:
其中,P1和P2均表示可聚合基团,通常是丙烯酸酯基或甲基丙烯酸酯基。
然而,随着技术的发展,液晶显示行业对LCD的显示质量要求更加严格,尤其是在TV行业中,TV尺寸普遍增大,LCD世代线也随之增大,大尺寸LCD面板的制作工艺难度也明显增加。因此,如何保证显示质量是亟待解决的问题。除了不断优化面板制造工艺外,对液晶材料的不断开发也是解决的手段之一,尤其对于PSA型液晶显示器来说,对可聚合化合物的各个方面的性能进行改善是研究的热点。
相比于现有的反应性单体(reactive monomer,RM),较优选的可聚合化合物应当在聚合期间在相同曝光时间下产生更小的预倾斜角或者在更短的UV曝光时间下产生相同的预倾斜角。使用这样的较优选的可聚合化合物可以节省显示器生产时间,从而加快显示器生产效率,降低成本。
目前,PSA型液晶显示器的生产中常见的问题是可聚合化合物的残留或去除以及预倾斜角的稳定性。在PSA型液晶显示器中,通过施加UV1辐射和UV2辐射使可聚合化合物聚合从而产生预倾斜角之后,少量始终未反应掉的可聚合化合物可能在显示器制成之后以不可控的方式聚合而影响显示器的品质,例如,残余的可聚合化合物会受到来自环境的 UV光或背光照明的影响而发生聚合,在接通的显示器区域内,经过多个寻址周期之后,预倾斜角会发生变化,透射率也会随之产生变化,而预倾斜角和透射率在未接通的区域中保持不变,从而产生“图像粘滞”效应。因此,期望的是在PSA型液晶显示器的生成期间,可聚合化合物尽可能完全地聚合,并且残余的可聚合化合物能够以受控的方式反应,而聚合速度越快,则越有利于实现该期望。此外,还期望在经过多个寻址周期之后,预倾斜角的变化小。
在PSA型液晶显示器的操作中观察到的另一个重要指标问题是预倾斜角的稳定性。如果形成的预倾斜角不够稳定,在显示器的使用过程中,预倾斜角会发生较明显变化从而造成显示画面不均、gamma漂移等问题。预倾斜角变化越大,PSA型液晶显示器的显示不均的问题越严重。因此,期望获得预倾斜角变化较小的可聚合化合物。
PSA型液晶显示器另外一个常见的问题是容易出现“碎亮点”,这是由于可聚合化合物在聚合过程中形成的部分聚合物颗粒过大造成的。此外,由于聚合物颗粒大小不均,导致聚合物的分布也不均匀,进而产生显示不均的问题。因此,期望获得能够形成颗粒尺寸较小且分布均匀的聚合物颗粒的可聚合化合物,从而改善“碎亮点”和显示不均的问题。
另一方面,应用于PSA型液晶显示器的聚合性液晶组合物的电压保持率也是信赖性的重要参数。聚合性液晶组合物应当具有较高的电压保持率(VHR),从而减少液晶显示器件烧屏、电压波动等问题。现有液晶显示器件常处在各种环境下并接触紫外线,而在 PSA型液晶显示器制作过程中和制作完成之后,也不可避免的暴露于UV辐射环境中,因此,聚合性液晶组合物必然需要具有较高的VHR。
另外,现有技术中的可聚合化合物通常具有高的熔点,并且在许多现有的常用液晶组合物中仅显示出有限的溶解性,常常会从液晶组合物中析出。此外,可聚合化合物具有自聚合的可能,这使得其在液晶组合物中的溶解性进一步变差。因此,通常需要在低温下引入溶有可聚合化合物的液晶组合物,以便降低可聚合化合物的自聚合的风险,这对可聚合化合物在液晶组合物中的溶解性提出更高的要求,尤其是其在低温下的溶解性。
因此,期待开发一种可以同时满足上述要求或至少满足上述要求中的一项的液晶组合物。
发明内容
发明目的:本发明的目的在于提供一种具有较高的电压保持率(初始,UV)、较低的聚合层表面粗糙度、较低的聚合物残留量、较快的聚合速度和较好的预倾斜角稳定性的包含可聚合化合物的液晶组合物。
本发明的目的还在于提供一种包含该液晶组合物的液晶显示器件。
技术方案:为了实现以上目的,本发明提供一种包含可聚合化合物的液晶组合物,该液晶组合物包含:
至少一种通式I的化合物
至少一种通式II的化合物
至少一种通式M的化合物
其中,
R和X1-X12各自独立地表示-H、卤素、-CN、-Sp2-P2、或含有1-12个碳原子的直链、支链或环状的烷基,其中含有1-12个碳原子的直链、支链或环状的烷基中的一个或不相邻的两个以上的-CH2-可以分别独立地被-CH=CH-、-C≡C-、-O-、-CO-、-CO-O-或-O-CO- 替代,一个或更多个-H可以分别独立地被-F或-Cl取代,其中,X1-X12中的至少一个表示 -Cl;
P1和P2各自独立地表示可聚合基团;
Sp1和Sp2各自独立地表示间隔基团或单键;
R1、R2、RM1和RM2各自独立地表示含有1-12个碳原子的直链或支链的烷基、 其中含有1-12个碳原子的直链或支链的烷基中的一个或不相邻的两个以上的-CH2-可以分别独立地被-CH=CH-、-C≡C-、-O-、-CO-、-CO-O-或-O-CO-替代;
Z1和Z2各自独立地表示-O-、-S-、-CO-、-CO-O-、-O-CO-、-O-CO-O-、-CH2O-、-OCH2-、-CH2S-、-SCH2-、-CF2O-、-OCF2-、-CF2S-、-SCF2-、-(CH2)n-、-CF2CH2-、-CH2CF2-、-(CF2)n-、 -CH=CH-、-CF=CF-、-CH=CF-、-CF=CH-、-C≡C-、-CH=CH-CO-O-、-O-CO-CH=CH-、 -CH2CH2-CO-O-、-O-CO-CH2CH2-、-CR1R2-或单键,其中,R1和R2各自独立地表示-H或含有1-12个碳原子的直链或支链的烷基,并且n表示1-4的整数;
ZM1和ZM2各自独立地表示单键、-CO-O-、-O-CO-、-CH2O-、-OCH2-、-C≡C-、-CH=CH-、-CH2CH2-或-(CH2)4-;
LN1和LN2各自独立地表示-F或-Cl;
LN3和LN4各自独立地表示-H、含有1-3个碳原子的烷基或卤素;
在本发明的一些实施方案中,优选地,R表示-Sp2-P2。
在本发明的一些实施方案中,优选地,a表示0或1。
在本发明的一些实施方案中,优选地,液晶组合物包含一种其中a=0的通式I的可聚合化合物和一种其中a=1的通式I的可聚合化合物。
在本发明的一些实施方案中,通式I的化合物选自由如下化合物组成的组:
其中,
X1-X12各自独立地表示-F、-Cl、-Sp2-P2、或含有1-5个碳原子的直链、支链或环状的烷基或烷氧基。
在本发明的一些实施方案中,优选地,Z1和Z2中至少一个表示单键;进一步优选地,Z1和Z2均表示单键。
相对于本发明的液晶组合物的总重量,通式I的化合物的重量百分比的下限值为0.001%、0.005%、0.01%、0.04%、0.08%、0.1%、0.2%、0.25%、0.28%、0.29%、0.3%、0.32%、0.33%、0.35%、0.5%、0.8%、1%、1.5%、2%、2.5%、3%或3.5%;相对于本发明的液晶组合物的总重量,通式I的化合物的重量百分比的上限值为5%、4%、3.5%、3%、2.5%、2%、1.5%、1%、0.8%、0.5%、0.35%、0.33%、0.32%、0.3%、0.29%、0.28%、0.25%、 0.2%、0.15%或0.1%。
在本发明的一些实施方案中,通式I的化合物占液晶组合物的重量百分比为0.001%-5%;优选地,通式I的化合物占液晶组合物的重量百分比为0.01%-2%;进一步优选地,通式I的化合物占所述液晶组合物的重量百分比为0.01%-1%。
本发明所涉及的可聚合基团是适用于聚合反应(例如,自由基或离子键聚合、加聚或缩聚)的基团,或者适用于聚合物主链上加成或缩合的基团。对于链式聚合,特别优选包含-C=C-或-C≡C-的可聚合基团,对于开环聚合,特别优选例如氧杂环丁烷或环氧基。
如本文所使用的,术语“间隔基团”是本领域技术人员已知的,并且描述于文献(例如,Pure Appl.Chem.2001,73(5),888和C.Tschierske,G.Pelzl,S.Diele,Angew.Chem.2004, 116,6340-6368)中。如本文所使用的,术语“间隔基团”表示在可聚合化合物中连接介晶基团和可聚合基团的柔性基团。典型的间隔基团例如为-(CH2)p1-、 -(CH2CH2O)q1-CH2CH2-、-(CH2CH2S)q1-CH2CH2-、-(CH2CH2NH)q1-CH2CH2-、 -CR0R00-(CH2)p1-或-(SiR0R00-O)p1-,其中,p1表示1-12的整数,q1表示1-3的整数,R0和 R00各自独立地表示-H或含有1-12个碳原子的直链、直链或环状的烷基。特别优选的间隔基团为-(CH2)p1-、-(CH2)p1-O-、-(CH2)p1-O-CO-、-(CH2)p1-CO-O-、-(CH2)p1-O-CO-O-或 -CR0R00-(CH2)p1-。
相对于本发明的液晶组合物的总重量,通式II的化合物的重量百分比的下限值为1%、 2%、4%、5%、5.5%、6%、8%、10%、12%、14%、16%、18%、20%、21.5%、22%、24%、 26%、28%、30%、35%、40%或45%;相对于本发明的液晶组合物的总重量,通式II的化合物的重量百分比的上限值为45%、44%、42%、40%、38%、36%、34%、32%、30%、28%、26%、24%、22%、21.5%、20%、18%、16%或15%。
在本发明的一些实施方案中,通式II的化合物占液晶组合物的重量百分比为1%-45%;优选地,通式II的化合物占液晶组合物的重量百分比为5%-45%;进一步优选地,通式II 的化合物占液晶组合物的重量百分比为5%-35%。
在本发明的一些实施方案中,通式II的化合物选自由如下化合物组成的组:
在本发明的一些实施方案中,优选地,R1和R2各自独立地表示含有1-10个碳原子的直链或支链的烷基、含有1-9个碳原子的直链或支链的烷氧基、或含有2-10个碳原子的直链或支链的烯基;进一步优选地,R1和R2各自独立地表示含有1-8个碳原子的直链或支链的烷基、含有1-7个碳原子的直链或支链的烷氧基、或含有2-8个碳原子的直链或支链的烯基;再进一步优选地,R1和R2各自独立地表示含有1-5个碳原子的直链或支链的烷基、含有1-4个碳原子的直链或支链的烷氧基、或含有2-5个碳原子的直链或支链的烯基。
在本发明的一些实施方案中,通式M的化合物选自由如下化合物组成的组:
相对于本发明的液晶组合物的总重量,通式M的化合物的重量百分比的下限值为1%、 2%、4%、6%、8%、10%、15%、20%、22%、24%、26%、28%、30%、35%、38.5%、40%、45%或50%;相对于本发明的液晶组合物的总重量,通式M的化合物的重量百分比的上限值为80%、75%、70%、65%、60%、58%、56%、55.5%、54%、52%、50%、45%、 40%、38.5%、35%、30%、28%、25.5%、25%、24%、22%或20%。
在本发明的一些实施方案中,通式M的化合物占液晶组合物的重量百分比为 1%-80%;优选地,通式M的化合物占液晶组合物的重量百分比为20%-60%;进一步优选地,通式M的化合物占液晶组合物的重量百分比为30%-50%。
关于通式M的化合物的含量,在需要保持本发明的液晶组合物的粘度较低且响应时间较短时,优选其下限值较高且上限值较高;进一步地,在需要保持本发明的液晶组合物的清亮点较高且温度稳定性良好时,优选其下限值较高且上限值较高;在为了将驱动电压保持为较低且介电各向异性的绝对值变大时,优选使其下限值变低且上限值变低。
在本发明的一些实施方案中,优选地,RM1和RM2各自独立地表示含有1-10个碳原子的直链或支链的烷基、含有1-9个碳原子的直链或支链的烷氧基、或含有2-10个碳原子的直链或支链的烯基;进一步优选地,RM1和RM2各自独立地表示含有1-8个碳原子的直链或支链的烷基、含有1-7个碳原子的直链或支链的烷氧基、或含有2-8个碳原子的直链或支链的烯基;再进一步优选地,RM1和RM2各自独立地表示含有1-5个碳原子的直链或支链的烷基、含有1-4个碳原子的直链或支链的烷氧基、或含有2-5个碳原子的直链或支链的烯基。
在本发明的一些实施方案中,RM1和RM2优选各自独立地为含有2-8个碳原子的直链状的烯基,进一步优选各自独立地为含有2-5个碳原子的直链状的烯基。
在本发明的一些实施方案中,优选地,RM1和RM2中的任意一者为含有2-5个碳原子的直链状的烯基,并且另一者为含有1-5个碳原子的直链状的烷基。
在本发明的一些实施方案中,RM1和RM2优选各自独立地为含有1-8个碳原子的直链状的烷基、或含有1-7个碳原子的直链状的烷氧基;进一步优选各自独立地为含有1-5个碳原子的直链状的烷基、或含有1-4个碳原子的直链状的烷氧基。
在本发明的一些实施方案中,优选地,RM1和RM2中的任意一者为含有1-5个碳原子的直链状的烷基,并且另一者为含有1-5个碳原子的直链状的烷基、或含有1-4个碳原子的直链状的烷氧基;进一步优选地,RM1和RM2两者均各自独立地为含有1-5个碳原子的直链状的烷基。
在重视可靠性的情形时,优选RM1和RM2均各自独立地为烷基;在重视降低化合物的挥发性的情形时,优选RM1和RM2均各自独立地为烷氧基;在重视粘度降低的情形时,优选RM1和RM2中至少一者为烯基。
本发明中的烯基优选自式(V1)至式(V9)中的任一者所表示的基团,特别优选为式(V1)、式(V2)、式(V8)或(V9)。式(V1)至式(V9)所表示的基团如下所示:
其中,*表示所键结的环结构中的碳原子。
本发明中的烯氧基优选自式(OV1)至式(OV9)中的任一者所表示的基团,特别优选为式(OV1)、式(OV2)、式(OV8)或(OV9)。式(OV1)至式(OV9)所表示的基团如下所示:
其中,*表示所键结的环结构中的碳原子。
在本发明的一些实施方案中,液晶组合物还包含至少一种通式III的化合物和至少一种通式IV的化合物:
其中,
R3、R4、R5和R6各自独立地表示含有1-12个碳原子的直链或支链的烷基、 其中含有1-12个碳原子的直链或支链的烷基中的一个或不相邻的两个以上的-CH2-可以分别独立地被-CH=CH-、-C≡C-、-O-、-CO-、-CO-O-或-O-CO-替代;
环和环各自独立地表示其中中的一个或更多个-CH2-可以被-O-替代,一个或更多个环中单键可以被双键替代,其中中的一个或更多个-H可以被-F、-Cl或-CN取代,一个或更多个环中 -CH=可以被-N=替代;
L1和L2各自独立地表示-F或-Cl;
L3和L4各自独立地表示-H、含有1-3个碳原子的烷基或卤素;
L5、L6、L7和L8各自独立地表示-H、-F或-Cl,其中,L5,L6,L7和L8中的至少两个表示-F或-Cl,并且,当L5、L6、L7和L8中的仅有两个表示-F或-Cl时,则-F或-Cl在同一个苯环上;
Z3和Z4各自独立地表示单键、-CO-O-、-O-CO-、-CH2O-、-OCH2-、-CH=CH-、-C≡C-、-CH2CH2-、-CF2CF2-、-(CH2)4-、-CF2O-或-OCF2-,其中,当Z3表示单键时,环为非芳香环;
n2表示0或1。
相对于本发明的液晶组合物的总重量,通式III的化合物的重量百分比的下限值为1%、 2%、4%、60%、8%、10%、15%、16%、18%、20%、22%、24%、26%、28%、28.5%、30%、34%、36%、38%、39.5%或40%;相对于本发明的液晶组合物的总重量,通式III 的化合物的重量百分比的上限值为50%、48%、46%、44%、42%、40%、39.5%、38%、 36%、34%、32%、30%、28.5%、28%、26%、24%、22%或20%。
在本发明的一些实施方案中,通式III的化合物占液晶组合物的重量百分比为1%-50%;优选地,通式III的化合物占液晶组合物的重量百分比为15%-50%;进一步优选地,通式III的化合物占液晶组合物的重量百分比为20%-45%。
在本发明的一些实施方案中,通式III的化合物选自由如下化合物组成的组:
相对于本发明的液晶组合物的总重量,通式IV的化合物的重量百分比的下限值为1%、2%、4%、5%、6%、8%、12%、14%、15%或16%;相对于本发明的液晶组合物的总重量,通式IV的化合物的重量百分比的上限值为20%、18%、16%、14%、12%、10%、 8%、6%或5%。
在本发明的一些实施方案中,通式IV的化合物占液晶组合物的重量百分比为1%-20%;优选地,通式IV的化合物占液晶组合物的重量百分比为1%-15%。
在本发明的一些实施方案中,通式IV的化合物选自由如下化合物组成的组:
除上述化合物以外,本发明的液晶组合物也可含有通常的向列型液晶、近晶型液晶、胆固醇型液晶、掺杂剂、抗氧化剂、紫外线吸收剂、红外线吸收剂、聚合性单体或光稳定剂等。
如下显示优选加入到根据本发明的液晶组合物中的可能的掺杂剂。
在本发明的一些实施方案中,掺杂剂占液晶组合物的重量百分比为0%-5%;优选地,掺杂剂占液晶组合物的重量百分比为0.01%-1%。
另外,本发明的液晶组合物中所使用的抗氧化剂、光稳定剂等添加剂优选以下物质:
其中,n表示1-12的正整数。
优选地,光稳定剂选自如下所示的光稳定剂:
在本发明的一些实施方案中,光稳定剂占液晶组合物的总重量百分比为0%-5%;优选地,光稳定剂占液晶组合物的总重量百分比为0.01%-1%;更优选地,光稳定剂占液晶组合物的总重量百分比为0.01%-0.1%。
即使在不存在聚合引发剂的情况下,本发明的含有可聚合化合物的液晶组合物也可以进行聚合,但为了促进聚合,其中还可以含有聚合引发剂。对于聚合引发剂,可以列举苯偶姻醚类、二苯甲酮类、苯乙酮类、苯偶酰缩酮类、酰基氧化膦类等。
本发明的液晶组合物可以用于通过液晶组合物中的可聚合化合物的聚合而被赋予液晶取向能力,并且利用液晶组合物中的双折射而控制液晶显示器件中的透射光量。
对于可聚合化合物的聚合方法,由于期望聚合快速进行,因此优选通过照射紫外线或电子束等活性能量线来进行聚合的方法。在使用紫外线时,可以使用偏振光源,也可以使用非偏振光源。另外,在将液晶组合物夹持在两个基板之间的状态下进行聚合时,至少照射面侧的基板相对于活性能量线必须具有适当的透明性。另外,也可以在光照射时采用掩模,仅使特定部分聚合,随后,通过改变电场、磁场或者温度等条件,使未聚合部分的取向状态产生变化,并且进一步照射活性能量线进行聚合。特别是在进行紫外线曝光时,优选在对液晶组合物施加电压的同时进行紫外线曝光。
紫外线或电子束等活性能量线照射时的温度优选为保持本发明液晶组合物的液晶状态的温度范围。优选在接近室温的温度(即,15~35℃)下进行聚合。对于产生紫外线的灯,可以使用金属卤化物灯、高压水银灯、超高压水银灯等。此外,对于所照射的紫外线的波长,优选照射波长在非液晶组合物的吸收波长区域之外的紫外线,优选根据需要阻断紫外线而使用。所照射的紫外线的强度优选为0.1mW/cm2-50 mW/cm2。在照射紫外线时,可以改变其强度,并且根据所照射的紫外线的强度适当选择照射紫外线的时间,优选10 s-600s。
如本文中使用的,术语“倾斜”和“倾斜角”将理解为液晶分子相对于液晶显示器件(优选为PSA型液晶显示器件)中液晶盒表面的倾斜配向。倾斜角表示液晶分子的纵向分子轴(液晶指向失)与液晶盒的外部板的表面之间形成的平均角度(<90°)。低值的倾斜角(即大的偏离90°的角)对应于大的倾斜。
本发明还提供包含本发明的通式I的化合物的液晶显示器件,优选地,PSA型液晶显示器件,更优选地,PS-VA、PS-OCB、PS-IPS、PS-FFS、PS-UB-FFS、PS-正性-VA或PS-TN 型液晶显示器件。
本发明还提供包含上述液晶组合物的液晶显示器件,优选地PSA型液晶显示器件,更优选地,PS-VA、PS-OCB、PS-IPS、PS-FFS、PS-UB-FFS、PS-正性-VA或PS-TN型液晶显示器件。
有益效果:
与现有技术相比,本发明提供的聚合性液晶组合物具有较高的电压保持率(尤其是 UV光照后的电压保持率表现优异),同时还具有较好的聚合层表面粗糙度、较低的聚合物残留量、较快的聚合速度和较好的预倾斜角稳定性,能够使液晶显示器件具有较好的电压稳定性和较快的响应速度,并能够有效降低或防止液晶显示器件出现“烧屏”、“图像粘滞”、“碎亮点”、“显示不均”等问题,具有较高的实际应用价值。
具体实施方式
以下将结合具体实施方案来说明本发明。需要说明的是,下面的实施例为本发明的示例,仅用来说明本发明,而不用来限制本发明。在不偏离本发明主旨或范围的情况下,可进行本发明构思内的其他组合和各种改良。
为便于表达,以下各实施例中,液晶化合物的基团结构用表1所列的代码表示:
表1液晶化合物的基团结构代码
以如下结构式的化合物为例:
该结构式如用表1所列代码表示,则可表达为:nCCGF,代码中的n表示左端烷基的C原子数,例如n为“3”,即表示该烷基为-C3H7;代码中的C代表环己烷基,G代表2- 氟-1,4-亚苯基,F代表氟取代基。
以下实施例中测试项目的简写代号如下:
Cp 清亮点(向列相-各向同性相的转变温度,℃)
Δn 光学各向异性(589nm,25℃)
Δε 介电各向异性(1KHz,25℃)
γ1 旋转粘度(mPa·s,25℃)
K11 展曲弹性常数
K33 弯曲弹性常数
Tc 低温相变点(℃)
Ra 粗糙度(nm)
ΔPTA 预倾斜角的稳定性(加电120h后预倾斜角变化)(°)
PTA 预倾斜角(°)
VHR(初始) 初始电压保持率(%)
VHR(UV) UV光照射后的电压保持率(%)
其中,
清亮点Cp:通过熔点仪测试获得。
Δn:在25℃使用阿贝折光仪在钠光灯(波长589nm)光源测试获得。
Δε=ε‖-ε⊥,其中,ε‖为平行于分子轴的介电常数,ε⊥为垂直于分子轴的介电常数,测试条件:25℃、1KHz和VA型测试盒(盒厚6μm)。
旋转黏度γ1:使用LCM-2型液晶物性评价***测试得到;测试条件:温度25℃,电压240V,盒厚20μm。
K11和K33:使用LCR仪和反平行摩擦盒测试液晶材料的C-V曲线,并且进行计算获得,测试条件:7μm反平行摩擦盒,V=0.1~20V。
Tc:将向列相液晶材料置于玻璃瓶中,分别在0℃、-10℃、-20℃、-30℃和-40℃的温度存储在冰箱中,然后观察第10天时向列相液晶材料的析晶情况。例如,样品在-20℃呈向列相而在-30℃变为晶体状态或近晶状态,则Tc为<-20℃。
表面粗糙度Ra:将含有可聚合化合物的液晶组合物经过UV光照聚合后,冲洗掉液晶分子,然后使用原子力显微镜(AFM)测试聚合后的聚合物层的形貌粗糙度。
预倾斜角PTA:使用晶体旋转法,将液晶灌注于VA型测试盒(盒厚3.5μm),施加电压(16V,60Hz),同时使用紫外光UV1进行照射,使得可聚合化合物发生聚合形成预倾斜角PTA1,然后向已形成预倾斜角PTA1的液晶组合物继续照射紫外光UV2,以消除PTA1状态下残留的可聚合物化合物,此时可聚合化合物形成的预倾斜角为PTA2。本发明通过比较UV1照射相同时间时形成的预倾斜角的大小(预倾斜角越小,聚合速度越快)或者比较形成相同预倾斜角所需时间(所需时间越段,聚合速度越快)来考察可聚合化合物的聚合速度。本发明通过施加不同照射时长的UV2后,洗脱出液晶测试盒中液晶,将洗脱出的液晶通过高效液相色谱(HPLC)测试可聚合化合物的浓度来考察可聚合化合物的残留量。
预倾斜角的稳定性ΔPTA:将预倾斜角PTA的测试中使用的测试盒经过UV1步骤和UV2步骤形成88±0.2°的预倾斜角后,向测试盒施加60Hz的SW波、20V的AC电压和2V的DC电压,在40℃且存在背光的环境下,经过固定的时间段后,测试测试盒的预倾斜角,ΔPTA(168h)=PTA(初始)-PTA(168h),ΔPTA(168h)越小,表示预倾斜角的稳定性越好。
VHR(初始):使用TOY06254型液晶物性评价***测试得到;测试条件:测试温度 60℃,测试电压5V,测试频率6Hz。
VHR(UV):使用TOY06254型液晶物性评价***测试得到;测试条件:在接近室温的温度(即,15-35℃)下进行聚合,紫外线的强度为0.1mW/cm2-50 mW/cm2,时间为2 h。
在以下的实施例中所采用的各成分,均可以通过公知的方法进行合成,或者通过商业途径获得。这些合成技术是常规的,所得到的各液晶化合物经测试符合电子类化合物标准。
按照以下实施例规定的各液晶组合物的配比制备液晶组合物。液晶组合物的制备是按照本领域的常规方法进行的,如采取加热、超声波、悬浮等方式按照比例混合制得。
表2可聚合化合物的结构及代码
对比例1-4和实施例1-8
按照表3中所列的各化合物及重量百分数配制成液晶组合物Host-1,如下表所示:
表3液晶组合物Host-1的配方及性能参数测试结果
将可聚合化合物RM-01、RM-02和RM-03加入100重量份数的液晶组合物Hsot-1中,作为对比例1-4,将可聚合化合物RM-1、RM-2、RM-3、RM-4、RM-5、RM-6和RM-7 加入100重量份数的液晶组合物Host-1中,作为实施例1-8,可聚合化合物的具体重量份数及相关性能测试结果如下表4所示:
由上表4数据可知,在母体液晶Host-1相同,仅可聚合化合物不同的情况下相较于对比例1-4(现有技术中的液晶组合物),本发明的液晶组合物具有更高的电压保持率,尤其是UV光照后的电压保持率表现优异,可靠性更高;本发明的液晶组合物中的可聚合化合物在形成聚合物层后还具有更低的表面粗糙度,均匀度更高;通过向液晶组合物施加不同时间的UV1后形成的PTA1的数据可以看出,本发明的液晶组合物的聚合速度更快,响应速度更快;在从聚合物残留的测试结果可以看出,本发明的液晶组合物可获得更低的聚合物残留量,响应速度更快;从预倾斜角稳定性测试结果可以看出,本发明的液晶组合物产生预倾斜角后,预倾斜角受电压驱动而产生的变化更小,具有更好的预倾斜角稳定性。
对比例5-6和实施例9-16
按照表5中所列的各化合物及重量百分数配制成液晶组合物Host-2,如下表所示:
表5液晶组合物Host-2的配方及性能参数测试结果
将可聚合化合物RM-01、RM-02和RM-03加入100重量份数的液晶组合物Host-2中,作为对比例5-7,将可聚合化合物RM-1、RM-2、RM-3、RM-4、RM-5、RM-6和RM-7 加入100重量份数的液晶组合物Host-2中,作为实施例9-16,可聚合化合物的具体重量份数及相关性能测试结果如下表6所示:
由上表6数据可知,在母体液晶Host-2相同,仅可聚合化合物不同的情况下,相较于对比例5-7(现有技术中的液晶组合物),本发明的液晶组合物具有更高的电压保持率,尤其是UV光照后的电压保持率表现优异,可靠性更高;本发明的液晶组合物中的可聚合化合物在形成聚合物层后还具有更低的表面粗糙度,均匀度更高;通过向液晶组合物施加不同时间的UV1后形成的PTA1的数据可以看出,本发明的液晶组合物的聚合速度更快,响应速度更快;在从聚合物残留的测试结果可以看出,本发明的液晶组合物可获得更低的聚合物残留量,响应速度更快;从预倾斜角稳定性测试结果可以看出,本发明的液晶组合物产生预倾斜角后,预倾斜角受电压驱动而产生的变化更小,具有更好的预倾斜角稳定性。
对比例8-10和实施例17-24
按照表7中所列的各化合物及重量百分数配制液晶组合物Host-3,如下表所示:
表7液晶组合物Host-3的配方及性能参数测试结果
将可聚合化合物RM-01、RM-02和RM-03加入100重量份数的液晶组合物Host-3中,作为对比例8-10,将可聚合化合物RM-1、RM-2、RM-3、RM-4、RM-5、RM-6和RM-7 加入100重量份数的液晶组合物Host-3中,作为实施例17-24,可聚合化合物的具体重量份数及相关性能测试结果如下表8所示:
由上表8数据可知,在母体液晶Host-3相同,仅可聚合化合物不同的情况下,相较于对比例8-10(现有技术中的液晶组合物),本发明的液晶组合物具有更高的电压保持率,尤其是UV光照后的电压保持率表现优异,可靠性更高;本发明的液晶组合物中的可聚合化合物在形成聚合物层后还具有更低的表面粗糙度,均匀度更高;通过向液晶组合物施加不同时间的UV1后形成的PTA1的数据可以看出,本发明的液晶组合物的聚合速度更快,响应速度更快;在从聚合物残留的测试结果可以看出,本发明的液晶组合物可获得更低的聚合物残留量,响应速度更快;从预倾斜角稳定性测试结果可以看出,本发明的液晶组合物产生预倾斜角后,预倾斜角受电压驱动而产生的变化更小,具有更好的预倾斜角稳定性。
综上,本发明提供的包含可聚合化合物的液晶组合物具有较高的电压保持率,尤其是 UV光照后的电压保持率表现优异,同时还具有较低的聚合物层表面粗糙度、较快的聚合速度、较小的聚合物残留量和较好的预倾斜角稳定性,使得包含其的液晶显示器件在具有较好的电压稳定性和较快的响应速度的情况下,能够有效降低或防止液晶显示器件出现“烧屏”、“图像粘滞”、“碎亮点”、“显示不均”等问题,具有较高的实用价值。
以上实施方式只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人了解本发明内容并加以实施,并不能以此限制本发明的保护范围,凡根据本发明精神实质所做的等效变化或修饰,都应涵盖在本发明的保护范围内。
Claims (10)
1.一种包含可聚合化合物的液晶组合物,其特征在于,所述液晶组合物包含:
至少一种通式I的化合物
至少一种通式II的化合物
至少一种通式M的化合物
其中,
R和X1-X12各自独立地表示-H、卤素、-CN、-Sp2-P2、或含有1-12个碳原子的直链、支链或环状的烷基,其中所述含有1-12个碳原子的直链、支链或环状的烷基中的一个或不相邻的两个以上的-CH2-可以分别独立地被-CH=CH-、-C≡C-、-O-、-CO-、-CO-O-或-O-CO-替代,一个或更多个-H可以分别独立地被-F或-Cl取代,其中,X1-X12中的至少一个表示-Cl;
P1和P2各自独立地表示可聚合基团;
Sp1和Sp2各自独立地表示间隔基团或单键;
R1、R2、RM1和RM2各自独立地表示含有1-12个碳原子的直链或支链的烷基、 其中所述含有1-12个碳原子的直链或支链的烷基中的一个或不相邻的两个以上的-CH2-可以分别独立地被-CH=CH-、-C≡C-、-O-、-CO-、-CO-O-或-O-CO-替代;
Z1和Z2各自独立地表示-O-、-S-、-CO-、-CO-O-、-O-CO-、-O-CO-O-、-CH2O-、-OCH2-、-CH2S-、-SCH2-、-CF2O-、-OCF2-、-CF2S-、-SCF2-、-(CH2)n-、-CF2CH2-、-CH2CF2-、-(CF2)n-、-CH=CH-、-CF=CF-、-CH=CF-、-CF=CH-、-C≡C-、-CH=CH-CO-O-、-O-CO-CH=CH-、-CH2CH2-CO-O-、-O-CO-CH2CH2-、-CR1R2-或单键,其中,R1和R2各自独立地表示-H或含有1-12个碳原子的直链或支链的烷基,并且n表示1-4的整数;
ZM1和ZM2各自独立地表示单键、-CO-O-、-O-CO-、-CH2O-、-OCH2-、-C≡C-、-CH=CH-、-CH2CH2-或-(CH2)4-;
LN1和LN2各自独立地表示-F或-Cl;
LN3和LN4各自独立地表示-H、含有1-3个碳原子的烷基或卤素;
2.根据权利要求1所述的液晶组合物,其特征在于,R表示-Sp2-P2。
3.根据权利要求1所述的液晶组合物,其特征在于,a表示0或1。
6.根据权利要求1所述的液晶组合物,其特征在于,所述通式I的化合物占所述液晶组合物的重量百分比为0.001%~5%,所述通式II的化合物占所述液晶组合物的重量百分比为1%~45%,所述通式M的化合物占所述液晶组合物的重量百分比为1%~80%。
7.根据权利要求1所述的液晶组合物,其特征在于,所述液晶组合物还包含至少一种通式III的化合物和至少一种通式IV的化合物:
其中,
R3、R4、R5和R6各自独立地表示含有1-12个碳原子的直链或支链的烷基、 其中所述含有1-12个碳原子的直链或支链的烷基中的一个或不相邻的两个以上的-CH2-可以分别独立地被-CH=CH-、-C≡C-、-O-、-CO-、-CO-O-或-O-CO-替代;
环和环各自独立地表示其中中的一个或更多个-CH2-可以被-O-替代,一个或更多个环中单键可以被双键替代,其中中的一个或更多个-H可以被-F、-Cl或-CN取代,一个或更多个环中-CH=可以被-N=替代;
L1和L2各自独立地表示-F或-Cl;
L3和L4各自独立地表示-H、含有1-3个碳原子的烷基或卤素;
L5、L6、L7和L8各自独立地表示-H、-F或-Cl,其中,L5,L6,L7和L8中的至少两个表示-F或-Cl,并且,当L5、L6、L7和L8中的仅有两个表示-F或-Cl时,则-F或-Cl在同一个苯环上;
Z3和Z4各自独立地表示单键、-CO-O-、-O-CO-、-CH2O-、-OCH2-、-CH=CH-、-C≡C-、-CH2CH2-、-CF2CF2-、-(CH2)4-、-CF2O-或-OCF2-,其中,当Z3表示单键时,环为非芳香环;
n2表示0或1。
9.根据权利要求7所述的液晶组合物,其特征在于,所述通式III的化合物占所述液晶组合物的重量百分比为1%-50%,所述通式IV的化合物占所述液晶组合物的重量百分比为1%-20%。
10.一种包含权利要求1-9中任一项所述的液晶组合物的液晶显示器件。
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