CN107003460A - 具有负光弹性常数的聚合材料 - Google Patents

具有负光弹性常数的聚合材料 Download PDF

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CN107003460A
CN107003460A CN201580064730.0A CN201580064730A CN107003460A CN 107003460 A CN107003460 A CN 107003460A CN 201580064730 A CN201580064730 A CN 201580064730A CN 107003460 A CN107003460 A CN 107003460A
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vinylpyridines
dopant
p2vp
aliphatic
doped poly
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张诗玮
K·M·奥康奈尔
C·沃尔福-古普塔
W·周
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Rohm and Haas Electronic Materials LLC
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Abstract

一种经掺杂的聚(2‑乙烯基吡啶)，其包含2wt％到30wt％的掺杂剂，所述掺杂剂是C9‑C25脂肪族多环化合物。

Description

具有负光弹性常数的聚合材料
技术领域
本发明涉及一种具有负光弹性常数的聚合物组合物。
背景技术
LCD装置包含如下形成的LC(液晶)盒：配置一对透明衬底，其中透明电极面向彼此提供；随后将液晶围封在这对衬底之间。LCD装置已经广泛用于便携式电话、便携式信息终端等，其中期望亮度增强和图像显示品质改进，以及使得LCD装置更轻且更薄。当LCD装置(如智能手机和平板电脑)在完全黑暗的状态下使用时，容易发生漏光，特别是拐角周围和边缘。一个重要的导致原因怀疑是LC盒中的薄玻璃在应力诱导下发生双折射。由于座架结构附接到显示器上或由于内部显示器结构，因此液晶显示器的一部分可能经历应力。一般来说，玻璃具有正光弹性常数，或Cp。因此，为了补偿玻璃衬底的压力诱导型双折射，需要具有负Cp值的材料作为补偿膜。小分子(如反芪)作为掺杂剂在聚合材料(例如聚(甲基丙烯酸甲酯))中用于改变Cp的用途已经揭露于H.Shafiee等人，《国际光学工程学会会刊(Proc.SPIE)》，2010，第7599卷，75990U中。然而，这个参考文献仅教导了Cp的正向变化。
发明内容
本发明提供了掺杂的聚(2-乙烯基吡啶)(P2VP)。掺杂的P2VP包含2wt％到30wt％的掺杂剂，所述掺杂剂是C9-C25脂族多环化合物。
本发明进一步提供掺杂的聚(2-乙烯基吡啶)(P2VP)，其包含2wt％到30wt％的式(II)掺杂剂
其中G表示1-5个选自由氟和氯组成的群组的取代基。
具体实施方式
除非另外规定，否则百分比是重量百分比(wt％)且温度是℃。除非另外规定，否则操作在室温(20-25℃)下进行。如本文中所用，术语“聚(2-乙烯基吡啶)”意指包含至少50wt％2-乙烯基吡啶聚合单元、优选至少60wt％、优选至少70wt％、优选至少80wt％、优选至少90wt％、优选至少95wt％、优选至少98wt％2-乙烯基吡啶聚合单元的聚合物或共聚物。
光弹性效应诱导双折射率是根据材料的光弹性常数(Cp)和施加到材料的应力的量(σ)来确定。光弹性常数如下测定：计算应力诱导的双折射率与在所施加应力仅诱导材料发生较小程度弹性变形的条件下施加到玻璃状材料的应力量值的比率。一种材料的光弹性双折射率不同于那种材料的本征双折射率(Δn0)。本征双折射率是指一种材料当完全在一个方向上定向(例如通过在一个方向上单向拉伸材料)时所展现的双折射的量。正本征双折射率材料在所述材料完全定向所沿的x方向上的折射率(nx)大于在另外两个方向(y和z)上的折射率ny和nz，其中x、y、z代表彼此间相互正交的三个不同方向。反之，负本征双折射率材料在所述材料完全定向所沿的x方向上的折射率小于在另外两个方向y和z上的折射率。正本征双折射率类型的材料总是倾向于正光弹性类型，而对于负双折射率类型的材料来说，其可以是负光弹性类型或正光弹性类型。
光弹性常数是各种材料的本征特性且可以具有正值或负值。因此，材料分成两类：一类具有正光弹性常数且另一类具有负光弹性常数。当具有正光弹性常数的材料沿着x方向经受较小程度的单向拉伸应力时，所述材料倾向于展现正双折射率(即，nx>ny)。反之，当具有负光弹性常数的材料沿着x方向经受较小程度的单向拉伸应力时，所述材料将展现负双折射率(即，nx<ny)。
延迟是薄片材料的双折射率的一种度量。其定义为薄片的Δn与厚度的乘积，其中Δn是nx与ny之间的差值的绝对值。
优选的是，C9-C25脂肪族多环化合物仅含有碳、氢和氧原子；优选不超过六个氧原子，优选不超过四个。优选的是，C9-C25脂肪族多环化合物是桥连多环化合物，优选双环、三环或四环化合物；这些化合物可以被烷基、烷氧基或羟基(优选甲基和/或羟基)取代；或其可以未被取代。优选的是，脂肪族多环化合物具有10到20个碳原子。优选的是，C9-C25脂肪族多环化合物包含键结到C2-C8非环状脂肪族取代基的C6-C20脂肪族多环取代基。优选的是，C2-C8非环状脂肪族取代基包含一到四个氧原子；优选至少两个、优选不超过三个。优选的是，非环状脂肪族取代基具有三到六个碳原子。优选的是，非环状脂肪族取代基具有至少一个酯基。优选的是，脂肪族多环取代基通过酯氧键结到非环状脂肪族取代基。优选的是，脂肪族多环取代基具有8到12个碳原子。优选的是，脂肪族多环取代基是桥连多环取代基，优选双环、三环或四环取代基。优选的是，C9-C25脂肪族多环化合物是式(I)化合物
其中R1是氢或甲基且R2是未被取代的或具有丙烯酸酯或甲基丙烯酸酯取代基的C6-C20脂肪族多环取代基。优选的是，R2是C7-C15脂肪族多环取代基；优选的是，R2是C8-C12脂肪族多环取代基。优选的是，R2是桥连多环取代基；优选双环、三环或四环取代基。优选的R2结构包括例如金刚烷、双环[2,2,1]烷烃、双环[2,2,2]烷烃、双环[2,1,1]烷烃；这些结构可以被烷基、烷氧基或羟基(优选甲基和/或羟基)取代。特别优选金刚烷和双环[2,2,1]烷烃。优选的是，R1是甲基。优选的是，R2未被取代。
优选的是，式(II)中的G表示1-3个、优选2-3个取代基。优选的是，取代基选自由氟和氯组成的群组。
优选的是，掺杂的P2VP是通过将P2VP与式(I)或(II)化合物在适合溶剂中混合来制备以供使用。根据特定掺杂剂的溶解性，可以使用单一溶剂或溶剂混合物来溶解所掺混的材料。优选的是，所掺杂P2VP溶液的含固量是在10-50wt％范围内。可以将溶液浇铸到剥离型衬底(如剥离型纸)上的独立膜上或工业上众所周知的连续浇铸带上。还可以将所掺杂的P2VP溶液直接涂覆到衬底(例如光学膜或薄片或玻璃衬底)上作为用于增强光学特性的涂层。然后优选在真空下，将所掺杂P2VP的湿涂层或湿膜烘烤足以产生基本上均一膜的时间。优选条件是50到100℃的温度和5到30小时的时间。
优选的是，所掺杂聚合物中的掺杂剂的含量按所掺杂聚合物的总重量计是大于5wt％，优选至少8wt％，优选至少10wt％，优选至少12wt％；优选不超过30wt％，优选不超过25wt％。
可以通过使用所属领域中众所周知的任何适合涂布方法将根据本发明的所掺杂P2VP直接涂布到液晶盒的玻璃衬底上。举例来说，所掺杂的P2VP可以通过浸涂、旋涂或槽模涂布法涂布到玻璃上。槽模涂布法因其涂布区域、涂布厚度和均一性相对容易控制而更优选。必要时，可以任选地将助粘剂并入涂层配方中以赋予涂层对LC盒的优良粘附性。玻璃衬底还可以用助粘剂进行表面改性以进一步改进所掺杂P2VP材料对玻璃的粘附性。所掺杂P2VP层的厚度的优选范围是小于100μm，更优选小于50μm，甚至更优选小于25μm；优选大于5μm，优选大于10μm。当此类所掺杂P2VP层的厚度大于100μm时，其不宜用作以较薄为消费者偏好的电子装置。反之，当此类所掺杂P2VP层的厚度小于5μm时，薄涂层在玻璃衬底发生变形时赋予玻璃衬底光学补偿的作用有限。
玻璃片厚度的优选范围是0.1mm到0.7mm，优选0.2mm到0.5mm。当玻璃衬底的厚度大于0.7mm时，光学涂层的作用可能不够强且这还将增加装置的厚度。当玻璃衬底小于0.1mm时，其物理硬度就装置制造来说有问题。
实例
三种不同聚合物聚(甲基丙烯酸甲酯)(PMMA)、聚(2-乙烯基吡啶)(P2VP)和聚(4-乙烯基吡啶)(P4VP)经小分子掺杂剂掺杂以制备复合物***。所测试的小分子包括以下：2-萘酚(用2-NP表示)、3-苯基苯酚(用3-PP表示)、反芪(用t-芪表示)、3,4,5-三氟苯甲酸(用TFBA表示)、3,4,5-三氟苯基乙酸(用TFPAA表示)、氰基苯甲酸(用CNBA表示)、4-甲基-联苯-2-甲腈(用4M2BCN表示)、2-氟-6-苯氧基苯甲腈(用FPHBN表示)、1-羟基甲基丙烯酸3-金刚烷酯(用HAMA表示)、1-羟基甲基丙烯酸3-金刚烷基甲酯(用MHAMA表示)和甲基丙烯酸异冰片烷酯(用IBOMA表示)。
复合物***的独立膜如下制备：首先将所掺混的配制物和对照物(不含掺杂剂的聚合物)浇铸到经聚(二甲基硅氧烷)或PDMS预处理(刷涂层)的玻璃衬底上。然后将所涂样品在75℃、在真空下烘烤至少4小时，然后将膜剥离用于光学表征。通过测量平面内膜延迟、同时向样品试样施加单轴向拉伸应力来进行光弹性测量。将聚合物膜切成约1”X3”(2.54X7.62cm)片段且安装在单轴向拉伸伸展台上，所述伸展台附接到Exicor 150AT双折射率测量***(Hinds Instruments)。在546纳米(nm)波长下测量膜的光学延迟与外施力的关系。手动地控制力且通过连接到样品安装握把之一的OMEGA DFG41-RS力变换器来测量力。外施力在0-15牛顿的范围内。光弹性常数或应力光学系数Cp是根据应力对双折射率曲线的斜率计算。不同复合物***的Cp测量结果示于下表中。
表1.由具有不同添加剂的P2VP制成的膜的光弹性特性
由25wt％乳酸乙酯溶液制备的膜
表2.由具有不同添加剂的P4VP制成的膜的光弹性特性
由25wt％乳酸乙酯溶液制备的膜
表3.由具有不同添加剂的PMMA制成的膜的光弹性特性
PMMA和经3-PP、2-NP、反芪、4M2BCN、HAMA掺杂的PMMA皆在苯甲醚中制备成25wt％溶液。经TFPAA、CNBA、TFBA掺杂的PMMA皆用苯甲醚和乳酸乙酯的混合溶剂(比率为70/30)制备成25wt％溶液。
通过改变添加剂装载量来进一步研究P2VP-TFBA和P2VP-HAMA***。通过将聚合物和添加剂溶解于乳酸乙酯中而将两种小分子添加剂按5wt％、10wt％、15wt％和20wt％的含量掺杂到P2VP基质聚合物中，以获得具有25wt％含固量的掺混溶液。制备独立膜且以此前段落中所述的相同方式表征。下表表明了复合物***的Cp结果与添加剂装载量的关系。在所有情况下，通过掺杂基质聚合物来获得负Cp。还清楚地表明，Cp的量值容易通过改变添加剂装载量来调节，其中较高的掺杂剂装载量通常导致复合物***具有较大的负Cp值。

Claims (7)

1.一种经掺杂的聚(2-乙烯基吡啶)，其包含2wt％到30wt％的掺杂剂，所述掺杂剂是C9-C25脂肪族多环化合物。
2.根据权利要求1所述的经掺杂的聚(2-乙烯基吡啶)，其中所述C9-C25脂肪族多环化合物是式(I)化合物
其中R1是氢或甲基且R2是未被取代的或具有丙烯酸酯或甲基丙烯酸酯取代基的C6-C20脂肪族多环取代基。
3.根据权利要求2所述的经掺杂的聚(2-乙烯基吡啶)，其中R2是C7-C15桥连多环取代基。
4.根据权利要求3所述的经掺杂的聚(2-乙烯基吡啶)，其包含10wt％到27wt％的所述掺杂剂。
5.一种经掺杂的聚(2-乙烯基吡啶)(P2VP)，其包含7wt％到30wt％的式(II)掺杂剂
其中G表示1-5个选自由氟和氯组成的群组的取代基。
6.根据权利要求5所述的经掺杂的聚(2-乙烯基吡啶)，其中G表示1-3个选自由氟和氯组成的群组的取代基。
7.根据权利要求6所述的经掺杂的聚(2-乙烯基吡啶)，其包含10wt％到27wt％的所述掺杂剂。
CN201580064730.0A 2014-12-18 2015-12-07 具有负光弹性常数的聚合材料 Pending CN107003460A (zh)

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