CN1093731A - 含二色性染料的垂直定向液晶聚合物膜 - Google Patents

含二色性染料的垂直定向液晶聚合物膜 Download PDF

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CN1093731A
CN1093731A CN94101118A CN94101118A CN1093731A CN 1093731 A CN1093731 A CN 1093731A CN 94101118 A CN94101118 A CN 94101118A CN 94101118 A CN94101118 A CN 94101118A CN 1093731 A CN1093731 A CN 1093731A
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S·J·匹克森
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Abstract

本发明涉及含至少一种二色性染料，垂直定向的 液晶聚合物膜。使该膜用于输出和读取数据的各种 技术中。其对比度是由膜中所含作为中介基团并以 同向排列的二色性染料获得的。在未处理膜中，其中 介基团，即二色性染料分子垂直定向于膜的表面，这 些分子对入射光只有低的吸收。对膜局部加热或辐 照(如用激光)可使垂直定向转变为各向同性。则二 色性染料将同样是各向同性的，导致对入射光具有相 当高的吸收。该膜适用于模拟数字光数据存储器。

Description

本发明涉及至少含一种二色性染料的液晶聚合物膜。这种聚合物膜已在EP-A1-422538中叙述，该专利公开了用作液晶聚合物组成嵌段的二色性染料。这些液晶聚合物可用于光信息存储薄膜，所述专利中公开的液晶聚合物都具有共平面和切向定向结构。
到目前为止，已知的光信息存储膜还没有达到最佳效果。如若要获得足够的对比度必须采用厚的膜，但使用这种厚膜就要求低的写入速度。此外，膜厚度的变化也常常会产生一些问题。本发明解决或者减少了这些问题的产生。
本发明在于液晶聚合物膜是垂直（homeotropically）定向的，“垂直定向”一词是指液晶聚合物中的中介（mesogenic）基团是垂直定向于膜表面的。该垂直定向与存在的二色性染料一起使得能够使用不同工艺读取和输出数据。
在这种情况下，对比度是由膜中所含的作为液晶聚合物中介基团，并以同向排列的二色性染料所获得的。二色性染料吸收一个方向偏振光的程度远大于其它方向。通常，以分子运动为基础得出的平均方向与杂料分子的长轴相一致。在未处理膜中，其中介基团，即二色性染料分子是垂直定向于膜的表面的，这些分子对入射光只存在低的吸收（应该指出光的偏振方向与其传播方向相垂直），用局部加热或辐照（如用激光）可使垂直定向转变为各向同性。在各向同性书写印迹的情况下，二色性染料会同样是各向同性定向的，导致对入射光有相当高的吸收。读取值表现为二色性染料在可见光、紫外光或红外光区最大吸收的函数。
在光数据存储器中采用这一技术使其能获得高的对比度，即使对薄膜也如此。由于垂直定向，可用非偏振光读取数据，所以不需偏振器，偏振器不仅价格昂贵而且在重氮盐波长（约410nm）区透射率低。这一写/读方法的另一优点是对膜厚度的均匀性没有极高的要求。根据本发明的垂直定向的液晶膜适用于模似和数字光数据存储器，当然也适用于模拟/数字结合的数据存储器。
二色性染料可以混合到液晶聚合物中或者与液晶聚合物共价键合。另一种可选择的方法是采用中介基团本身就是二色性染料的液晶聚合物，当然这种情况就不需加入二色性染料。这类中介基团的实例是芪的侧基团和全芳族Schiff碱（即两侧为芳环取代的亚胺基团）。
原则上，如能足够稳定地与聚合物相混合或与聚合物相键合的任何二色性染料都可被采用。
供模拟数据存储器用的特别优选的是吸收紫外光的二色性染料，因为所述液晶膜可用重氮盐复制。适用的二色性染料的实例是由MerckR制造的D2和苏丹橙G。供人可读的可见光二色性存储器优先选用D2和苏丹橙G。
对数字存储器，特别优选的是在适当的红外波长（780-820nm）范围内能调节膜的反射率的红外二色性染料。适用的红外二色性染料是crocomium染料、Squarilium染料和红外氮杂芳甲烷染料。
原则上所有具有向列相或近晶A相的合用的液晶聚合物在可见视场内都是透明的，优选范围为Tg＝85℃至Tc＝120℃。其实例包括液晶聚酯、液晶聚氨酯、液晶聚碳酸酯、液晶聚（甲基）丙烯酸酯、液晶聚酰亚胺、液晶聚酰胺及液晶聚酰胺酰亚胺。
侧链型液晶聚酯和侧链型液晶聚氨酯是特别优选的，因为它们是容易制备的并具有相当好的热稳定性和化学稳定性以及耐紫外辐射。
已发现具有根据下述式1的中介基团的聚氨酯和聚酯是特别适用的：
Figure 941011186_IMG1
式中R1＝卤素、-R2、-OR2、
Figure 941011186_IMG2
、CN、或CF3;
R2＝-H或具有1-3个碳原子的烷基;
R3可以代表与R1相同的基团，但也可独立地选自R1;
Q代表连接中介基团到聚合物主链的单体基团;
n为0或1;
m为0或1;
y为0-3的整数;
p为2-4的整数;
R4＝具有1-12个碳原子的烷基;
x为0-6的整数;
z＝-C＝N-、-N＝C-、 、-C＝C-、
Figure 941011186_IMG4
。
具有根据式1侧基的聚酯类和聚氨酯类是很适用的，特别是因为不同的间隔基团长度及烷基R4的长度以及分别采用二酰氯类和二异氰酸酯类混合物，所以可严格设定Tg和Tc。为此目的，可参见EP-A-0550105。在所述的文献中用于设定这些液晶聚氨酯类的Tg和Tc的技术可同等地应用于具有根据式1中介基团的液晶聚酯类中。对于液晶聚氨酯类的制备和其它信息也引用于该申请，这些公开内容在此列入本文作为公开内容的一部分。
侧链型液晶聚酯的专门制备方法可参阅EP-A-0478052（公开日期：1992、1、4）。
上面提到的聚酯类和聚氨酯类的其它优点在于它们具有二色性侧基，如果在紫外波长区域z为-C＝N-、-N＝C-及-C＝C-。
一般，膜是通过将聚合物溶液置于基片上并蒸发溶剂而制得的，适用的基片包括PET、PET-金、PET-ITO、PET-铝、金属、玻璃、醋酸纤维素、聚碳酸酯、聚碳酸酯-铝、硅等。通常所用的膜厚为0.5-10微米。
液晶聚合物可以用几种方式进行垂直定向。
1.用诱导表面活性剂（硅烷、高级醇等如正十二烷醇和LiquicoatR，购自Merck）处理基片表面使液晶聚合物具有垂直定向。
2.用针或细金属丝极化（电晕）液晶层或采用在基片上设置一层铟-锡氧化物（ITO）层或某些其它导电层，通过该导电层间液晶层施加极化场。或者，可在液晶层的每面设置导电层，并在其上施加电场。
3.将聚合物膜通过热压辊挤压层合后使聚合物垂直定向为具有近晶A相定向。产生的剪切形变使中介基团垂直定向。
在用表面处理方法制备垂直定向聚合物膜时，聚合物膜的粘度和膜层厚度是重要的。
当展望在模拟存储器中采用固态激光器供数据的写入时，液晶膜必须是或者必须制成吸收红外光的。一般是在液晶膜内混入红外吸收染料或采用红外吸收染料与液晶聚合物相结合的方法制备的。含有几乎不定向或不具有二色性的红外吸收染料也是可行的，但此种情况在写入操作时吸收不会令人满意。因此最好选用分子不具有细长形状（如扁平形分子或四面体分子）的红外吸收染料，或者可采用在垂直于分子轴方向有最高吸收率的红外二色性染料。当然，在这种情况下采用定向染料也是可行的。
对于数字存储器，为了使该存储器在红外波长区域能进行书写和读取，采用二色性红外染料是可行的。在写入时采用的激光功率（光强度）愈高则读出时所用的激光功度愈低。对于磁盘的制造，遵循背景透射70%和写入透射是背景透射的40%即28%的标准，二色性比率（α‖/α⊥）至少要求为8.7。
本发明用下面的非限制性实施例加以说明。
Croconium染料（CR）是根据EP-0478052中实施例4制备的。
根据EP-0350113实施例4用实施例1的二元醇和己二酰二氯制成含约5%CR红外染料的液晶聚酯（LCP）薄层，将含20%（重量）的LCP和染料的环戊酮溶液（η＝5mPa）在2000rpm转速下以旋涂法涂敷在敷铝的PET基片上制成含红外染料的LCP膜（约0.5微米厚）。干燥约24小时后用电晕极化方法（V＝6-10KV、T＝40-80℃）对试样进行垂直定向。结果得到透明垂直定向的液晶聚酯层。
所得试样的反射光谱示于图1。主要的反射出现在由LCP的羟基-硝基-芪侧链引起的紫外波长区域和由CR红外染料引起的红外波长区域。将试样均匀地加热至高于Tc并迅速冷却到低于Tg，可制得非定向、透明的各向同性膜，该各向同性膜的光谱也示于图1。根据垂直定向试样和各向同性试样所得的光谱间的差异，可得出二色性与液晶侧链和红外染料成正比的结论。观察到的这种效应可用于数据存储器。

Claims (2)

1、至少含一种二色性染料的液晶聚合物膜，其特征在于该液晶聚合物膜是垂直定向的。
2、根据权利要求1的液晶聚合物膜，其特征在于二色性染料是液晶聚合物的一种中介基团。
CN94101118A 1993-01-26 1994-01-25 含二色性染料的垂直定向液晶聚合物膜 Pending CN1093731A (zh)

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CN112912467A (zh) * 2019-02-01 2021-06-04 捷恩智株式会社 液晶复合体、液晶调光元件及调光窗

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CN105807472A (zh) * 2014-12-31 2016-07-27 厦门天马微电子有限公司 一种显示面板及其制作方法、显示装置
CN105807472B (zh) * 2014-12-31 2019-04-23 厦门天马微电子有限公司 一种显示面板及其制作方法、显示装置
CN112912467A (zh) * 2019-02-01 2021-06-04 捷恩智株式会社 液晶复合体、液晶调光元件及调光窗
CN112912467B (zh) * 2019-02-01 2023-10-20 捷恩智株式会社 液晶复合体、液晶调光元件及调光窗

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