CN114879399A - 一种聚合物稳定胆甾相液晶变色玻璃及其制备方法和应用 - Google Patents
一种聚合物稳定胆甾相液晶变色玻璃及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及液晶显示和电致变色技术领域,尤其是一种聚合物稳定胆甾相液晶变色玻璃的制备方法,包括以下步骤:步骤S1、将负性胆甾相液晶、液晶性单体、手性剂和引发剂混合,得到胆甾相液晶混合物;步骤S2、在毛细作用下,将所述胆甾相液晶混合物流入液晶玻璃盒内,待胆甾相液晶混合物均匀填满整个液晶玻璃盒,依次施加不同电场和高频交流电后,进行紫外固化,得到所述聚合物稳定胆甾相液晶变色玻璃。利用所述制备方法制备得到的聚合物稳定胆甾相液晶变色玻璃可以在电压恒定的条件下,通过手动切换外加直流电场的方向来改变所述聚合物稳定胆甾相液晶变色玻璃的反射带的带宽,同时可以显示出明显的颜色变化。
Description
技术领域
本发明涉及液晶显示和电致变色技术领域,尤其涉及一种聚合物稳定胆甾相液晶变色玻璃及其制备方法和应用。
背景技术
具有宽波反射特性的胆甾相液晶(Ch-LC)应用范围广泛,其中反射波宽范围在可见光波段的Ch-LC广泛的应用与移动信息工具、电子书及其他小尺寸显示器件,无需配置背光源,通过反射自然光即可实现彩色显示,可起到减少能源消耗、节能环保的重要作用,用作液晶显示面板光增亮膜,可通过对光的反射和再回收提高背光源的利用效率、减少背光源能耗,用作燃料敏化太阳电池的柔性反射背板,可提高电池的输出光电流和转换效率。另一方面,宽波反射谱带在红外光范围的Ch-LC用于建筑节能领域,通过对辐射在建筑上的太阳光中大部分红外光进行反射,在保障建筑内部采光的同时减少红外热量对室内温度的影响,可有效节约夏季用电能耗,用于激光防护器件,可同时防护不同波段的激光辐射,减少层状结构光耗损并提高可见光透过率。胆甾相液晶的反射带宽可以通过调控胆甾相液晶材料体系内的螺距梯度或螺距随机分布来实现反射波普的拓宽,常用的形式螺距非均匀分布的方式具体有:层叠法,光诱导分子扩散产生螺距非均匀分布,热诱导分子扩散产生螺距非均匀分布,手性化合物螺旋扭曲力变化,电磁场诱导螺距非均匀分布。
在上述光诱导、热诱导和电磁场诱导等外部刺激源中,电场因其响应速度快、应用范围广、操作简单和实用性强而被认为是最简单的方法。然而,目前对聚合物稳定胆甾相液晶(PSCLC)的电诱导反射带拓宽的研究主要集中在如何拓宽带宽和降低阈值电压等方面。研究表明,利用直流电场可以拓宽具有负介电各向异性的聚合物稳定胆陪相液晶的反射带宽。但当外加电压恒定时,反射带的带宽是无法调整的。
发明内容
本发明的目的是为了解决现有技术中存在的缺点,而提出的一种聚合物稳定胆甾相液晶变色玻璃及其制备方法和应用;利用所述制备方法制备得到的聚合物稳定胆甾相液晶变色玻璃可以在电压恒定的条件下,通过手动切换外加直流电场的方向来改变所述聚合物稳定胆甾相液晶变色玻璃的反射带的带宽,同时可以显示出明显的颜色变化。
为了实现上述目的,本发明采用了如下技术方案:
设计一种聚合物稳定胆甾相液晶变色玻璃的制备方法,包括以下步骤:
步骤S1、将负性胆甾相液晶、液晶性单体、手性剂和引发剂混合,得到胆甾相液晶混合物;
步骤S2、在毛细作用下,将所述胆甾相液晶混合物流入液晶玻璃盒内,待胆甾相液晶混合物均匀填满整个液晶玻璃盒,首先施加直流电场处理,后在施加高频交流电时进行紫外固化,得到所述聚合物稳定胆甾相液晶变色玻璃;
所述液晶玻璃盒为PI/ITO双拼液晶玻璃盒,预处理加直流电场PI层接负极,由于液晶性单体含有酯基醚基等吸电子基团,可吸附溶液中正性离子,施加电场后,由于静电力的作用,单体沿电场方向运动,又由于电极与界面间的电极极化和界面极化的作用,在玻璃基板上形成双电层,单体被固定在基板表面;后加高频紫外固化使液晶层在施加电场和紫外固化的条件下,由于在器件的ITO层至PI层厚度方向上具有单体分布梯度,导致不同单体含量处的聚合速率不同,形成了不同疏密程度的液晶性聚合物网络,且所述液晶性聚合物网络的疏密程度呈梯度分布。
进一步优选的,所述负性胆甾相液晶、液晶性单体、手性剂和引发剂的质量比为100:(9-12):(2-3):1。
进一步优选的,所述的液晶性单体的结构式如下:
所述的手性剂的结构式如下:
所述的引发剂的结构式如下:
进一步优选的,在步骤S1中的混合温度为100-140℃,时间为10-14h。
进一步优选的,在步骤S2中的直流电的电压为130-170V。
进一步优选的,在步骤S2中的高频交流电的电压为130-170V,频率为1kHz。
进一步优选的,在步骤S2中的紫外固化的强度为1-5mW/cm2,时间为20-40min;
所述紫外固化在施加交流电的条件下进行,且交流电的电压为130-170V,频率为1kHz。
进一步优选的,所述的液晶玻璃盒的上下两层玻璃板之间的间距为25-35μm。
本发明还提供了一种聚合物稳定胆甾相液晶变色玻璃,包括由下至上依次设置的下层PI层玻璃基板、液晶性聚合物层和上层ITO层玻璃基板;液晶性聚合物层中的聚合物网络密度呈梯度分布。
进一步优选的,聚合物稳定胆甾相液晶变色玻璃在电致变色领域中的应用。
本发明提出的一种聚合物稳定胆甾相液晶变色玻璃的制备方法,有益效果在于:
利用本发明制备得到的聚合物稳定胆甾相液晶变色玻璃可以通过手动切换施加直流电场的方向来实现反射带拓宽的转变,这种方法更简单更高效,能够精准控制,并且在改变直流电场电压,可以出现明显的颜色变化。
附图说明
图1为本发明的原理示意图;
图2为本发明的电响应原理示意图;
图3为本发明的上极板聚合物网络示意图;
图4为本发明的下极板聚合物网络示意图;
图5为本发明的ITO,PI层的反射带宽柱状图;
图6为本发明聚合物稳定胆甾相液晶变色玻璃在改变直流电场方向后施加电压与波长的关系图;
图7为本发明聚合物稳定胆甾相液晶变色玻璃在直流电场下施加电压和颜色的变化图;
图8为本发明制备PSCLC的实物图;
图9为本发明聚合物稳定胆甾相液晶变色玻璃的结构示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。
实施例1
在净化间(黄光室温条件下),将负性胆甾相液晶,手性剂、液晶性单体和引发剂在棕色玻璃瓶中搅拌混合,其中,所述负性胆甾相液晶、手性剂、液晶性单体、引发剂的质量比为100:9:3:1,混合的温度为140℃,时间为10h,得到胆甾相液晶混合物;
将所述胆甾相液晶混合物灌至PI/ITO双拼液晶玻璃盒(上层玻璃板的厚度为1mm,下层玻璃板的厚度为1mm,两层玻璃板之间的间距为25μm)中,所述胆甾相液晶混合物在毛细作用下缓慢流入液晶玻璃盒中至所述胆甾相液晶混合物填满整个液晶玻璃盒,施加直流电(130V)PI层接负极ITO层接正极加电5min后,再施加交流电(130V,1kHz)的条件下进行紫外固化(紫外光波长为365nm,强度为5mW/cm2)20min,得到所述聚合物稳定胆甾相液晶变色玻璃。
实施例2
在净化间(黄光室温条件下),将负性胆甾相液晶,手性剂、液晶性单体和引发剂在棕色玻璃瓶中搅拌混合,其中,所述负性胆甾相液晶、手性剂、液晶性单体、引发剂的质量比为100:10:2.5:1,混合的温度为120℃,时间为12h,得到胆甾相液晶混合物;
将所述胆甾相液晶混合物灌至PI/ITO双拼液晶玻璃盒(上层玻璃板的厚度为1mm,下层玻璃板的厚度为1mm,两层玻璃板之间的间距为30μm)中,所述胆甾相液晶混合物在毛细作用下缓慢流入液晶玻璃盒中至所述胆甾相液晶混合物填满整个液晶玻璃盒,施加直流电(150V)PI层接负极ITO层接正极加电5min后,再施加交流电(150V,1kHz)的条件下进行紫外固化(紫外光波长为365nm,强度为3mW/cm2)30min,得到所述聚合物稳定胆甾相液晶变色玻璃。
实施例3
在净化间(黄光室温条件下),将负性胆甾相液晶,手性剂、液晶性单体和引发剂在棕色玻璃瓶中搅拌混合,其中,所述负性胆甾相液晶、手性剂、液晶性单体、引发剂的质量比为100:12:2:1,混合的温度为140℃,时间为14h,得到胆甾相液晶混合物;
将所述胆甾相液晶混合物灌至PI/ITO双拼液晶玻璃盒(上层玻璃板的厚度为1mm,下层玻璃板的厚度为1mm,两层玻璃板之间的间距为35μm)中,所述胆甾相液晶混合物在毛细作用下缓慢流入液晶玻璃盒中至所述胆甾相液晶混合物填满整个液晶玻璃盒,施加直流电(170V)PI层接电源负极ITO层接正极加电5min后,再在施加交流电(170V,1kHz)的条件下进行紫外固化(紫外光波长为365nm,强度为1mW/cm2)30min,得到所述聚合物稳定胆甾相液晶变色玻璃。
参考图1-9,一种聚合物稳定胆甾相液晶变色玻璃的制备方法,具体步骤如下:
将负性胆甾相液晶、液晶性单体、手性剂和引发剂混合,得到胆甾相液晶混合物;
在毛细作用下,将所述胆甾相液晶混合物流入液晶玻璃盒至所述胆甾相液晶混合物填满整个液晶玻璃盒,依次施加不同电场和高频交流电后,进行紫外固化,得到所述聚合物稳定胆甾相液晶变色玻璃。
在本发明中,若无特殊说明,所有原料组分均为本领域技术人员熟知的市售产品。
本发明将负性胆甾相液晶、液晶性单体、手性剂和引发剂混合,得到胆甾相液晶混合物。在本发明中,所述负性胆甾相液晶、液晶性单体、手性剂和引发剂的质量比优选为100:(9-12):(2-3):1,预处理施加电场为直流电场。
在本发明中,液晶性单体的结构式如下:
所述的手性剂的结构式如下:
所述的引发剂的结构式如下:
在本发明中,负性胆甾相液晶的型号为HNG30500-100,具有较小的双折射率△n=ne-n0=-0.098,其中ne和n0分别为1.574,1.476(589nm,20℃),常温下的介电各向异性△ε为-7.4,加电时液晶分子沿垂直电场方向排列;所述液晶性单体上具有更多的吸电子基团,例如酯基和醚基,预处理使液晶性单体沿电场方向运动,同时由于界面效应在液晶玻璃盒基板处形成双电层,液晶性单体被固定在玻璃基板表面,在液晶盒中形成局部单体浓度不均匀。后加高频交流电进行紫外固化,由于单体之间反应生成的液晶性聚合物网络骨架上,也由于存在这些吸电子基团,网络会吸附液晶混合溶液中的正性离子,在直流电场下网络可由正极向负极产生平动运动,由于聚合物网络与液晶分子的锚定效应,因此在外加电场的作用下,网络带动带动液晶分子产生平动运动,反导致螺距呈梯度分布,螺距P增大,根据Δλ=Δn×p,从而射带变宽。所述手性剂的作用是使液晶形成螺旋结构即为胆甾相液晶;所述引发剂通过吸收光能,由基态变为激发态,产生自由基,从而引发单体聚合交联成聚合物网络;
所述液晶玻璃盒为PI/ITO双拼液晶玻璃盒,预处理加直流电场PI层接负极,由于液晶性单体含有酯基等吸电子基团,可吸附溶液中正性离子,施加电场后,由于静电力的作用,单体沿电场方向运动,又由于电极与界面间的电极极化和界面极化的作用,在玻璃基板上形成双电层,单体被固定在基板表面。后加高频紫外固化使所述液晶层在施加电场和紫外固化的条件下,由于在器件的ITO层至PI层厚度方向上具有单体分布梯度,导致不同单体含量处的聚合速率不同,形成了不同疏密程度的液晶性聚合物网络(局部单体含量多聚合速度快,可形成致密的液晶性聚合物网络,弹性模量较高;局部单体含量少处聚合速度慢,则表现为稀疏的网络,弹性模量较低),且所述液晶性聚合物网络的疏密程度呈梯度分布。
在本发明中,所述混合的温度优选为120℃,时间优选为12h;所述混合优选在净化间中进行;所述净化间优选提供室温和黄光环境。
得到胆甾液晶混合物后,本发明在毛细作用下,将所述胆甾相液晶混合物流入液晶玻璃盒至所述胆甾相液晶混合物填满整个液晶玻璃盒,依次施加直流电和高频交流电后,进行紫外固化,得到所述聚合物稳定胆甾相液晶变色玻璃。
在本发明中,所述液晶玻璃盒上下两层玻璃板之间的间距优选为30μm。所述液晶玻璃盒的上层玻璃板的厚度优选为1mm;所述液晶玻璃盒的下层玻璃层的厚度优选为1mm。在本发明中,所述液晶玻璃盒优选PI/ITO双拼液晶玻璃盒。
在本发明中,所述预处理直流电的电压优选为150V,时间优选为5min。
在本发明中,施加所述直流电的目的是使液晶性单体沿电场运动,同时胆甾相液晶分子的原有结构被打乱。
在本发明中,所述紫外固化的强度优选为3mW/cm2,时间优选为30min。所述紫外固化采用的紫外光波长优选为365nm;所述紫外固化优选在施加交流电的条件下进行;所述交流电的电压为150V,频率为1kHz。
在本发明中,紫外固化过程中施加所述交流电的目的是降低聚合物网络生长对液晶分子排列的扰乱,体系仍然能够保持结构规整的光子带隙。
在本发明中,所述紫外固化的目的是使单体聚合,与液晶发生相分离,在这个过程中发生的变化为在聚合的初始阶段,单体与液晶具有一定的相容性,此时体系为均一物质。随着光照时间的增加,聚合物分子量增加相容性降低,与液晶分子发生相分离,最终析出的聚合物交联形成聚合物网络,从而得到了聚合物稳定胆甾相液晶。
参考图9,本发明还提供了上述技术方案所述的制备方法制备得到的聚合物稳定胆甾相液晶变色玻璃,包括由下至上依次设置的下层PI层玻璃基板1、液晶性聚合物层2和上层ITO层玻璃基板3;液晶性聚合物层2中的聚合物网络密度呈梯度分布。
在本发明中,所述聚合物稳定胆甾相液晶变色玻璃的工作原理具体为:液晶性单体上存在酯基和醚基,生成的聚合物网络骨架上,由于存在这些吸电子基团,加直流电场预处理使单体吸附溶液中的阳离子沿电场方向运动。如图1所示,当施加直流电场预处理后,吸附阳离子的单体沿电场方向运动,在负基板处聚集在液晶玻璃盒厚方向自上而下形成单体浓度梯度,从而导致不同深度的聚合速率不同,即靠近负基板处聚合速率快,形成的聚合物网络致密,弹性模量较高,而正基板处聚合速率慢,形成的聚合物网络稀疏,弹性模量较低。如图2所示,对获得的器件施加直流电场,网络会吸附液晶混合溶液中的正性离子,在直流电场下由正极向负极产生平动运动,由于聚合物网络与液晶分子的锚定效应,胆甾相液晶中的螺旋结构产生平动运动,导致螺距形成梯度分布,反射带变宽。因此,当PI层接负极时,负极基板处形成的聚合物网络密集,弹性模量较大,施加相同的电压时,正极附近的拉伸位移大。而当PI为正极时,ITO层负基板处的聚合物网络稀疏,弹性模量较小,同时由于PI层对电场也存在一定的分压作用,当施加相同电压时,正极附近的拉伸位移较小,负基板处压缩较大。
由图3-4可知,PI层基板和ITO层基板的聚合物网络,PI层网络较ITO层致密。
由图5-6可知,PI层接正极,得到所述聚合物稳定胆甾相液晶变色玻璃在收到电诱导后的反射波长,图5为PI层接负极的测试结果。由图可知随着电压的增加带隙沿长波方向红移,同时沿短波方向蓝移,带隙拓宽。施加相同的电压(70V),当PI层为正极时,正极附近的聚合物网络密度大,弹性模量大,同时由于PI层的分压作用,在施加相同电压时,负极处的压缩位移较大,则在短波方向有较多的拓宽,反射带隙位于520-730nm之间。而当PI为负极时,正极附近的高分子网络密度较低,弹性较低,所以当施加相同电压时,正极处的拉伸位移较大,则在长波方向有较多的拓宽。反射带隙位于470-740nm之间;
由图7-8可知,反射色可以从红色调到橙色和黄色,所述聚合物稳定胆甾相液晶变色玻璃可以应用在电致变色领域。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,包括以下步骤:
步骤S1、将负性胆甾相液晶、液晶性单体、手性剂和引发剂混合,得到胆甾相液晶混合物;
步骤S2、在毛细作用下,将所述胆甾相液晶混合物流入液晶玻璃盒内,待胆甾相液晶混合物均匀填满整个液晶玻璃盒,依次施加直流电场和高频交流电后,进行紫外固化,得到所述聚合物稳定胆甾相液晶变色玻璃;
所述液晶玻璃盒为PI/ITO双拼液晶玻璃盒,预处理加直流电场PI层接负极,由于液晶性单体含有酯基吸电子基团,可吸附溶液中正性离子,施加电场后,由于静电力的作用,单体沿电场方向运动,又由于电极与界面间的电极极化和界面极化的作用,在玻璃基板上形成双电层,单体被固定在基板表面;
后加高频紫外固化使液晶层在施加电场和紫外固化的条件下,由于在器件的ITO层至PI层厚度方向上具有单体分布梯度,导致不同单体含量处的聚合速率不同,形成了不同疏密程度的液晶性聚合物网络,且所述液晶性聚合物网络的疏密程度呈梯度分布。
2.根据权利要求1所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,所述负性胆甾相液晶、液晶性单体、手性剂和引发剂的质量比为100:(9-12):(2-3):1。
3.根据权利要求2所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,在步骤S1中的混合温度为100-140℃,时间为10-14h。
4.根据权利要求3所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,在步骤S2中的直流电场的电压为130-170V。
5.根据权利要求3所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,在步骤S2中的高频交流电的电压为130-170V,频率为1kHz。
6.根据权利要求5所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,在步骤S2中的紫外固化的强度为1-5mW/cm2,时间为20-40min;
所述紫外固化在施加交流电的条件下进行,且交流电的电压为130-170V,频率为1kHz。
7.根据权利要求6所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,所述的液晶玻璃盒的上下两层玻璃板之间的间距为25-35μm。
8.根据权利要求1-7任一项所述的制备方法制备得到的聚合物稳定胆甾相液晶变色玻璃,其特征在于,包括由下至上依次设置的下层PI层玻璃基板(1)、液晶性聚合物层(2)和上层ITO层玻璃基板(3);所述液晶性聚合物层(2)中的聚合物网络密度呈梯度分布。
9.根据权利要求8所述的聚合物稳定胆甾相液晶变色玻璃的制备方法,其特征在于,聚合物稳定胆甾相液晶变色玻璃在电致变色领域中的应用。
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