CN115386384A - 可切换光透过率、颜色循环变化的薄膜材料及其制备方法 - Google Patents
可切换光透过率、颜色循环变化的薄膜材料及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:50%~99%液晶单体、1%~40%手性化合物、0.01%~50%离子液体、0.1%~20%液晶性紫外光可聚合单体和光引发剂。本发明可切换光透过率、颜色循环变化的薄膜材料,对普通液晶温控膜的配方做了改进,本发明中加入的离子液体:1‑正丁基3‑甲基咪唑双(三氟甲基磺酰基)酰亚胺([bmim][Tf2N]),实现了温控膜加电控颜色变化的双重效果,而直流电引发的颜色变化的主要作用组分是离子液体,是因为离子液体与液晶分子在直流电作用下发生了氧化还原反应,生成了显色基团,另外交流电引发的颜色交替变化的主要原因与直流电类似,但不同之处在于,液晶分子本身的有序性,使得颜色产生了交替变化。
Description
技术领域
本发明属于新材料技术领域,具体涉及可切换光透过率、颜色循环变化的薄膜材料。
背景技术
目前,颜色变化光学薄膜材料主流是电致变色薄膜材料,但只能实现颜色的变化,不能实现薄膜光透过率变化。也就是说目前的电致变色薄膜多是在透明膜的基础上实现有颜色和没有颜色的变化,但没有在此基础上实现光透过到光不透过的变化,即无法做到在一块薄膜上不同条件下分别在光透过状态和光散射状态实现颜色变化。
为解决上述问题,本发明提供一种可切换光透过率、颜色循环变化的薄膜材料。
发明内容
本发明所要解决的技术问题在于针对上述现有技术的不足,提供一种可切换光透过率、颜色循环变化的薄膜材料,本发明对普通液晶温控膜的配方做了改进,本发明加入的离子液体:1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺([bmim][Tf2N]),实现了温控膜加电控颜色变化的双重效果。
为解决上述技术问题,本发明采用的技术方案是:一种可切换光透过率、颜色循环变化的薄膜材料,其特征在于,由以下质量分数的组分制成:50%~99%液晶单体、1%~40%手性化合物、0.01%~50%离子液体、0.1%~20%液晶性紫外光可聚合单体和光引发剂;所述光引发剂的质量分数是所述液晶性紫外光可聚合单体质量分数的0.5%~2.5%。
优选地,所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb和A的混合物、8cb和B的混合物或,8cb、A和B的混合物;所述液晶单体中所述8cb的用量占比为10%~99%;
优选地,所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯或4-(4-己氧基苯甲酰氧基)苯甲酸-R-(+)-2-辛酯;
所述手性化合物的化学结构式为:
优选地,所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;所述离子液体的化学结构式为:
优选地,所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;所述液晶性紫外光可聚合单体的化学结构式为:
优选地,所述光引发剂为二苯甲酮、安息香双甲醚、氯代硫杂蒽酮、2,4-二乙基硫杂蒽酮、异丙基硫杂蒽酮、2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯甲酮、2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基-1-丙酮、2-苯基-2-N-二甲氨基-1-(4-吗啉苯基)-丁酮或2,4,6-三甲基苯甲酰基-二苯基氧化膦。
本发明还提供上述可切换光透过率、颜色循环变化的薄膜材料的制备方法,该方法包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行室温或加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,降温至室温;将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料。
优选地,所述紫外光辐照的强度为0.1~50mw/cm2,时间为0.5~600s。
优选地,所述具有垂直取向的液晶盒为两片镀有氧化铟锡的玻璃导电层相对而成,两片所述镀有氧化铟锡的玻璃之间的距离为20微米。
优选地,每片所述镀有氧化铟锡的玻璃上镀有聚酰亚胺层。
本发明与现有技术相比具有以下优点:
1、本发明对普通液晶温控膜的配方做了改进,本发明中加入的离子液体:1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺([bmim][Tf2N]),实现了温控膜加电控颜色变化的双重效果,而直流电引发的颜色变化的主要作用组分是离子液体,是因为离子液体与液晶分子在直流电作用下发生了氧化还原反应,生成了显色基团,另外交流电引发的颜色交替变化的主要原因与直流电类似,但不同之处在于,液晶分子本身的有序性,使得颜色产生了交替变化;制备出的薄膜材料通过温度实现透明与不透明的主要作用组分是液晶分子。
2、本发明的原理为由于液晶分子本身的有序性和大于普通电解质的粘度,使得混入其中的离子液体在交流电的作用下显示出随频率变化的颜色变化。随着温度变化可以有透明不透明的切换,且在每个切换后都仍能实现颜色的循环变化,或像在普通电解质中一样,实现施加直流电后,染色并保持。
3、本发明在制备可切换光透过率、颜色循环变化的薄膜材料时采用具有垂直取向的液晶盒,垂直取向液晶盒是为使有序性的液晶分子在灌入液晶盒后具备有序的垂直于界面的取向,从而使薄膜材料在初始状态呈现出透明状态。垂直取向液晶盒的表面镀上聚酰亚胺层,由于聚酰亚胺分子与液晶分子间的相互作用,获得垂直于基板取向的液晶分子。
下面结合附图和实施例对本发明作进一步详细说明。
附图说明
图1(a)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为28℃的情况下为透明无色的图片。
图1(b)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为28℃施加直流电的情况下为透明红色的图片。
图1(c)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为28℃施加低频交流电的情况下为透明黄色的图片。
图1(d)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为28℃施加低频交流电的情况下为透明绿色的图片。
图2(a)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为39℃的情况下为不透明无色的图片。
图2(b)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为39℃施加直流电的情况下为不透明红色的图片。
图2(c)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为39℃施加低频交流电的情况下为不透明黄色的图片。
图2(d)是实施例1中可切换光透过率、颜色循环变化的薄膜材料在温度为39℃施加低频交流电的情况下为不透明绿色的图片。
图3是本发明中具有垂直取向的液晶盒的示意图。
具体实施方式
实施例1
本实施例可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:99%液晶单体、1%手性化合物、0.01%离子液体、0.1%液晶性紫外光可聚合单体和0.025%光引发剂;
所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb和B的混合物;
所述8cb和B的用量比为95:5;
所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯;
所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;
所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;
所述光引发剂为二苯甲酮;
制备本实施例可切换光透过率、颜色循环变化的薄膜材料的制备方法,包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行室温(25℃)搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,自然降温至室温(25℃);将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为30mw/cm2,时间为400s;
所述具有垂直取向的液晶盒为两片镀有氧化铟锡玻璃,导电层(图3中ITO层)相对而成,所述两片镀有氧化铟锡玻璃之间的距离为20微米,两片镀有氧化铟锡玻璃的两端之间采用间隔垫和胶封,液晶混合物通过毛细作用灌入具有垂直取向的液晶盒中,每片所述镀有氧化铟锡的玻璃上镀有聚酰亚胺层。
对本实施例得到的可切换光透过率、颜色循环变化的薄膜材料进行试验:
在温度为28℃时薄膜材料为光透过状态,如图1(a)所示,在这一状态下施加直流电,可以得到红色透明薄膜材料,如图1(b)所示;施加低频交流电,可以得到随频率变化的,颜色由无到红到黄到绿到无的循环变化的透明薄膜材料,如图1(a)-(d)所示。
在温度为39℃时薄膜为光散射状态,即光不透过状态,为白色薄膜(图2(a)所示),在这一状态下施加直流电,可以得到红色不透明薄膜(图2(b)所示);施加低频交流电,可以得到随频率变化的,颜色由无到红到黄到绿到无的循环变化的不透明薄膜,如图2(a)-(d)所示;
本实施例得到的可切换光透过率、颜色循环变化的薄膜材料会在某一点的温度发生相变,对应的就是宏观状态透明与不透明的变化。薄膜材料在其转变温度以上,薄膜材料呈透过状态,在其转变温度以下,薄膜材料呈不透过状态;在直流电的电场强度为2v/微米的情况下,薄膜材料显示红色;在低频交流电的电场强度为2v/微米,频率为0.001hz~50hz的情况下,薄膜材料呈现多种颜色循环转变。
本实施例得到可切换光透过率、颜色循环变化的薄膜材料可以实现6种不同状态切换:即透明无色、不透明无色、透明红色、不透明红色、透明红黄绿循环色、不透明红黄绿循环色。
实施例2
本实施例可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:90%液晶单体、10%手性化合物、10%离子液体、5%液晶性紫外光可聚合单体和0.03%光引发剂;
所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb、A和B的混合物;
所述8cb、A和B的用量比为99:0.5:0.5;
所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯;
所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;
所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;
所述光引发剂为异丙基硫杂蒽酮;
本实施例中,所述液晶单体还可以为8cb和B的混合物,所述8cb和B的用量比为90:10;所述B的化学式:
本实施例中,光引发剂还可以为2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯甲酮、2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基-1-丙酮、2-苯基-2-N-二甲氨基-1-(4-吗啉苯基)-丁酮或2,4,6-三甲基苯甲酰基-二苯基氧化膦。
制备本实施例可切换光透过率、颜色循环变化的薄膜材料的制备方法,包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,自然降温至室温(26℃);将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为20mw/cm2,时间为500s。
本实施例得到可切换光透过率、颜色循环变化的薄膜材料可以实现6种不同状态切换:即透明无色、不透明无色、透明红色、不透明红色、透明红黄绿循环色、不透明红黄绿循环色。
实施例3
本实施例可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:85%液晶单体、15%手性化合物、20%离子液体、9%液晶性紫外光可聚合单体和0.18%光引发剂;
所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb、A和B的混合物;
所述8cb、A和B的用量比为70:20:10;
所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯;
所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;
所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;
所述光引发剂为安息香双甲醚;
制备本实施例可切换光透过率、颜色循环变化的薄膜材料的制备方法,包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,自然降温至室温(26℃);将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为30mw/cm2,时间为200s。
本实施例得到可切换光透过率、颜色循环变化的薄膜材料可以实现6种不同状态切换:即透明无色、不透明无色、透明红色、不透明红色、透明红黄绿循环色、不透明红黄绿循环色。
实施例4
本实施例可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:50%液晶单体、20%手性化合物、50%离子液体、10%液晶性紫外光可聚合单体和0.25%光引发剂;
所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb、A和B;
所述8cb、A和B的用量比为50:30:20;
所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯;
所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;
所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;
所述光引发剂为氯代硫杂蒽酮;
制备本实施例可切换光透过率、颜色循环变化的薄膜材料的制备方法,包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,缓慢降温至室温(25℃);将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为0.1mw/cm2,时间为600s。
本实施例得到可切换光透过率、颜色循环变化的薄膜材料可以实现6种不同状态切换:即透明无色、不透明无色、透明红色、不透明红色、透明红黄绿循环色、不透明红黄绿循环色。
实施例5
本实施例可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:60%液晶单体、40%手性化合物、30%离子液体、20%液晶性紫外光可聚合单体和0.2%光引发剂;
所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb、A和B的混合物;
所述8cb、A和B的用量比为40:30:30;
所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯;
所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;
所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;
所述光引发剂为2-羟基-2-甲基-1-苯基丙酮;
制备本实施例可切换光透过率、颜色循环变化的薄膜材料的制备方法,包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,自然降温至室温(25℃);将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为50mw/cm2,时间为0.5s。
本实施例得到可切换光透过率、颜色循环变化的薄膜材料可以实现6种不同状态切换:即透明无色、不透明无色、透明红色、不透明红色、透明红黄绿循环色、不透明红黄绿循环色。
实施例6
本实施例可切换光透过率、颜色循环变化的薄膜材料,由以下质量分数的组分制成:60%液晶单体、30%手性化合物、40%离子液体、15%液晶性紫外光可聚合单体和0.15%光引发剂;
所述液晶单体为近晶A相到向列相转变的液晶材料,所述液晶单体为8cb、A和B的混合物;
所述8cb和A和B的用量比为10:30:60;
所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-R-(+)-2-辛酯;
所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺;
所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯;
所述光引发剂为2,4,6-三甲基苯甲酰基-二苯基氧化膦;
制备本实施例可切换光透过率、颜色循环变化的薄膜材料的制备方法,包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,自然降温至室温(26℃);将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为40mw/cm2,时间为300s。
本实施例得到可切换光透过率、颜色循环变化的薄膜材料可以实现6种不同状态切换:即透明无色、不透明无色、透明红色、不透明红色、透明红黄绿循环色、不透明红黄绿循环色。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制。凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化,均仍属于本发明技术方案的保护范围内。
Claims (9)
1.一种可切换光透过率、颜色循环变化的薄膜材料,其特征在于,由以下质量分数的组分制成:50%~99%液晶单体、1%~40%手性化合物、0.01%~50%离子液体、0.1%~20%液晶性紫外光可聚合单体和光引发剂;所述光引发剂的质量分数是所述液晶性紫外光可聚合单体质量分数的0.5%~2.5%。
3.根据权利要求1所述的一种可切换光透过率、颜色循环变化的薄膜材料,其特征在于,所述手性化合物为4-(4-己氧基苯甲酰氧基)苯甲酸-S-(+)-2-辛酯或4-(4-己氧基苯甲酰氧基)苯甲酸-R-(+)-2-辛酯。
4.根据权利要求1所述的一种可切换光透过率、颜色循环变化的薄膜材料,其特征在于,所述离子液体为1-正丁基3-甲基咪唑双(三氟甲基磺酰基)酰亚胺。
5.根据权利要求1所述的一种可切换光透过率、颜色循环变化的薄膜材料,其特征在于,所述液晶性紫外光可聚合单体为1,4-双[4-(6-丙烯酰氧基己氧基)苯甲酰氧基]-2-甲基苯。
6.根据权利要求1所述的一种可切换光透过率、颜色循环变化的薄膜材料,其特征在于,所述光引发剂为二苯甲酮、安息香双甲醚、氯代硫杂蒽酮、2,4-二乙基硫杂蒽酮、异丙基硫杂蒽酮、2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯甲酮、2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基-1-丙酮、2-苯基-2-N-二甲氨基-1-(4-吗啉苯基)-丁酮或2,4,6-三甲基苯甲酰基-二苯基氧化膦。
7.如权利要求1-6任一项所述的一种可切换光透过率、颜色循环变化的薄膜材料的制备方法,其特征在于,该方法包括以下步骤:
S1、将所述液晶单体、手性化合物、离子液体、液晶性紫外光可聚合单体和光引发剂混合后,进行室温搅拌或加热搅拌,直至混合均匀,得到液晶混合物;
S2、将S1得到的液晶混合物灌入具有垂直取向的液晶盒中,降温至室温;将装有液晶混合物的液晶盒进行紫外光辐照,得到可切换光透过率、颜色循环变化的薄膜材料;所述紫外光辐照的强度为0.1mw/cm2~50mw/cm2,时间为0.5s~600s。
8.根据权利要求7所述的一种可切换光透过率、颜色循环变化的薄膜材料的制备方法,其特征在于,所述具有垂直取向的液晶盒为两片镀有氧化铟锡的玻璃导电层相对而成,两片所述镀有氧化铟锡的玻璃之间的距离为20微米。
9.根据权利要求8所述的一种可切换光透过率、颜色循环变化的薄膜材料的制备方法,其特征在于,每片所述镀有氧化铟锡的玻璃上镀有聚酰亚胺层。
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