CN108251099B - 一种光照下可凝胶化且自修复的电致变色溶液及其应用 - Google Patents
一种光照下可凝胶化且自修复的电致变色溶液及其应用 Download PDFInfo
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- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1516—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising organic material
- G02F1/15165—Polymers
Abstract
本发明涉及一种电致变色溶液,所述电致变色溶液包含:溶剂、阳极电活性材料、阴极电活性材料以及含芳基丙烯酸酯和/或含芳基丙烯酸内酯的聚合物。此外,本发明还包含所述电致变色溶液的电致变色器件。本发明的电致变色溶液在自然太阳光照下可凝胶化且可自修复,此外,对电致变色溶液的电致变色性能无影响。
Description
技术领域
本发明涉及电致变色领域,更特别地涉及光照下可凝胶化且自修复的电致变色溶液。
背景技术
电致变色是一种电驱动变色技术,是材料在外加电压作用下通过得失电子使材料自身颜色发生变化的过程。其在电致变色窗、汽车后视镜、电致变色眼镜、高分辨率光电摄像器材、光电化学能转换/储存器、军事伪装和装饰材料等具有极大的应用价值。
电致变色器件的基本结构类似三明治,电致变色介质置于由两个镀有导电材料的基底中间。电致变色器件按照电致变色介质物理状态可以分为3类,一类是溶液型电致变色器件,其中,电致变色材料始终溶解在溶剂中。第二类为半溶液型电致变色器件,器件在着色态和透明态之间转换的过程中伴随着电子的传输和材料化学性质的改变,当器件处于透明状态时,电致变色材料溶解于溶剂中;当器件处于着色状态时,电致变色材料会在电极表面富集。第三类为全固态电致变色器件,在器件变色的整个过程中,电致变色材料始终处于固体状态。
在上述三种类型的电致变色器件中,溶液型电致变色器件具有结构简单、制备工艺简便和响应时间短等特点,所以一直是电致变色器件研究的热点并被广泛应用。但是,在长期使用过程中,电致变色溶液可能产生相分离、沉积或缺陷从而影响视觉;此外,由于不可避免的外力作用,可能会导致电致变色器件破裂,从而泄露有毒的电致变色溶液并可能危及到驾驶员或其他人员的安全。
为了克服上述问题,美国专利US5801873采用丙烯酸类的聚合物作为电致变色溶液的增稠剂,从而增加溶液的粘稠度,避免在电致变色器件中产生相分离或沉积,以及降低溶液流动速度,使得在电致变色器件破裂后方便清理和降低有毒物质对人员的伤害。虽然其浓度较高(最佳浓度为7~15%(w/w)),但由于没有交联所以对溶液的凝胶化能力有限;而且在加工方面,其首先在玻璃基底的导电层上通过溶剂挥发制得聚丙烯酸类的薄膜,增加了工艺的复杂性。美国专利US8928966向电致变色溶液中加入具有抗蠕变性能的交联的聚合物电解质,但是聚合物电解质可以导电,对电致变色器件的性能会有一定的影响。中国专利CN201410165629.1向电致变色溶液中引入可经紫外光交联的丙烯酸衍生物,形成的凝胶的稳定性好、工艺简单、能抑制电致变色器件破裂后溶液的流出等,但是对由于撞击导致的凝胶破裂难以修复。
发明内容
本发明的目的在于针对现有技术的不足,提供一种电致变色溶液,其可凝胶化且凝胶破裂后可在自然光照下自修复。此外,本发明还提供了包含所述电致变色溶液的溶液型电致变色器件。
本发明解决上述技术问题的技术方案如下:
一种光照下可凝胶化且自修复的电致变色溶液,包含溶剂、阳极电活性材料、阴极电活性材料、含有式1和/或式2结构单元的聚合物;
式1 式2
式1中,Ar为芳基或取代芳基; 式2中,R为H、C1~10烃基或OH。
本发明中,包含式1、式2结构单元的聚合物具有共同的芳基丙烯酸酯(式2为自身环合形成内酯)的共轭体系,可发生自动断键和结合的平衡反应,进而赋予所述的电致变色溶液在光照条件下形成凝胶和自修复功能。
本发明中,包含式1和/或式2结构单元的聚合物在光照条件下发生自动断键和结合的平衡反应机理如方程式1所示:
方程式1
作为优选,所述的电致变色溶液包含具有式3结构单元的聚合物(本发明也称为包含邻氧萘酮单元的聚合物):
式3。
本发明中,式1中,Ar例如可为苯基、取代苯基、萘环、取代萘环等。
作为优选,式1中,Ar为苯基或取代苯基;优选的具有式1结构单元的聚合物的结构式如式4:
式4
式4中,R1为H、C1~4烃基。
更进一步优选,式4中,R1为H。本发明中,优选的式4结构单元的聚合物也称为包含肉桂酰氧单元的聚合物。
所述的聚合物为包含所述式1和/或式2结构单元例如包含肉桂酰氧基团和/或邻氧萘酮基团的线性结构聚合物,也可以是支化结构聚合物。
进一步优选,所述的聚合物为包含所述式1和/或式2结构单元的超支化聚合物。
超支化聚合物由于支化度高,分子链缠结少,因此与相同分子量的线性聚合物相比,其黏度低得多,溶解性好且方便注入电致变色器件中;其次,超支化聚合物具有高度的分枝结构,固化时收缩率小。
本发明中,所述的包含所述式1和/或式2结构单元的聚合物优选为含有酰胺键、酰亚胺键、醚键、酯键、氨酯键、羟基、酮基、羧基、硝基、氰基或巯基的超支化聚合物,上述基团的存在有助于所述聚合物在常用的电致变色溶液的极性溶剂中溶解。
所述的聚合物可以在与所述溶剂、阳极电活性材料和阴极电活性材料混合之前合成,也可以通过单体反应并在与所述溶剂、阳极电活性材料和阴极电活性材料混合之后形成。
作为优选,所述的聚合物通过单体反应并在与所述溶剂、阳极电活性材料和阴极电活性材料混合之后形成,采用该方法可降低电致变色溶液的起始粘稠度,方便注入电致变色器件中。
本发明中,所述的电致变色溶液中,所述的聚合物的浓度为1~15 %(w/v);
所述的单位%(w/v)为所述的聚合物的质量除以电致变色溶液的体积。本发明中,所述的聚合物的浓度低于1%(w/v),凝胶强度差且自修复缓慢;当所述的聚合物的浓度高于15%(w/v),交联度高从而导致凝胶存在收缩现象。
所述的电致变色溶液中,所述的聚合物的浓度进一步优选为2~5 %(w/v)。
所述的阳极电活性材料选自三苯胺、取代的三苯胺、二茂铁、取代的二茂铁、二茂铁盐、取代的二茂铁盐、吩噻嗪、取代的吩噻嗪、噻嗯、取代的噻嗯、吩嗪和取代的吩嗪中的至少一种。
作为优选,所述的电致变色溶液中,所述的阳极电活性材料的浓度为0.001~0.5mmol/L;进一步优选为0.002~0.1 mmol/L。
作为优选,所述的阴极电活性材料选自紫精、取代的紫精、葱醌和取代的蒽醌中的至少一种。
作为优选,所述的电致变色溶液中,所述的阴极电活性材料的浓度为0.001~0.55mmol/L;进一步优选为0.002~0.1 mmol/L。
本发明中,所述的溶剂选自对所述的聚合物、阳极电活性材料和阴极电活性材料具有良好溶解或溶胀能力且不发生化学反应的化学试剂。
作为优选,所述的溶剂为碳酸丙烯酯、丁内酯、2-乙酰基丁内酯、γ-戊内酯、碳酸乙烯酯、环丁砜、3-甲基环丁砜、二甲基乙酰胺、二甲基甲酰胺、乙腈、戊二腈、2-甲基戊二腈、3-羟基丙腈、四乙二醇二甲醚、二甲基亚砜、乙氧基乙醇和环戊酮中的至少一种。
本文术语“电活性”被定义为在暴露于特定的电势差下时,经历其氧化态的改变。阴极电活性材料在电场作用下通过从阴极接受电子被还原;阳极电活性材料在电场作用下通过向阳极供给电子被氧化。阴极电活性材料和阳极电活性材料配合使用能够起到平衡电荷的作用。其中,所述阳极电活性材料和阴极电活性材料中的至少一种为电致变色材料,即具备电致变色性能。
在所述电致变色溶液中,还可添加其它功能性材料,如紫外光稳定剂、热稳定剂、抗氧化剂、增稠剂、粘度改性剂和氧化还原稳定剂。
本发明还包括一种电致变色器件,包括前基底和后基底;所述的前基底某一表面镀制有导电材料,所述的后基底某一表面镀制有导电材料;所述的前基底的导电材料的表面和后基底的导电材料的表面相向放置,并通过密封胶粘结周围从而形成密封腔室,所述的密封腔室内填充有所述的电致变色溶液。
所述前基底或后基底可以是由任何具有足以使该电致变色器件在所暴露的环境中使用的强度和可加工成预定形状的材料制造。
作为优选,所述的前基底和后基底独自选自聚甲基丙烯酸甲酯、聚酯、聚氯乙烯、聚偏氯乙烯、聚酰胺、聚酰亚胺、聚丙烯、聚乙烯、聚碳酸酯等有机高分子材料,以及玻璃、陶瓷、金属中的至少一种。
进一步优选,所述的前基底和后基底材质相同;
作为优选,所述的前基底和后基底为玻璃。
作为优选,所述的前基底和后基底镀制的导电材料独自选自氧化锡、氧化锌、氧化锡铟、氧化铟镓锌复合物、掺氟氧化锡、掺铝氧化锌和掺氟氧化锌中的至少一种。
除导电材料外,根据具体使用时对功能和性能的要求,在基底上可以涂布例如反射材料、抗反射材料、亲水材料、紫外光阻挡材料等功能性材料;
例如,为适应具体的功能和性能的要求,预先在所述的前基底和后基底的表面镀制反射材料、抗反射材料、亲水材料、紫外光阻挡材料等至少一种功能性材料后再镀制所述的导电材料。
本发明还包括所述的溶液型电致变色器件的应用,应用于交通工具的后视镜、建筑和飞机的窗户、滤光器、装饰材料、隐身材料、信息显示和军事技术等。
一种优选的应用,将所述的电致变色器件用于组装制备建筑渐变玻璃、车用智能变色窗、飞机舷窗、变色太阳眼镜或汽车防弦目后视镜。
同现有技术相比,本发明的有益效果体现在:
本发明通过加入在自然光照下可形成交联网络结构的聚合物来实现电致变色溶液的凝胶化,从而抑制电致变色溶液内产生相分离或沉积,以及在电致变色器件破裂时溶液泄露等不良现象。而且,对由于外界撞击等导致的微裂纹,通过光照即可实现自愈合,从而对延长电致变色器件的使用寿命具有显著的作用。
附图说明
图1是本发明应用例所述的电致变色器件的剖面图。图中,1和2是玻璃基底;3和4是玻璃基底上镀的透明导电材料;5是边框胶;6是填充电致变色溶液的空腔。
具体实施方式
以下结合具体实施例对本发明作进一步详细描述,有必要指出的是本实施例只用于对本发明进行进一步的说明,不能理解为对本发明保护范围的限制。
实施例1:
以肉桂酰氯和过量的丁二醇为原料,以吡啶为盐酸吸收剂,于室温反应2小时(反应式如下式所示),反应结束后加入乙酸乙酯,再用水洗涤3次,有机相经减压蒸馏除去溶剂,得到结构式1所示的化合物。
将结构式1所示的化合物与4,4',4''-三苯基甲烷三异氰酸酯、六亚甲基二异氰酸酯、丁二醇、微量有机锡催化剂二月桂酸二丁基锡、1,1’-二新戊基-4,4’-联吡啶双(六氟硼酸盐)与5,10-二异丙基-5,10-二甲基吩嗪溶解于碳酸丙烯酯中,配成电致变色溶液(结构式1所示的化合物的浓度为10 mmol/L;4,4',4''-三苯基甲烷三异氰酸酯的浓度为20mmol/L;六亚甲基二异氰酸酯的浓度为10 mmol/L;丁二醇的浓度为35 mmol/L;1,1’-二新戊基-4,4’-联吡啶双(六氟硼酸盐)的浓度为50 mmol/L;5,10-二异丙基-5,10-二甲基吩嗪的浓度为50 mmol/L;),灌注于如图1所示的电致变色器件中,然后用胶封口,即得到具有电致变色功能的器件。
测试结果:上述电致变色溶液于室温~30度自然光照(太阳光辐射强度介于60-115W/m2)4小时,凝胶化;凝胶切开后,自然光照7小时,修复完好。制得的电致变色器件在无外加电压情况下测得的500 nm波长光的反射率为77%,通电之后测得的500 nm波长光的反射率为5.4%;在室温下通电循环10000次(电致变色器件通电5秒后断电5秒为一个循环),在无外加电压情况下测得的500 nm波长光的反射率为75%,通电之后测得的500 nm波长光的反射率为5.6%。
实施例2:
利用原子转移自由基聚合法,以结构式2所示的香豆素型苯乙烯(结构式2所示化合物)和丙烯酸甲氧基乙酯(摩尔比为1:4)为聚合单体、以2-溴丙酸乙酯为引发剂,以CuCl/Me10TATD为催化剂,于二氧六环溶剂中60度反应24小时,得到结构式3所示的聚合物。
将结构式3所示的聚合物、1,1’-二己基-4,4’-联吡啶双(三氟甲磺酸盐)与5,10-二氢-5,10-二甲基吩嗪溶解于丁内酯中,配成电致变色溶液(结构式3所示的化合物的浓度为5 %(w/v);1,1’-二己基-4,4’-联吡啶双(三氟甲磺酸盐)的浓度为50 mmol/L;5,10-二氢-5,10-二甲基吩嗪的浓度为50 mmol/L;),灌注于如图1所示的电致变色器件中,然后用胶封口,即得到具有电致变色功能的器件。
测试结果:上述电致变色溶液于室温~30度自然光照(太阳光辐射强度介于60-115W/m2)7小时,凝胶化;凝胶切开后,自然光照12小时,修复完好。制得的电致变色器件在无外加电压情况下测得的500 nm波长光的反射率为68%,通电之后测得的500 nm波长光的反射率为4.3%;在室温下通电循环10000次(电致变色器件通电5秒后断电5秒为一个循环),在无外加电压情况下测得的500 nm波长光的反射率为66%,通电之后测得的500 nm波长光的反射率为5.2%。
上述实施例中的电致变色溶液采用常温自然太阳光照交联从而实现溶液的凝胶化,其工艺简单,形成的凝胶自修复性好,且对电致变色器件的性能无影响。
Claims (4)
1.一种光照下可凝胶化且自修复的电致变色溶液的制备方法,其特征在于,所述电致变色溶液的制备方法为:以肉桂酰氯和过量的丁二醇为原料,以吡啶为盐酸吸收剂,于室温反应2小时,反应结束后加入乙酸乙酯,再用水洗涤3次,有机相经减压蒸馏除去溶剂,得到如下所示的中间化合物;
将所述中间化合物与4,4',4”-三苯基甲烷三异氰酸酯、六亚甲基二异氰酸酯、丁二醇、微量有机锡催化剂二月桂酸二丁基锡、1,1'-二新戊基-4,4'-联吡啶双(六氟硼酸盐)与5,10-二异丙基-5,10-二甲基吩嗪溶解于碳酸丙烯酯中,配成电致变色溶液;所述中间化合物的浓度为10mmol/L;4,4',4”-三苯基甲烷三异氰酸酯的浓度为20mmol/L;六亚甲基二异氰酸酯的浓度为10mmol/L;丁二醇的浓度为35mmol/L;1,1’-二新戊基-4,4’-联吡啶双(六氟硼酸盐)的浓度为50mmol/L;5,10-二异丙基-5,10-二甲基吩嗪的浓度为50mmol/L。
2.一种溶液型电致变色器件,其特征在于,包括前基底和后基底;所述的前基底某一表面镀制有导电材料,所述的后基底某一表面镀制有导电材料;所述的前基底的导电材料的表面和后基底的导电材料的表面通过密封胶复合并形成密封腔室,所述的密封腔室内填充有权利要求1所制备得到的电致变色溶液。
3.如权利要求2所述的溶液型电致变色器件,其特征在于,所述的前基底和后基底镀制的导电材料独自选自氧化锡、氧化锌、氧化锡铟、氧化铟镓锌复合物、掺氟氧化锡、掺铝氧化锌和掺氟氧化锌中的至少一种。
4.一种权利要求2或3所述的溶液型电致变色器件的应用,其特征在于,用于组装制备建筑渐变玻璃、车用智能变色窗、飞机舷窗、变色太阳眼镜或汽车防弦目后视镜。
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