CN114892392A - 一种电致发光变色纤维及其制备方法和应用 - Google Patents

一种电致发光变色纤维及其制备方法和应用 Download PDF

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CN114892392A
CN114892392A CN202210442656.3A CN202210442656A CN114892392A CN 114892392 A CN114892392 A CN 114892392A CN 202210442656 A CN202210442656 A CN 202210442656A CN 114892392 A CN114892392 A CN 114892392A
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陈培宁
向阳
吴景霞
彭慧胜
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Fudan University
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Abstract

本发明涉及一种电致发光变色纤维及其制备方法和应用。制备方法包括以下步骤：(1)制备发光活性纤维：将发光浆料涂覆在导电纤维基底上，加热烘干，得到涂有多层电致发光活性层的发光活性纤维；(2)制备变色纤维：将外电极负载于发光活性纤维表面，得到电致变色纤维；(3)制备绝缘变色纤维：在电致变色纤维外部涂覆透明绝缘聚合物，得到涂有透明绝缘封装层的电致发光变色纤维。该电致发光变色纤维的应用领域包括彩色显示、智能家居、功能服饰、汽车内饰等。与现有技术相比，本发明具有变色材料加工性能好、变色形式不单一等优点。

Description

一种电致发光变色纤维及其制备方法和应用
技术领域
本发明涉及智能电子器件技术领域，具体涉及一种电致发光变色纤维及其制备方法和应用。
背景技术
发光器件已成为信息传递的重要窗口，推动着信息技术的快速发展，随着可穿戴电子器件的迅猛发展，对发光器件的要求也越来越高。
目前，对于电致变色的研究多集中于变色材料本身的制备合成，比如电致变色共轭聚合物和无机小分子电致变色材料等等，但是这些材料有着分散性不好，加工成膜性差等缺点影响到变色性能，目前多数处于实验室研究阶段，离产业化之路比较远。而且材料的变色形式比较单一，仅仅体现在颜色发生变化，由于没有发光效果，在夜晚的应用受到限制。
因此，如果能够将发光效果和变色效果结合起来，将会较大地拓宽该智能电子器件的应用领域和使用条件。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种变色材料加工性能好、变色形式不单一的电致发光变色纤维及其制备方法和应用。
本发明的目的可以通过以下技术方案来实现：
本发明利用不同的单色电致发光材料，通过双活性层结构设计，实现了实时可逆可调的发光变色纤维。由于该变色纤维具备超柔、可编织等特点，可以将其与传统纤维相结合进行织造，在可穿戴电子织物领域具有重要的应用价值，具体方案如下：
本发明提供的变色纤维，包括：(1)导电纤维，作为纤维基底电极，该导电纤维表面修饰有聚合物绝缘层；(2)多种发光活性层，依次涂覆在绝缘聚合物修饰的导电纤维表面；(3)外电极，包括但不限于金属丝或金属粒子，平行、缠绕或涂覆在涂覆了多层发光聚合物活性层的导电纤维基底上；(4)透明封装层，浸涂在变色纤维上，从而形成电极-发光层-电极结构，即三明治结构。
一种电致发光变色纤维的制备方法，该方法包括以下步骤：
(1)制备发光活性纤维：将发光浆料涂覆在导电纤维基底上，加热烘干，得到涂有多层电致发光活性层的发光活性纤维；
(2)制备变色纤维：将外电极负载于发光活性纤维表面，得到电致变色纤维；
(3)制备绝缘变色纤维：在电致变色纤维外部涂覆透明绝缘聚合物，得到涂有透明绝缘封装层的电致发光变色纤维。
进一步地，所述的电致发光活性层包括2-3层，步骤(1)的具体步骤为：
(1-1)将电致发光材料、溶剂、胶粘剂和表面活性剂混合后，得到发光浆料；
(1-2)将发光浆料涂覆在导电纤维基底上，加热烘干；
(1-3)重复上述步骤，得到涂有多层电致发光活性层的发光活性纤维。
进一步地，所述的电致发光材料包括SiO2基电致发光材料或金属硫化物型电致发光材料，电致发光材料的粒径为10-60μm，优选20-50μm；电致发光材料在电致发光活性层中的占比为10-90wt％，优选30-60wt％。
进一步地，所述的SiO2基电致发光材料包括SiO2:Ge或SiO2:Er；所述金属硫化物型电致发光材料包括CaS、SrS、ZnS、CaGa2S4或SrGa2S4。
进一步地，所述的导电纤维包括镀金属纳米粒子化学纤维、离子凝胶纤维、金属导电纤维或导电聚合物覆盖纤维中的一种或多种，导电纤维的直径为50-400μm，优选100-300μm；导电纤维的电导率为10-3-104S/cm，优选10-3-10-1S/cm。
进一步地，所述的涂覆包括浸涂、烘干和卷绕；
所述浸涂的时间在5-30s；所述烘干的温度为60-200℃，优选100-150℃；所述卷绕的速度为3-10m/min；单层电致发光活性层的厚度为20-200μm，优选40-100μm。
进一步地，所述的外电极包括金属丝或金属粒子，负载方式包括平行负载、缠绕或涂覆；
所述的金属丝包括铜丝、钢丝、钛丝或钨丝；所述的金属粒子包括导电银胶、银纳米线、铜纳米线或纳米银；
负载方式为平行排列时，排列间距为0.1-2mm，优选0.4-1mm；
负载方式为缠绕时，螺距为0.1-2mm，优选0.4-1mm；缠绕速度为1-10m/min，优选地3-7m/min。
负载方式为涂覆时，浸涂时间为5-30s，浸涂后，在温度为60-200℃，优选100-150℃下烘干。
进一步地，所述的绝缘聚合物为溶剂型固态树脂，包括聚乙烯、聚丙烯、聚氯乙烯、聚苯乙烯、ABS、聚四氟乙烯、聚对苯二甲酸乙二酯、聚芳酯、聚氨酯树脂或聚酰胺；绝缘聚合物的重均分子量(Mw)为8万-15万，透明绝缘封装层的厚度为5-100μm，优选20-50μm。
一种如上所述方法制备的电致发光变色纤维。
一种如上所述电致发光变色纤维的应用，该电致发光变色纤维应用于彩色显示、智能家居、功能服饰或汽车内饰。
与现有技术相比，本发明具有以下优点：
(1)本发明的变色纤维能够随着电压的变化显示出不同的颜色、具有优异电致变色性能、使用寿命长、直径可控；
(2)本发明工艺，通过溶液加工的方法，简单、高效，条件温和，成本低，适合工业化生产；
(3)本发明方法通过引入不同颜色发光粉可以实现各种颜色的实时变化，较大地拓宽了变色范围,在功能服饰领域具有广阔的应用前景。
附图说明
图1为本发明发光变色纤维制备示意图。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
一种电致发光变色纤维的制备方法，该方法包括以下步骤：
(1)制备发光活性纤维：将发光浆料涂覆在导电纤维基底上，加热烘干，得到涂有2-3层电致发光活性层的发光活性纤维；
(1-1)将电致发光材料、溶剂、胶粘剂和表面活性剂混合后，得到发光浆料；
(1-2)将发光浆料涂覆在导电纤维基底上，加热烘干；
(1-3)重复上述步骤，得到涂有多层电致发光活性层的发光活性纤维。
电致发光材料包括SiO2基电致发光材料或金属硫化物型电致发光材料，电致发光材料的粒径为10-60μm，优选20-50μm；电致发光材料在电致发光活性层中的占比为10-90wt％，优选30-60wt％。SiO2基电致发光材料包括SiO2:Ge或SiO2:Er；所述金属硫化物型电致发光材料包括CaS、SrS、ZnS、CaGa2S4或SrGa2S4。
导电纤维包括镀金属纳米粒子化学纤维、离子凝胶纤维、金属导电纤维或导电聚合物覆盖纤维中的一种或多种，导电纤维的直径为50-400μm，优选100-300μm；导电纤维的电导率为10-3-104S/cm，优选10-3-10-1S/cm。
涂覆包括浸涂、烘干和卷绕；浸涂的时间在5-30s；所述烘干的温度为60-200℃，优选100-150℃；所述卷绕的速度为3-10m/min；单层电致发光活性层的厚度为20-200μm，优选40-100μm。
(2)制备变色纤维：将外电极负载于发光活性纤维表面，得到电致变色纤维；外电极包括金属丝或金属粒子，负载方式包括平行负载、缠绕或涂覆；金属丝包括铜丝、钢丝、钛丝或钨丝；所述的金属粒子包括导电银胶、银纳米线、铜纳米线或纳米银；
负载方式为平行排列时，排列间距为0.1-2mm，优选0.4-1mm；
负载方式为缠绕时，螺距为0.1-2mm，优选0.4-1mm；缠绕速度为1-10m/min，优选地3-7m/min。
负载方式为涂覆时，浸涂时间为5-30s，浸涂后，在温度为60-200℃，优选100-150℃下烘干。
(3)制备绝缘变色纤维：在电致变色纤维外部涂覆透明绝缘聚合物，得到涂有透明绝缘封装层的电致发光变色纤维。绝缘聚合物为溶剂型固态树脂，包括聚乙烯、聚丙烯、聚氯乙烯、聚苯乙烯、ABS、聚四氟乙烯、聚对苯二甲酸乙二酯、聚芳酯、聚氨酯树脂或聚酰胺；绝缘聚合物的重均分子量(Mw)为8万-15万，透明绝缘封装层的厚度为5-100μm，优选20-50μm。该电致发光变色纤维应用于彩色显示、智能家居、功能服饰或汽车内饰。
在符合本领域常识的基础上，上述各优越条件，可任意组合，即得本发明各较佳实例。
本发明所用试剂和原料均市售可得。本发明中，室温是指环境温度为10-30℃。
以下实施例中使用的试剂均为外购试剂，其中各种溶剂均购自国药化学试剂有限公司。以下实施例中各种设备皆为市售设备。
以下各实施例中变色纤维制备示意图可参考图1。
实施例1
第一步：在室温25℃下，将30g铜掺杂的市售硫化锌粉(直径28μm)加入到50g N-甲基吡咯烷酮溶剂中，然后加入28.7g氰乙基纤维素胶黏剂，0.5g十二烷基苯磺酸钠表面活性剂，磁力搅拌30min，搅拌速度为500rpm，得到分散均匀的浆料1；将40g锰掺杂的市售硫化锌粉(直径20μm)加入到50g去离子水中，然后加入48.6g聚氨酯胶黏剂，0.4g十二烷基苯磺酸钠表面活性剂，磁力搅拌35min，搅拌速度为400rpm，得到分散均匀的浆料2。将10g聚乙烯加入到20g十氢萘溶剂中，然后加入0.2g十二烷基苯磺酸钠表面活性剂，磁力搅拌30min，搅拌速度为400rpm，得到分散均匀的浆料3；
第二步：开启连续浸涂装置，将浆料1以7m/min的速度均匀涂覆在铜丝纤维(直径150μm)表面，然后180℃在线烘干，直径达到190μm；将浆料2以8m/min的速度均匀涂覆在涂有浆料1的铜丝纤维上，然后100℃在线烘干，直径达到230μm；将浆料3以8m/min的速度均匀涂覆在涂有浆料2的铜丝纤维上，得到变色纤维，总直径为260μm，最后收集并卷绕在线轴上。
第三步：开启绕外电极装置，将铜丝(直径100μm)以5m/min的速度缠绕在步骤二得到的变色纤维上，螺距为0.4mm，最后收集并卷绕在线轴上。
第四步：开启封装装置，将60wt％聚对苯二甲酸乙二酯溶液以10m/min速度均匀涂覆在纤维表面，然后150℃在线烘干，最后收集并卷绕在线轴上，得到封装的双活性层发光变色纤维，封装层厚度控制在20μm左右。
所制得变色纤维，在内电极和外电极之间施加2千赫兹，60-150V的正弦交流电压，实现从橙光到白光再到蓝光的变色范围。由于柔性的内电极、活性层厚度的精细控制，双活性层发光变色纤维在弯折，水洗后依然变色均匀和稳定工作。
实施例2
第一步：在室温25℃下，将30g铜掺杂的市售CaS粉(直径20μm)加入到60g丙酮溶剂中，然后加入33.4g聚偏氟乙烯胶黏剂，0.4g十六烷基苯磺酸钠表面活性剂，磁力搅拌30min，搅拌速度为500rpm，得到分散均匀的浆料1；将30g锰掺杂的市售GaN粉(直径30μm)加入到50g间二甲苯溶剂中，然后加入52.4g SBS胶黏剂，0.3g十六烷基苯磺酸钠表面活性剂及其他助剂，磁力搅拌35min，搅拌速度为500rpm，得到分散均匀的浆料2；将15g聚四氟乙烯加入到30g丙酮溶剂中，然后加入0.3g十六烷基苯磺酸钠表面活性剂，磁力搅拌30min，搅拌速度为500rpm，得到分散均匀的浆料3。
第二步：开启连续浸涂装置，将浆料1以10m/min的速度均匀涂覆在铜丝纤维(直径100μm)表面，然后150℃在线烘干，直径达到150μm；将浆料2以10m/min的速度均匀涂覆在涂有浆料1的铜丝纤维上，然后100℃在线烘干，直径达到200μm；将浆料3以10m/min的速度均匀涂覆在涂有浆料2的铜丝纤维上，得到变色纤维，直径为240μm，最后收集并卷绕在线轴上。
第三步：开启绕外电极装置，将铜丝(直径100μm)以7m/min的速度缠绕在步骤二得到的变色纤维上，螺距为0.5mm，最后收集并卷绕在线轴上。
第四步：开启封装装置，将40wt％丙烯酸酯树脂溶液以8m/min速度均匀涂覆在纤维表面，然后120℃在线烘干，最后收集并卷绕在线轴上，得到封装的双活性层发光变色纤维，封装层厚度控制在25μm左右。
所制得变色纤维，在内电极和外电极之间施加50赫兹，60-120V的正弦交流电压，实现从橙光到白光再到绿光的变色范围。由于柔性的内电极、活性层厚度的精细控制，双活性层发光变色纤维在弯折，水洗后依然变色均匀和稳定工作。
实施例3
第一步：在室温25℃下，将30g铜掺杂的市售CaS粉(直径20μm)加入到40g N,N-二甲基甲酰胺溶剂中，然后加入28.9g环氧树脂胶黏剂，0.2g吐温80表面活性剂，磁力搅拌40min，搅拌速度为600rpm，得到分散均匀的浆料1；将30g锰掺杂的市售GaN粉(直径30μm)加入到70g甲苯溶剂中，然后加入64.3g ABS胶黏剂，0.4g吐温80表面活性剂，磁力搅拌40min，搅拌速度为500rpm，得到分散均匀的浆料2；将20g聚氨酯加入到40g去离子水溶剂中，然后加入0.3g吐温80表面活性剂，磁力搅拌40min，搅拌速度为400rpm，得到分散均匀的浆料3。
第二步：开启连续浸涂装置，将浆料1以8m/min的速度均匀涂覆在铜丝纤维(直径120μm)表面，然后150℃在线烘干，直径达到160μm；将浆料2以12m/min的速度均匀涂覆在涂有浆料1的铜丝纤维，然后120℃在线烘干，直径达到200μm；将浆料3以12m/min的速度均匀涂覆在涂有浆料2的铜丝纤维上，得到变色纤维，直径为250μm，最后收集并卷绕在线轴上。
第三步：开启绕外电极装置，将铜丝(直径80μm)以5m/min的速度缠绕在步骤二得到的变色纤维上，螺距为0.6mm，最后收集并卷绕在线轴上。
第四步：开启封装装置，将30wt％聚偏氟乙烯树脂溶液以10m/min速度均匀涂覆在纤维表面，然后150℃在线烘干，最后收集并卷绕在线轴上，得到封装的双活性层发光变色纤维，封装层厚度控制在30μm左右。
所制得变色纤维，在内电极和外电极之间施加2千赫兹，60-150V的正弦交流电压，实现从橙光到白光再到绿光的变色范围。由于柔性的内电极、活性层厚度的精细控制，双活性层发光变色纤维在弯折，水洗后依然变色均匀和稳定工作。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。

Claims (10)

1.一种电致发光变色纤维的制备方法，其特征在于，该方法包括以下步骤：
(1)制备发光活性纤维：将发光浆料涂覆在导电纤维基底上，加热烘干，得到涂有多层电致发光活性层的发光活性纤维；
(2)制备变色纤维：将外电极负载于发光活性纤维表面，得到电致变色纤维；
(3)制备绝缘变色纤维：在电致变色纤维外部涂覆透明绝缘聚合物，得到涂有透明绝缘封装层的电致发光变色纤维。
2.根据权利要求1所述的一种电致发光变色纤维的制备方法，其特征在于，所述的电致发光活性层包括2-3层，步骤(1)的具体步骤为：
(1-1)将电致发光材料、溶剂、胶粘剂和表面活性剂混合后，得到发光浆料；
(1-2)将发光浆料涂覆在导电纤维基底上，加热烘干；
(1-3)重复上述步骤，得到涂有多层电致发光活性层的发光活性纤维。
3.根据权利要求2所述的一种电致发光变色纤维的制备方法，其特征在于，所述的电致发光材料包括SiO2基电致发光材料或金属硫化物型电致发光材料，电致发光材料的粒径为10-60μm，优选20-50μm；电致发光材料在电致发光活性层中的占比为10-90wt％，优选30-60wt％。
4.根据权利要求3所述的一种电致发光变色纤维的制备方法，其特征在于，所述的SiO2基电致发光材料包括SiO2:Ge或SiO2:Er；所述金属硫化物型电致发光材料包括CaS、SrS、ZnS、CaGa2S4或SrGa2S4。
5.根据权利要求1所述的一种电致发光变色纤维的制备方法，其特征在于，所述的导电纤维包括镀金属纳米粒子化学纤维、离子凝胶纤维、金属导电纤维或导电聚合物覆盖纤维中的一种或多种，导电纤维的直径为50-400μm，优选100-300μm；导电纤维的电导率为10-3-104S/cm，优选10-3-10-1S/cm。
6.根据权利要求1所述的一种电致发光变色纤维的制备方法，其特征在于，所述的涂覆包括浸涂、烘干和卷绕；
所述浸涂的时间在5-30s；所述烘干的温度为60-200℃，优选100-150℃；所述卷绕的速度为3-10m/min；单层电致发光活性层的厚度为20-200μm，优选40-100μm。
7.根据权利要求1所述的一种电致发光变色纤维的制备方法，其特征在于，所述的外电极包括金属丝或金属粒子，负载方式包括平行负载、缠绕或涂覆；
所述的金属丝包括铜丝、钢丝、钛丝或钨丝；所述的金属粒子包括导电银胶、银纳米线、铜纳米线或纳米银；
负载方式为平行排列时，排列间距为0.1-2mm，优选0.4-1mm；
负载方式为缠绕时，螺距为0.1-2mm，优选0.4-1mm；缠绕速度为1-10m/min，优选地3-7m/min。
负载方式为涂覆时，浸涂时间为5-30s，浸涂后，在温度为60-200℃，优选100-150℃下烘干。
8.根据权利要求1所述的一种电致发光变色纤维的制备方法，其特征在于，所述的绝缘聚合物为溶剂型固态树脂，包括聚乙烯、聚丙烯、聚氯乙烯、聚苯乙烯、ABS、聚四氟乙烯、聚对苯二甲酸乙二酯、聚芳酯、聚氨酯树脂或聚酰胺；绝缘聚合物的重均分子量(Mw)为8万-15万，透明绝缘封装层的厚度为5-100μm，优选20-50μm。
9.一种如权利要求1-8任一项所述方法制备的电致发光变色纤维。
10.一种如权利要求9所述电致发光变色纤维的应用，其特征在于，该电致发光变色纤维应用于彩色显示、智能家居、功能服饰或汽车内饰。
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