CN110320722B - 可见光至中红外等离激元异质微腔电致变色器件 - Google Patents

可见光至中红外等离激元异质微腔电致变色器件 Download PDF

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CN110320722B
CN110320722B CN201910669423.5A CN201910669423A CN110320722B CN 110320722 B CN110320722 B CN 110320722B CN 201910669423 A CN201910669423 A CN 201910669423A CN 110320722 B CN110320722 B CN 110320722B
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张彤
苏丹
杨毅
秦妍妍
张晓阳
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Abstract

本发明公开了可见光至中红外等离激元异质微腔电致变色器件，由阵列化的电致变色单元所组成，每个电致变色单元具体结构包括透明导电顶电极、电解液层、电解液框、介孔核壳结构层、底电极及驱动电路。该电致变色器件利用电致还原及氧化的方式在纳米核壳结构的介孔中实现金属原子的吸附，可快速改变纳米核壳结构的结构，通过动态调控其局域表面等离激元谐振峰的方式实现器件光谱及颜色的控制，颜色变色速度优于20 s,变色范围可覆盖可见光到中红外宽谱波段；此外，利用表面等离激元纳米核壳结构的突破衍射极限的光操控特性，可以将像素单元进一步减小，结合光学系统实现电致变色器件空间分辨率达到光学衍射极限。

Description

可见光至中红外等离激元异质微腔电致变色器件
技术领域
本发明属于可见光伪装、金属纳米材料等领域，具体是一种可见光至中红外等离激元异质微腔电致变色器件。
背景技术
变色材料在智能玻璃、伪装、显示等多领域具有广泛应用。常见可见光变色材料主要可以分为无机类和有机类两种。早期，可见光无机变色材料主要包括卤化银，氧化钨体材料等，近年来，无机变色材料的表现形式更为丰富，且表现出化学性质稳定、寿命长、实用性较强等显著优点。然而，大部分无机变色材料存在颜色变化单一、响应速度慢等问题，限制了其伪装应用场合。相对于通常的无机材料，有机变色材料可变颜色多样，响应速度相对较快，可以实现宽色域变色，然而有机材料通常耐久性差、寿命较短，此外，有机材料容易受温度影响，在高温下容易变形，影响材料变色性能，且有机变色材料通常在红外波段也有较强的吸收，难满足现代化伪装技术对伪装材料的多谱兼容性等需求。因此，能够同时满足色域覆盖范围广、快速响应、多谱兼容性好、寿命长的可见光变色材料及变色机制仍然亟待发展，需引入新理论与新机制。
目前基于金属-介质复合结构的表面等离激元超材料的突破传统光学衍射极限的特性及颜色随材质、尺寸及结构的变化已经得到广泛研究，在变色材料方面展示出远优于传统材料的特性，如光谱色谱可精细调控、单种结构实现颜色多色变化，光学截面大、稳定性好等特点。
本发明利用等离激元纳米颗粒的局域表面等离激元效应，针对现有变色材料变色范围小、响应时间长、稳定性差的问题等瓶颈问题，并结合新机理、新技术提出了一种可见光至中红外等离激元异质微腔电致变色器件，提出了一种利用介孔纳米核壳结构的介孔作为金属生长模板，实现等离激元材料之间的去耦及器件颜色的宽色域调控。变色器件具有色彩调节范围大、空间分辨率高、稳定性高、尺寸小及低成本等优点，可广泛应用于自适应伪装、智能玻璃等领域。
发明内容
本发明的目的是解决已有变色材料的变色速度慢、无法覆盖宽色域、空间分辨率低及稳定性差等等技术问题，提出一种可见光至中红外等离激元异质微腔电致变色器件，利用介孔纳米结构中的介孔作为模板，可有效降低表面等离激元结构间的耦合，并可实现更宽光谱的表面等离激元谐振调谐，实现宽色域变色；该变色器件具有色彩调节范围大、空间分辨率高、稳定性高、尺寸小及低成本等优点，可广泛应用于自适应伪装、智能玻璃等领域。
为达到上述目的，本发明提出一种可见光至中红外等离激元异质微腔电致变色器件，由阵列化的电致变色单元所组成，每个电致变色单元包括透明导电顶电极、电解液层、电解液框、介孔核壳结构层、底电极及驱动电路；其中，电解液层填充于电解液框内部；所述介孔核壳结构层由介孔核壳结构周期性或者随机性按周期排布构成，介孔核壳结构包括两个部分：表面等离激元纳米结构和介孔介质壳层，介孔介质壳层随机分布有介孔，所述驱动电路与透明导电顶电极及底电极相连。
所述电致变色/变波长器件具有颜色快速切换、可见光至中红外宽色域变色、空间分辨率高、稳定性高等特点，器件的变色工作方式如下：初始状态时，电解液中含有一定量的金属离子，当透明导电顶电极接驱动电路正极，底电极接驱动电路负极时，电解液中的带正电荷的金属离子得电子被还原，在该电致反应中，表面等离激元纳米结构起到催化及成核位的作用，使得新还原的金属原子填充于介孔介质壳层的介孔中，进而改变表面等离激元结构的谐振峰及宏观的颜色，通过改变通电时间可以改变沉积于介孔中金属的体积，进而可实现结构光谱从可见光至中红外连续可调，从而实现结构颜色调控，其中颜色的调控范围由介孔的深度决定；当金属离子还原填充满介孔后，通过驱动电路正负极反接，也即当透明导电顶电极接驱动电路负极，底电极接驱动电路正极时，底电极处的金属原子失去电子被还原，介孔中的纳米金属体积变小，进而可实现结构光谱从中红外到可见光逆向调节，进而实现颜色的逆向可变。
作为本发明的一种改进，所述电致变色单元的尺寸大小为100纳米至10厘米，电致变色单元之间的距离为200纳米至10厘米, 所述电致变色单元阵列为k×t二维面阵，其中k和t取值为2到1000000。
作为本发明的一种改进，所述透明导电顶电极为氧化铟锡（ITO）、掺铝氧化锌（AZO）、掺氟氧化锡（FTO）、石墨烯等半导体透明导电材料，厚度为50纳米到300纳米。
作为本发明的一种改进，所述电解液层包括金属离子和导电电解质，其中金属离子可为Ag+,Au2+,Au3+,Cu+,Cu2+等，导电电解质包括氯化铜等。
作为本发明的一种改进，所述电解液框的供选材料包括聚丙烯，聚乙烯，聚酰亚胺等绝缘聚合物材料。
作为本发明的一种改进，所述表面等离激元纳米结构的供选材料包括，包括金、银、铜、钯、铑等金属或氧化铟锡、氧化铟钛及氧化铟锑等半导体及其合金材料，其形貌可为球形、三角板、棒状、线状、盘状等形状，尺寸范围为10 纳米 - 500 纳米之间；
作为本发明的一种改进，介孔介质壳层的供选材料包括二氧化硅、氧化铝、二氧化钛等介质材料，介孔的孔径取值范围为1 纳米-20 纳米；介孔的尺寸为1 纳米-10 纳米。
作为本发明的一种改进，所述底电极的供选材料为金属材料，供选材料包括金、银、铜、铝、钛、镍和铂等金属电极材料，厚度为50纳米到300纳米。
有益效果：
第一、利用在底电极上均匀排列或者随机组装的介孔纳米结构上的介孔作为模板，在表面等离激元纳米结构上原位电致还原/氧化金属原子/离子，并利用表面等离激元材料的谐振谱可随着介孔中金属材料的填充进行调谐的特性，可实现宽色域变色，光谱在可见光到中红外波段连续可调；另一方面，介孔纳米结构中的介质材料壳层可作为表面等离激元介电系数的控制层，可有效降低表面等离激元结构间的耦合，降低不同纳米结构中颜色串扰，进而实现大范围颜色均一的薄膜；另外，所利用的材料均为无机材料，具有良好的长时稳定性，并可适用于各种复杂环境。
第二、利用介孔核壳纳米结构在亚波长尺度高效操控入射光子，单个结构尺寸可远小于半波长量级；相比于有机染料材料，由于表面等离激元结构的存在，介孔核壳纳米结构的光学截面通常是其几何截面的数倍至数百倍，仅需远小于波长的尺寸的材料即可获得大色彩饱和度。因而，器件色彩像素空间分辨率可达衍射限，远超现有有机材料体系的变色材料。
第三、利用电致反应及金属纳米颗粒的催化效应，可大幅度加速化学反应进程，因此可在介孔模板中迅速氧化/还原金属原子/离子，使得颜色迅速可逆改变，宽色域颜色变化速度小于20s。
附图说明
图1是一种可见光至中红外等离激元异质微腔电致变色器件的探测单元结构示意图；
图2是一种可见光至中红外等离激元异质微腔电致变色器件的探测单元导电示意图，其中，2a为正向导电示意图，2b为反向导电示意图；
图3是介孔核壳结构层结构示意图，图中具有基于表面等离激元介孔核壳结构可为以下六种形式：三角板介孔核壳结构(a)，星型介孔核壳结构（b），正面体介孔核壳结构（c），双球介孔核壳结构（d），正方体介孔核壳结构（e）和棒状介孔核壳结构（f）。
图4是基于表面等离激元介孔核壳结构结构的归一化电场强度与入射波长之间的关系示意图。
具体实施方式
下面通过具体实施例和对比例进一步说明本发明：
实施例1：
如图1所示为本发明的可见光至中红外等离激元异质微腔电致变色器件的探测单元结构示意图，可见光至中红外等离激元异质微腔电致变色器件由阵列化的电致变色单元1所组成，每个电致变色单元1包括透明导电顶电极2、电解液层3、电解液框4、介孔核壳结构层5、底电极6及驱动电路7；其中，电解液层3填充于电解液框4内部；所述介孔核壳结构层5由介孔核壳结构51周期性或者随机性按周期排布构成，介孔核壳结构51包括两个部分：表面等离激元纳米结构52和介孔介质壳层53，介孔介质壳层53随机分布有介孔54，所述驱动电路7与透明导电顶电极2及底电极6相连。
初始状态时，电解液3中含有一定量的金属Ag+离子，当透明导电顶电极接驱动电路正极，底电极接驱动电路负极时，电解液3中的带正电荷的Ag+离子得电子被还原，在该电致反应中，表面等离激元纳米结构52起到催化及成核位的作用，使得新还原的Ag原子填充于介孔介质壳层53的介孔中，进而改变表面等离激元结构的谐振峰及宏观的颜色，通过改变通电时间可以改变沉积于介孔中Ag的体积，进而可实现结构光谱从可见光至中红外连续可调，从而实现结构颜色调控，其中颜色的调控范围由介孔的深度决定；当Ag+还原填充满介孔后，通过驱动电路7正负极反接，也即当透明导电顶电极接驱动电路负极，底电极接驱动电路正极时，底电极处的Ag原子失去电子被氧化，介孔54中的纳米Ag体积变小，进而可实现结构光谱从中红外到可见光逆向调节，进而实现颜色的逆向可变。
以上所述仅为本发明的较佳实施方式，本发明的保护范围并不以上述实施方式为限，但凡本领域普通技术人员根据本发明所揭示内容所作的等效修饰或变化，皆应纳入权利要求书中记载的保护范围内。

Claims (9)

1.一种可见光至中红外等离激元异质微腔电致变色器件，其特征在于：由阵列化的电致变色单元（1）所组成，每个电致变色单元（1）包括透明导电顶电极（2）、电解液层（3）、电解液框（4）、介孔核壳结构层（5）、底电极（6）及驱动电路（7）；其中，电解液层（3）填充于电解液框（4）内部；所述介孔核壳结构层（5）由介孔核壳结构（51）周期性或随机性排布构成，介孔核壳结构（51）包括两个部分：表面等离激元纳米结构（52）和介孔介质壳层（53），介孔介质壳层（53）随机分布有介孔（54），所述驱动电路（7）与透明导电顶电极（2）及底电极（6）相连，所述电解液层（3）包括金属离子和导电电解质，其中金属离子为Ag+,Au2+,Au3+,Cu+,Cu2+中的一种，导电电解质包括氯化铜。
2.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述电致变色单元（1）之间的距离为200纳米至10厘米, 所述电致变色单元（1）阵列为k×t二维面阵，其中k和t取值为2到1000000。
3.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述透明导电顶电极（2）为半导体透明导电材料制成，其厚度为50纳米到300纳米，所述的半导体透明导电材料为氧化铟锡、掺铝氧化锌、掺氟氧化锡、石墨烯中的一种。
4.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述电解液框（4）的材料为绝缘聚合物材料，其包括聚丙烯，聚乙烯，聚酰亚胺中的一种。
5.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述表面等离激元纳米结构（52）的供选材料为金、银、铜、钯或铑。
6.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述表面等离激元纳米结构（52）的供选材料为氧化铟锡、氧化铟钛、氧化铟锑或者其合金材料。
7.根据权利要求5或6所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述的等离激元纳米结构（52）为球形、三角板、棒状、线状、或盘状。
8.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述的介孔介质壳层（53）的供选材料包括二氧化硅、氧化铝或二氧化钛，介孔（54）的孔径取值范围为1纳米-20纳米，介孔（54）的深度尺寸为1纳米-10纳米。
9.根据权利要求1所述的可见光至中红外等离激元异质微腔电致变色器件，其特征在于：所述底电极（6）的供选材料包括金、银、铜、铝、钛、镍或铂，厚度为50纳米到300纳米。
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