CN107475674A - 三稳态光致变色复合薄膜的制备方法 - Google Patents

三稳态光致变色复合薄膜的制备方法 Download PDF

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CN107475674A
CN107475674A CN201710685520.4A CN201710685520A CN107475674A CN 107475674 A CN107475674 A CN 107475674A CN 201710685520 A CN201710685520 A CN 201710685520A CN 107475674 A CN107475674 A CN 107475674A
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蓝碧健
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Abstract

本发明属于薄膜技术领域，涉及一种三稳态光致变色复合薄膜的制备方法；本发明提出的方法是在聚对苯二甲酸丁二醇酯基板上依次蒸镀7,7,8,8‑四氰基对苯二醌二甲烷层、镁层、(2‑亚‑(1,8‑萘)并(六氢嘧啶基))‑N‑氰基亚胺层、铝层以及四(4‑硝基苯氧甲基)甲烷层，构建多层复合结构，利用复合结构中各组分间的协同效应，获得三稳态光致变色薄膜。本发明的优点在于：(1)首次获得绿蓝紫三稳态光致变色薄膜；(2)首先实现了三稳态光致变色薄膜双向变色。

Description

三稳态光致变色复合薄膜的制备方法
技术领域
本发明属于薄膜材料技术领域，具体涉及一种三稳态光致变色复合薄膜的制备方法。
背景技术
光致变色是指某一化合物在一定波长光的照射下分子内发生化学反应，分子结构由具有一种颜色的A构型转变成了另一种颜色的B构型，同时伴随着化合物吸收光谱的变化。B构型在另一波长光的照射下或者热的作用下又能恢复到原来的A构型。光致变色材料在光信息存储、光开关、光学器件、光学镜片、光制动器、荧光传感器、防伪和装饰材料等领域都具有潜在的应用前景。
宋秀美等成系列假二苯乙烯型偶氮苯，利用IR、NMR、ESI-MS和元素分析等技术手段确定目标化合物结构，并通过UV-Vis光谱研究其光致变色性能，测定其溶液态光致顺反异构速率常数，同时考察其在聚甲基丙烯酸甲酯掺杂薄膜中抗疲劳性能(应用化学，2016.33：442-451)。陈尚军等利用加水法制备了嵌段共聚物封装的纳米胶束，胶束的尺寸分布窄，在水溶液中具有较好的稳定性和分散性，纳米胶束封装作用可诱导产生聚集诱导荧光增长效应，在500～700nm范围内呈现出明显的荧光性质，同时，纳米胶束微环境对包裹光致变色分子性能无限制作用，经紫外光和可见光的交替照射，实现荧光从有到无的光控可逆调节(上海师范大学学报(自然科学版)，2016，45：641-649.)。徐雪春等以多芳氨基甲烷类化合物和乙烯醇缩聚物为原料制备了固体薄膜，经电子束辐照后，由无色透明逐渐变为绿色。紫外一可见吸收光谱表明其主吸收峰位于626nm处，吸光度响应与辐照剂量在5-50kGy范围内近似呈线性关系。同时还研究了电子能量、剂量率、分次辐照、后辐照效应和辐照温度等因素对薄膜剂量响应的影响(核技术，2014，37：：020205)。
与现有文件相比，本发明要解决的技术问题是如何通过组份及结构的协同关系，以获得具有绿、蓝、紫三稳态特性的光致变色薄膜，从而扩展光致变色薄膜的应用领域。
发明内容
本发明的目的在于提供一种三稳态光致变色复合薄膜的制备方法。
本发明提出的三稳态光致变色复合薄膜的制备方法，具体步骤如下：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，得三稳态光致变色复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述三稳态光致变色复合薄膜45秒，用测色仪检测光照后的三稳态光致变色复合薄膜的颜色分别为蓝色、绿色及紫色。
如果不使用镁层，本发明还提供如下技术方案作为对比：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为蓝色、蓝色及蓝色。
如果不使用铝层，本发明还提供如下技术方案作为对比：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为蓝色、蓝色及蓝色。
如果不使用7,7,8,8-四氰基对苯二醌二甲烷层，本发明还提供如下技术方案作为对比：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为天蓝色、天蓝色及天蓝色。
如果不使用(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层，本发明还提供如下技术方案作为对比：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的光致变色薄膜的颜色分别为墨绿色、墨绿色及墨绿色。
如果不使用四(4-硝基苯氧甲基)甲烷层，本发明还提供如下技术方案作为对比：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的光致变色薄膜的颜色分别为灰黑色、灰黑色及灰黑色。
如果调换7,7,8,8-四氰基对苯二醌二甲烷层与四(4-硝基苯氧甲基)甲烷层的蒸镀顺序，本发明还提供如下技术方案作为对比：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的四(4-硝基苯氧甲基)甲烷层、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的7,7,8,8-四氰基对苯二醌二甲烷，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的光致变色薄膜的颜色分别为紫色、紫色及紫色。
由上述对比技术方案可知，当三稳态光致变色复合薄膜中组分或结构改变，则光致变色效应消失，说明本发明的技术效果是所有组分特定协同作用的结果，不能简单增减。不仅如此，本发明制备的光致变色薄膜在白光下为蓝色，在波长为365nm的紫外光照射下变为绿色，而在波长为254nm的紫外光照射下变为紫色，即光致变色薄膜的颜色既可以向长波长转变，也可以向短波长转变，这一性质是以往文献中未曾报道的，产生了意想不到的技术效果，具有创造性。
具体实施方式
下面通过实例进一步描述本发明。
实施例1
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，各镀层沉积速率均为0.12nm/s，得三稳态光致变色复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述三稳态光致变色复合薄膜45秒，用测色仪检测光照后的三稳态光致变色复合薄膜的颜色分别为蓝色、绿色及紫色。
实施例2
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，各镀层沉积速率均为0.12nm/s，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为蓝色、蓝色及蓝色。
实施例3
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，各镀层沉积速率均为0.12nm/s，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为蓝色、蓝色及蓝色。
实施例4
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，各镀层沉积速率均为0.12nm/s，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为天蓝色、天蓝色及天蓝色。
实施例5
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，各镀层沉积速率均为0.12nm/s，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为墨绿色、墨绿色及墨绿色。
实施例6
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层，各镀层沉积速率均为0.12nm/s，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为灰黑色、灰黑色及灰黑色。
实施例7
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的四(4-硝基苯氧甲基)甲烷层、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的7,7,8,8-四氰基对苯二醌二甲烷，各镀层沉积速率均为0.12nm/s，得多层复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射上述多层复合薄膜45秒，用测色仪检测光照后的多层复合薄膜的颜色分别为紫色、紫色及紫色。

Claims (1)

1.一种三稳态光致变色复合薄膜的制备方法，其特征在于具体步骤如下：
将厚度为0.2mm、面积为16cm2的聚对苯二甲酸丁二醇酯基板依次用甲醇、乙醇及去离子水洗涤1次，晾干，放置于真空镀膜机中，在真空度为2×10-3Pa下依次蒸镀35nm厚的7,7,8,8-四氰基对苯二醌二甲烷、5nm厚的镁层、65nm厚的(2-亚-(1,8-萘)并(六氢嘧啶基))-N-氰基亚胺层、10nm厚的铝层以及75nm厚的四(4-硝基苯氧甲基)甲烷层，得三稳态光致变色复合薄膜；用白光、波长为365nm的紫外光以及波长为254nm的紫外光分别照射三稳态光致变色复合薄膜45秒，用测色仪检测光照后的三稳态光致变色复合薄膜的颜色。
CN201710685520.4A 2017-08-11 2017-08-11 三稳态光致变色复合薄膜的制备方法 Pending CN107475674A (zh)

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