CN113621162B - 一种透明导电膜 - Google Patents
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Abstract
本发明公开了一种透明导电膜,包括:透明聚酰亚胺基膜和附着在透明聚酰亚胺基膜表面的导电层,其中,透明聚酰亚胺由二酐单体、二胺单体和端基为氨基的树枝状聚酰胺‑胺共聚制得。本发明所述导电膜透明性好,导电性好,且银纳米线不易脱落。
Description
技术领域
本发明涉及导电膜技术领域,尤其涉及一种透明导电膜。
背景技术
随着时代的发展,柔性电子产品的应用越来越广。柔性透明导电薄膜是柔性电子器件中的重要组成部分,由于氧化铟锡并不适合应用到柔性电子器件中,寻找新一代材料引起了研究者的广泛关注。银纳米线作为一种新型的纳米材料,在纳米尺度上有很多新奇的性能,其优良的导电性及良好的光学性能被认为是替代氧化铟锡的最佳材料。
聚酰亚胺材料具有良好的耐高温性能、机械性能,可以用于柔性透明导电薄膜中,但是聚酰亚胺与银纳米线之间的附着力较差,柔性透明导电薄膜在使用过程中会经常弯折,导致银纳米线容易脱落,影响导电性,进而影响其使用寿命。
发明内容
基于背景技术存在的技术问题,本发明提出了一种透明导电膜,本发明所述导电膜透明性好,导电性好,且银纳米线不易脱落。
本发明提出了一种透明导电膜,包括:透明聚酰亚胺基膜和附着在透明聚酰亚胺基膜表面的导电层,其中,透明聚酰亚胺由二酐单体、二胺单体和端基为氨基的树枝状聚酰胺-胺共聚制得。
优选地,二胺单体为2-(3-氨基苯基)-5-氨基苯并咪唑、2-(4-氨基苯基)-5-氨基苯并咪唑中的至少一种。
上述二酐单体可以为4,4'-(4,4'-异丙基二苯氧基)二(邻苯二甲酸酐)(BPADA)、4,4-六氟异丙基邻苯二甲酸酐(6FDA)、4,4'-氧双邻苯二甲酸酐(ODPA)、3,3,4,4-二苯基砜四羧酸二酸酐(DSDA)、1,2,4,5-环己烷四甲酸二酐、1,2,3,4-环戊烷四甲酸二酐等。
优选地,二酐单体、二胺单体、树枝状聚酰胺-胺的摩尔比为1:0.92-0.94:0.08-0.1。
优选地,树枝状聚酰胺-胺的支化代数为1.0。
上述树枝状大分子是通过多官能团单体(又称支化基元)逐步重复反应得到的具有树枝状高度支化结构的大分子。以乙二胺和丙烯酸甲酯为例,其合成方法为:以乙二胺为核与丙烯酸甲酯通过Michael加成反应生成一个四元酯(支化代数为0.5代);然后四元酯与乙二胺发生酰胺化反应生成一个四元酰胺化合物(支化代数为1.0代,其端基为氨基);重复Michael加成和酰胺化反应,即可得到不同代数的树枝状聚酰胺-胺。
上述树枝状聚酰胺-胺可以按照本领域常规方法制得,也可以从市场购得。
本发明选用支化代数为1.0的树枝状聚酰胺-胺,可以在引入适量活性氨基的同时,避免支化代数过高导致基膜的其他性能降低的问题,使得基膜的机械性能、耐高温等性能不会发生较大变化。
优选地,在透明聚酰亚胺的制备过程中,在惰性气体氛围中,向含有催化剂、树枝状聚酰胺-胺和二胺单体的水溶液中加入二酐单体,进行反应得到聚酰胺酸溶液,亚胺化得到透明聚酰亚胺。
优选地,催化剂为三乙胺。
优选地,催化剂和二酐单体的摩尔比为2-2.5:1。
优选地,反应温度为10-15℃,反应时间为3-5h。
优选地,亚胺化的程序为:于80-90℃保温1-2h,然后于180-190℃、210-220℃分别保温0.8-1.2h。
优选地,导电层是在透明聚酰亚胺基膜表面涂覆导电墨水,再干燥获得;其中,导电墨水的原料包括:银纳米线、胶黏剂、分散剂和溶剂。
上述导电墨水的原料还可以包括流平剂、消泡剂、表面活性剂等助剂。
上述溶剂可以为N-甲基吡咯烷酮、N,N-二甲基甲酰胺、甲苯、乙酸乙酯、水等。
上述分散剂可以为醋酸纤维素、聚乙烯吡咯烷酮、十二烷基磺酸钠、十六烷基二甲基溴化氨、氟碳表面活性剂等。
优选地,胶黏剂为聚氨酯胶黏剂、环氧树脂胶黏剂中的至少一种。
优选地,银纳米线、胶黏剂、分散剂和溶剂的重量比为0.4-0.5:0.8-1.2:0.5-0.7:100。
上述水均为去离子水。
有益效果:
1.本发明选用端基为氨基的树枝状聚酰胺-胺、适宜的二胺单体与二酐单体反应,将树枝状聚酰胺-胺引入聚酰亚胺主链中,从而引入了多个酰胺基团和活泼氨基;酰胺基团和氨基均可与银纳米线表面的羟基形成氢键,固定银纳米线,并且氨基可与胶黏剂中的环氧基团、异氰酸酯基团等进行共价结合,形成交联网络,牢固固定银纳米线,从而大幅提高本发明的导电性能;
2.二胺单体选用2-(3-氨基苯基)-5-氨基苯并咪唑、2-(4-氨基苯基)-5-氨基苯并咪唑,其含有酰胺基团可与银纳米线表面的羟基形成氢键,进一步固定银纳米线,改善导电性能;
3.二胺单体选用2-(3-氨基苯基)-5-氨基苯并咪唑、2-(4-氨基苯基)-5-氨基苯并咪唑,与树枝状聚酰胺-胺、适宜的二酐单体以适宜比例制备聚酰亚胺基膜,通过引入苯并咪唑单元和柔性链段,减弱分子间的CTC作用,增强了PI薄膜的透明性,且反应在水中进行,更加环保。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
以下实施例和对比例中的端基为氨基的树枝状聚酰胺-胺是:乙二胺与丙烯酸甲酯发生Michael加成反应生成四元酯,然后与乙二胺发生酰胺化反应制得,其支化代数为1.0代,其端基为氨基。
实施例1
一种透明导电膜,包括:透明聚酰亚胺基膜和附着在透明聚酰亚胺基膜表面的导电层;
其中,在透明聚酰亚胺基膜的制备过程中,将2mmol三乙胺、0.1mmol端基为氨基的树枝状聚酰胺-胺、0.92mmol的2-(3-氨基苯基)-5-氨基苯并咪唑溶于400ml水中,通入氮气排除空气,然后缓慢加入1mmol的4,4'-(4,4'-异丙基二苯氧基)二(邻苯二甲酸酐),控制温度为15℃,保温反应3h得到聚酰胺酸溶液;将聚酰胺酸溶液涂覆在清洁干燥后的玻璃载体表面,然后于90℃保温1h,然后于180℃、210℃分别保温1.2h得到透明聚酰亚胺基膜;
依次用丙酮、乙醇、水清洗透明聚酰亚胺基膜并干燥,然后在透明聚酰亚胺基膜表面涂覆导电墨水,于160℃干燥0.5h得到透明导电膜,其中,导电墨水的原料按重量份包括:银纳米线0.2g、聚氨酯胶黏剂0.4g、氟碳表面活性剂0.25g和甲苯50g。
实施例2
一种透明导电膜,包括:透明聚酰亚胺基膜和附着在透明聚酰亚胺基膜表面的导电层;
其中,在透明聚酰亚胺基膜的制备过程中,将2.5mmol三乙胺、0.08mmol端基为氨基的树枝状聚酰胺-胺、0.94mmol的2-(4-氨基苯基)-5-氨基苯并咪唑溶于400ml水中,通入氮气排除空气,然后缓慢加入1mmol的4,4'-氧双邻苯二甲酸酐,控制温度为10℃,保温反应5h得到聚酰胺酸溶液;将聚酰胺酸溶液涂覆在清洁干燥后的玻璃载体表面,然后于80℃保温2h,然后于190℃、220℃分别保温0.8h得到透明聚酰亚胺基膜;
依次用丙酮、乙醇、水清洗透明聚酰亚胺基膜并干燥,然后在透明聚酰亚胺基膜表面涂覆导电墨水,于160℃干燥0.5h得到透明导电膜,其中,导电墨水的原料按重量份包括:银纳米线0.25g、水溶性环氧树脂胶黏剂0.6g、十二烷基磺酸钠0.35g和水50g。
实施例3
一种透明导电膜,包括:透明聚酰亚胺基膜和附着在透明聚酰亚胺基膜表面的导电层;
其中,在透明聚酰亚胺基膜的制备过程中,将2.3mmol三乙胺、0.09mmol端基为氨基的树枝状聚酰胺-胺、0.93mmol的2-(3-氨基苯基)-5-氨基苯并咪唑溶于400ml水中,通入氮气排除空气,然后缓慢加入1mmol的4,4'-(4,4'-异丙基二苯氧基)二(邻苯二甲酸酐),控制温度为12℃,保温反应4.5h得到聚酰胺酸溶液;将聚酰胺酸溶液涂覆在清洁干燥后的玻璃载体表面,然后于85℃保温1.5h,然后于185℃、215℃分别保温1h得到透明聚酰亚胺基膜;
依次用丙酮、乙醇、水清洗透明聚酰亚胺基膜并干燥,然后在透明聚酰亚胺基膜表面涂覆导电墨水,于160℃干燥0.5h得到透明导电膜,其中,导电墨水的原料按重量份包括:银纳米线0.23g、水溶性环氧树脂胶黏剂0.5g、十二烷基磺酸钠0.3g和水50g。
对比例1
一种透明导电膜,在透明聚酰亚胺基膜的制备过程中,不添加端基为氨基的树枝状聚酰胺-胺,2-(3-氨基苯基)-5-氨基苯并咪唑的用量为1.02mmol,其他同实施例3。
检测实施例1-3和对比例1制得的透明导电膜的性能,结果如表1所示。
表1检测结果
备注:百格法测试附着力,涂层100%保留时为0级;涂层保留较完整,仅有少数边角破损时为1级;边角破损较多但无整格脱落时为2级;边角破损严重,有少量整格脱落时为3级;边角破损严重,有较多整格脱落,但涂层保留面积>65%时为4级;涂层保留面积<65%时为5级。
由表1可以看出,实施例1-3的透明性好,方阻较低,且经1000次弯折后,其方阻变化不大,银纳米线不易脱落,导电性良好;实施例3的透明性高于对比例1。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种透明导电膜,其特征在于,包括:透明聚酰亚胺基膜和附着在透明聚酰亚胺基膜表面的导电层,其中,透明聚酰亚胺由二酐单体、二胺单体和端基为氨基的树枝状聚酰胺-胺共聚制得;
二胺单体为2-(3-氨基苯基)-5-氨基苯并咪唑、2-(4-氨基苯基)-5-氨基苯并咪唑中的至少一种;
二酐单体、二胺单体、树枝状聚酰胺-胺的摩尔比为1:0.92-0.94:0.08-0.1;
树枝状聚酰胺-胺的支化代数为1.0;
导电层是在透明聚酰亚胺基膜表面涂覆导电墨水,再干燥获得;其中,导电墨水的原料包括:银纳米线、胶黏剂、分散剂和溶剂;
胶黏剂为聚氨酯胶黏剂、环氧树脂胶黏剂中的至少一种。
2.根据权利要求1所述透明导电膜,其特征在于,在透明聚酰亚胺的制备过程中,在惰性气体氛围中,向含有催化剂、树枝状聚酰胺-胺和二胺单体的水溶液中加入二酐单体,进行反应得到聚酰胺酸溶液,亚胺化得到透明聚酰亚胺。
3.根据权利要求2所述透明导电膜,其特征在于,催化剂为三乙胺。
4.根据权利要求2所述透明导电膜,其特征在于,催化剂和二酐单体的摩尔比为2-2.5:1。
5.根据权利要求2所述透明导电膜,其特征在于,反应温度为10-15℃,反应时间为3-5h。
6.根据权利要求2所述透明导电膜,其特征在于,亚胺化的程序为:于80-90℃保温1-2h,然后于180-190℃、210-220℃分别保温0.8-1.2h。
7.根据权利要求1所述透明导电膜,其特征在于,银纳米线、胶黏剂、分散剂和溶剂的重量比为0.4-0.5:0.8-1.2:0.5-0.7:100。
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