CN109369945A - 一种可挠性导电膜及其制备方法 - Google Patents

一种可挠性导电膜及其制备方法 Download PDF

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CN109369945A
CN109369945A CN201810943686.6A CN201810943686A CN109369945A CN 109369945 A CN109369945 A CN 109369945A CN 201810943686 A CN201810943686 A CN 201810943686A CN 109369945 A CN109369945 A CN 109369945A
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flexible
conducting film
basement membrane
nano
parts
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CN109369945B (zh
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靳世东
曾西平
王海波
康剑龙
李晓明
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China Tech Powerise Technology Co Ltd Of Shenzhen
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China Tech Powerise Technology Co Ltd Of Shenzhen
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Priority to US17/252,743 priority patent/US11180623B2/en
Priority to PCT/CN2018/107805 priority patent/WO2020037768A1/zh
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Abstract

本发明涉及导电膜领域，尤其涉及一种可挠性导电膜及其制备方法。本发明针对现有的硬质基材不耐弯折、ITO导电材料柔性效果差、难以满足柔性电子器件对导电膜的需求等问题，提供一种具有良好可挠性和导电性的导电膜及其制备方法。本发明的可挠性导电膜包括可挠性基膜和涂布于可挠性基膜表面的导电层，可挠性基膜以沙林树脂为主体，其成膜后具有优异的防腐性、耐化学品性、硬度和柔韧性；以银纳米线导电浆料为导电层，导电性好、柔性效果佳。本发明制得的可挠性导电膜可弯曲、不易破碎，在经过20‑50万次的弯折后膜层表面无龟裂、无折伤，电阻变化率小于5％，具有良好的可挠性与导电性。

Description

一种可挠性导电膜及其制备方法
技术领域
本发明涉及导电膜领域，尤其涉及一种可挠性导电膜及其制备方法。
背景技术
透明导电膜是一种具备导电功能的薄膜，透明导电膜因其具有重量轻、可变形、不易碎等优点广泛的应用于液晶显示器、太阳能电池、光电子和各种光学领域。目前应用最广泛的透明导电膜是在PET、PMMA、TAC、COP、玻璃、陶瓷等硬质基材上制备的，但这些基材存在质脆、不易变形等缺陷，在弯曲半径2mm、弯折10万次以上的条件下，会出现折伤、龟裂、脆化等现象，限制了硬质基材在透明导电膜的应用。
氧化铟锡(ITO)材料作为触摸屏技术的传统导电材料，具有良好的光电特性，但由于其在柔性方面表现较差、不耐反复挠曲，不适合用于柔性触控产品。近年来，已经出现了种类繁多的氧化铟锡替代材料，比如银纳米线、金纳米线、铜纳米线、镍纳米线、银纳米颗粒、金纳米颗粒、铜纳米颗粒、镍纳米颗粒、石墨烯、导电高分子(PEDOT、PSS)材料等。其中银纳米线具有金属银的高导电性、绝佳的柔韧性，且原材料来源广泛、价格低廉。形貌均一可控、高长径比的纳米银线是超大尺寸、柔性触摸屏的透明电极材料的最佳选择，目前已开始局部取代ITO材料并进入产业化生产。
从柔性电子对可挠性的功能需求来看，受力弯曲碎裂的特性使硬质基材和ITO导电材料在柔性电子组件应用上碰到瓶颈。因此，提供一种具有良好的弯曲可挠性和导电性的透明导电膜是本领域的一项技术问题。
发明内容
本发明针对现有的硬质基材不耐弯折、ITO材料柔性效果差等问题，提供一种具有良好可挠性和导电性的导电膜及其制备方法。
本发明采用以下技术方案：
一种可挠性导电膜，该可挠性导电膜包括可挠性基膜和涂布于可挠性基膜表面的导电层，可挠性基膜包括以下重量份的组分：
水性介质70-90份；
沙林树脂5-20份；
抗氧剂1-5份；
流平剂0.5-2份；
功能性粒子0.1-0.5份；
消泡剂1-2份。
进一步的，可挠性基膜的厚度为20-50μm。
进一步的，功能性粒子为纳米TiO2、纳米ZnO、纳米SiO2、纳米CeO2中的任意一种无机纳米填充粒子。添加功能性粒子，将纳米材料与沙林树脂制成复合材料，使得制得的可挠性材料具有抗冲击韧性，耐磨耐刮擦性能以及抗化学品的性能。优选的，功能性粒子为纳米TiO2。
具体的，水性介质为电阻率达到18MΩ*cm(25℃)的水，主要用作溶剂；沙林树脂为美国杜邦公司的沙林树脂群组，作为成膜的主体树脂，具有高透明、耐弯折、耐化性良好的特点，优选SURLYN HPD3001；抗氧化剂为亚磷酸酯与酚类抗氧化剂复合使用，可防止以沙林树脂为主体的可挠性基膜变色氧化，优选的使用抗氧剂168和酚类抗氧剂1790，二者质量比为1:3；流平剂选用水性流平剂，优选BYK333；消泡剂为有机硅消泡剂。
与硬质基材透明导电膜相比，在以沙林树脂为主体制成的可挠性基膜上制备的透明导电薄膜不仅具有相同的光电特性，而且还具有许多独特优点，如可弯曲、重量轻、不易破碎、可采用卷对卷工业化连续生产方式等。
进一步的，导电层为涂布并固化在可挠性基膜表面的导电浆料，导电浆料为银纳米线、金纳米线、铜纳米线、镍纳米线、银纳米颗粒、金纳米颗粒、铜纳米颗粒、镍纳米颗粒中的任意一种或多种混合制成。
进一步的，导电层为涂布并固化在可挠性基膜表面的银纳米线导电浆料。
进一步的，银纳米线导电浆料中含有0.1-0.5％的银纳米线，银纳米线的直径为10-100nm，长径比≥1000。
本发明还提供一种可挠性导电膜的制备方法，包括以下步骤：
(1)按各组分的重量份数称取可挠性基膜原料，将水性介质加入到三口烧瓶中，加热至微沸状态，边搅拌边加入沙林树脂，搅拌速度100-200rpm，待沙林树脂溶解后，依次加入抗氧剂、流平剂、功能型粒子、消泡剂，继续搅拌2-2.5h混合均匀，获得可挠性基膜涂布液，待用；
(2)将步骤(1)配制的可挠性基膜涂布液以狭缝涂布的方式涂覆在承载膜上，涂布速度为10-20m/min，固化，得可挠性基膜；
(3)将导电浆料以狭缝涂布的方式均匀涂覆于可挠性基膜表面，涂布速度为10-20m/min，固化温度为70-130℃，得导电层；
(4)将固化后的可挠性基膜和导电层采用激光镭射的方式从承载膜上取下，即得可挠性导电膜。
进一步的，步骤(2)中可挠性基膜涂布时的固化方式采用热风固化或远红外加热固化或电加热固化。优选的，固化方式为同时采用热风固化和电加热固化两种方式。
进一步的，热风固化的温度为50-100℃，电加热固化的温度为80-130℃。
进一步的，步骤(1)中可挠性基膜涂布液的黏度为5-30mpa.s，表面张力为20-40mN/m。
具体的，承载膜为在可挠性导电膜制备过程中起承载作用的硬质基材，其中承载膜可选用PET、PMMA、COP等材料，厚度主要为100-188μm；优选的，承载膜为厚度188μm的PET基材。
本发明的可挠性导电膜，以沙林树脂为主体，取代硬质基材的触控材料，其成膜后具有优异的耐溶剂性，防腐性、耐化学品性、硬度和柔韧性佳；添加功能性粒子，将纳米材料与沙林树脂制成复合材料，使得制得的可挠性材料具有抗冲击韧性、耐磨耐刮擦性能以及抗化学品的性能。
本发明的可挠性导电膜的制备方法简单，易于操作，通过混合搅拌获得可挠性基膜涂布液，再采用狭缝涂布的方式实现涂布固化，利用硬质承载膜作承载作用，制得的可挠性导电膜可弯曲、不易破碎，在经过20-50万次的弯折后膜层表面无龟裂、无折伤，电阻变化率小于5％，具有良好的可挠性与导电性。
具体实施方式
下面将结合本发明具体实施例，对本发明的技术方案进行清楚、完整的描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通的技术人员在没有做出创造性劳动的前提下所获得的所有其它实施例，都属于本发明的保护范围。
实施例1
一种可挠性导电膜，该可挠性导电膜包括可挠性基膜和涂布于可挠性基膜表面的导电层，可挠性基膜包括以下重量份的组分：
超纯水70份；
沙林树脂5份；
抗氧剂1份；
流平剂0.5份；
功能性粒子0.1份；
消泡剂1份。
本实施例的可挠性导电膜的制备方法，包括以下步骤：
(1)按各组分的重量份数称取可挠性基膜原料，将超纯水加入到三口烧瓶中，加热至微沸状态，边搅拌边加入沙林树脂，搅拌速度100rpm，待沙林树脂溶解后，依次加入抗氧剂、流平剂、功能型粒子、消泡剂，继续搅拌2h混合均匀，获得可挠性基膜涂布液，待用；
(2)上机涂布将厚度为188μm厚的PET基材放卷，放卷速度为100m/min，PET基材薄膜进行电晕处理，电晕功率为1.0kw；将步骤(1)配制的可挠性基膜涂布液以狭缝涂布方式涂布在电晕处理后的PET基材一面，涂布流量为50ml/min，涂布速度为10m/min；采用热风固化和电加热固化，热风固化温度为50℃，电加热固化温度为130℃，固化时间2min，制得20μm厚度的可挠性基膜；
(3)将银纳米线导电浆料以狭缝涂布的方式均匀涂覆于可挠性基膜表面，泵速30ml/min，湿膜厚度30μm，涂布速度为10m/min，固化温度为梯度升温70-130℃，固化时间为2min，形成一层均匀的导电层；
(4)将固化后的可挠性基膜和导电层采用激光镭射的方式从承载膜上取下，即得可挠性导电膜。
将本实施例制得的可挠性导电膜进行耐候性测试，测试条件如下：
耐UV测试：辐照强度0.35W/M2，温度60℃，时间240h；
氙气耐候测试：辐射强度0.8W/M2，温度40℃，湿度55％，时间240h；
高温高湿测试：温度85℃，湿度85％，时间240h；
冷热冲击测试：低温-30℃，高温90℃，时间240h。
耐候性测试结果如表1所示。
表1可挠性导电膜耐候性测试结果
实施例2
一种可挠性导电膜，该可挠性导电膜包括可挠性基膜和涂布于可挠性基膜表面的导电层，可挠性基膜包括以下重量份的组分：
超纯水80份；
沙林树脂15份；
抗氧剂3份；
流平剂1.5份；
功能性粒子0.3份；
消泡剂1.5份。
本实施例的可挠性导电膜的制备方法，包括以下步骤：
(1)按各组分的重量份数称取可挠性基膜原料，将超纯水加入到三口烧瓶中，加热至微沸状态，边搅拌边加入沙林树脂，搅拌速度150rpm，待沙林树脂溶解后，依次加入抗氧剂、流平剂、功能型粒子、消泡剂，继续搅拌2.5h混合均匀，获得可挠性基膜涂布液，待用；
(2)上机涂布将厚度为188μm厚的PET基材放卷，放卷速度为100m/min，PET基材薄膜进行电晕处理，电晕功率为1.0kw；将步骤(1)配制的可挠性基膜涂布液以狭缝涂布方式涂布在电晕处理后的PET基材一面，涂布流量为30ml/min，涂布速度为15m/min；采用热风固化和电加热固化，热风固化温度为80℃，电加热固化温度为100℃，固化时间1.5min，制得30μm厚度的可挠性基膜；
(3)将银纳米线导电浆料以狭缝涂布的方式均匀涂覆于可挠性基膜表面，泵速30ml/min，湿膜厚度30μm，涂布速度为10m/min，固化温度为梯度升温70-130℃，固化时间为2min，形成一层均匀的导电层；
(4)将固化后的可挠性基膜和导电层采用激光镭射的方式从承载膜上取下，即得可挠性导电膜。
将本实施例制得的可挠性导电膜进行耐候性测试，测试条件与实施例1相同，测试结果如表2所示。
表2可挠性导电膜耐候性测试结果
实施例3
一种可挠性导电膜，该可挠性导电膜包括可挠性基膜和涂布于可挠性基膜表面的导电层，可挠性基膜包括以下重量份的组分：
超纯水90份；
沙林树脂20份；
抗氧剂5份；
流平剂2份；
功能性粒子0.5份；
消泡剂2份。
本实施例的可挠性导电膜的制备方法，包括以下步骤：
(1)按各组分的重量份数称取可挠性基膜原料，将超纯水加入到三口烧瓶中，加热至微沸状态，边搅拌边加入沙林树脂，搅拌速度200rpm，待沙林树脂溶解后，依次加入抗氧剂、流平剂、功能型粒子、消泡剂，继续搅拌2h混合均匀，获得可挠性基膜涂布液，待用；
(2)上机涂布将厚度为188μm厚的PET基材放卷，放卷速度为100m/min，PET基材薄膜进行电晕处理，电晕功率为1.0kw；将步骤(1)配制的可挠性基膜涂布液以狭缝涂布方式涂布在电晕处理后的PET基材一面，涂布流量为50ml/min，涂布速度为20m/min；采用热风固化和电加热固化，热风固化温度为100℃，电加热固化温度为80℃，固化时间1min，制得50μm厚度的可挠性基膜；
(3)将银纳米线导电浆料以狭缝涂布的方式均匀涂覆于可挠性基膜表面，泵速30ml/min，湿膜厚度30μm，涂布速度为10m/min，固化温度为梯度升温70-130℃，固化时间为2min，形成一层均匀的导电层；
(4)将固化后的可挠性基膜和导电层采用激光镭射的方式从承载膜上取下，即得可挠性导电膜。
将本实施例制得的可挠性导电膜进行耐候性测试，测试条件与实施例1相同，测试结果如表3所示。
表3可挠性导电膜耐候性测试结果
对比例1
本对比例中的导电膜以50μm厚度的PET为基膜，将银纳米线浆料以狭缝涂布的方式均匀涂布在基膜表面，泵速30ml/min，湿膜厚度30um，涂布速度为10m/min，固化温度为梯度升温70-130℃，固化时间为2min，形成一层均匀的导电层，制得透明导电膜。
将实施例1-3制得的可挠性导电膜进行光学性能测试，结果如表4所示。
表4可挠性导电膜光学性能测试结果
将实施例1-3和对比例1制得的导电膜(电阻60Ω)进行弯折性能测试，弯折R＝2mm，分别测试弯折10万次、20万次、30万次、50万次后，各导电膜的电阻变化及膜面状态，结果如表5所示。
表5导电膜弯折性能测试
由表1-5可知，本发明各实施例以沙林树脂为主体制备可挠性基膜，再结合具有高导电性和绝佳柔韧性的银纳米线作为导电层，制备得到的可挠性导电膜具有高透过率、低雾度、低b*值等良好的光学特性，可满足透明导电薄膜的需求；同时具有良好的可挠性和导电性，弯折20-50万次后，导电膜层无龟裂、无折伤，且电阻变化率小于5％，使得其可广泛应用于柔性电子组件上，可满足柔性光电产品对导电膜的需求。通过耐候性能测试也可看出，本发明实施例制得的可挠性导电膜具有较强的耐候性，使其可适用于各种环境，扩大了其应用范围。
以上借助具体实施例对本发明做了进一步描述，但是应该理解的是，这里具体的描述，不应理解为对本发明的实质和范围的限定，本领域内的普通技术人员在阅读本说明书后对上述实施例做出的各种修改，都属于本发明所保护的范围。

Claims (10)

1.一种可挠性导电膜，其特征在于，所述可挠性导电膜包括可挠性基膜和涂布于所述可挠性基膜表面的导电层，所述可挠性基膜包括以下重量份的组分：
水性介质70-90份；
沙林树脂5-20份；
抗氧剂1-5份；
流平剂0.5-2份；
功能性粒子0.1-0.5份；
消泡剂1-2份。
2.根据权利要求1所述的可挠性导电膜，其特征在于，所述可挠性基膜的厚度为20-50μm。
3.根据权利要求1所述的可挠性导电膜，其特征在于，所述功能性粒子为纳米TiO2、纳米ZnO、纳米SiO2、纳米CeO2中的任意一种无机纳米填充粒子。
4.根据权利要求1-3中任一项所述的可挠性导电膜，其特征在于，所述导电层为涂布并固化在所述可挠性基膜表面的导电浆料，所述导电浆料为银纳米线、金纳米线、铜纳米线、镍纳米线、银纳米颗粒、金纳米颗粒、铜纳米颗粒、镍纳米颗粒中的任意一种或多种混合制成。
5.根据权利要求4所述的可挠性导电膜，其特征在于，所述导电层为涂布并固化在所述可挠性基膜表面的银纳米线导电浆料。
6.根据权利要求5所述的可挠性导电膜，其特征在于，所述银纳米线导电浆料中含有0.1-0.5％的银纳米线，所述银纳米线的直径为10-100nm，长径比≥1000。
7.一种如权利要求1-6中任一项所述的可挠性导电膜的制备方法，其特征在于，包括以下步骤：
(1)按各组分的重量份数称取可挠性基膜原料，将水性介质加入到三口烧瓶中，加热至微沸状态，边搅拌边加入沙林树脂，搅拌速度100-200rpm，待沙林树脂溶解后，依次加入抗氧剂、流平剂、功能型粒子、消泡剂，继续搅拌2-2.5h混合均匀，获得可挠性基膜涂布液，待用；
(2)将步骤(1)配制的可挠性基膜涂布液以狭缝涂布的方式涂覆在承载膜上，涂布速度为10-20m/min，固化，得可挠性基膜；
(3)将导电浆料以狭缝涂布的方式均匀涂覆于可挠性基膜表面，涂布速度为10-20m/min，固化温度为70-130℃，得导电层；
(4)将固化后的可挠性基膜和导电层采用激光镭射的方式从承载膜上取下，即得可挠性导电膜。
8.根据权利要求7所述的可挠性导电膜的制备方法，其特征在于，步骤(2)中可挠性基膜涂布时的固化方式采用热风固化或远红外加热固化或电加热固化。
9.根据权利要求8所述的可挠性导电膜的制备方法，其特征在于，所述热风固化的温度为50-100℃，所述电加热固化的温度为80-130℃。
10.根据权利要求7所述的可挠性导电膜的制备方法，其特征在于，步骤(1)中可挠性基膜涂布液的黏度为5-30mpa.s，表面张力为20-40mN/m。
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