CN115109294B - 抗静电膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种抗静电膜及其制备方法,所述抗静电膜的制备方法包括以下步骤:获得碳纳米管水性分散液;将所述碳纳米管分散液、水性粘结树脂、烯烃乳液、水以及助剂混合均匀,得到碳纳米管抗静电涂布液;将所述碳纳米管抗静电涂布液涂布于基材表面,固化后得到抗静电薄膜原膜;以及将所述抗静电薄膜原膜在有机萃取溶剂中漂洗后,即获得所述透明抗静电膜。本发明的方法制备出的抗静电膜在保证优异导电性的同时获得更加优越的透光率,实现高透光和高导电的结合,是一种综合性能优异的透明抗静电薄膜。
Description
技术领域
本发明是关于抗静电膜,特别是关于一种抗静电膜及其制备方法。
背景技术
透明抗静电膜是电子包装和保护材料中大量实用的一类功能薄膜,利用其表面导电特性避免电荷聚集形成的高电压,带来对电子器件的损伤。以往以涂布导电高分子材料(如PEDOT等)和碳材料(如炭黑、碳纳米管、石墨烯等)于透明基材表面,使塑料基材获得一定的表面导电性。但高导电性与高透光率对于薄膜材料是一组矛盾问题,高导电性需要大量导电材料的添加,而此时往往带来透光率的急剧下降。
公开于该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解,而不应当被视为承认或以任何形式暗示该信息构成已为本领域一般技术人员所公知的现有技术。
发明内容
本发明的目的在于提供一种抗静电膜及其制备方法,其能够使抗静电膜具备优异的导电性和高透光率。
为实现上述目的,本发明的实施例提供了一种抗静电膜的制备方法,包括以下步骤:
获得碳纳米管水性分散液;
将所述碳纳米管分散液、水性粘结树脂、烯烃乳液、水以及助剂混合均匀,得到碳纳米管抗静电涂布液;
将所述碳纳米管抗静电涂布液涂布于基材表面,固化后得到抗静电薄膜原膜;以及
将所述抗静电薄膜原膜在有机萃取溶剂中漂洗后,即获得所述透明抗静电膜。
在本发明的一个或多个实施方式中,所述碳纳米管水性分散液按照质量百分比计,包括以下原料组分:
在本发明的一个或多个实施方式中,所述碳纳米管为单壁碳纳米管或者少壁碳纳米管,所述少壁碳纳米管为的管壁层数少于5层的碳纳米管;和/或,所述碳纳米管的直径0.4-4nm。
在本发明的一个或多个实施方式中,所述分散剂为阳离子型表面活性剂、阴离子型表面活性剂和非离子型表面活性剂中的一种或多种。
在本发明的一个或多个实施方式中,所述分散剂由阴离子型表面活性剂与非离子型表面活性剂组成,且所述阴离子型表面活性剂与非离子型表面活性剂的质量比为(1-10):1。
在本发明的一个或多个实施方式中,所述获得碳纳米管水性分散液的步骤包括:将所述碳纳米管、分散剂和分散液润湿剂采用纳米研磨和高压均质分散手段将其均匀分散在水中,并使用300-600目滤网过滤后,即得到所述碳纳米管水性分散液。
在本发明的一个或多个实施方式中,所述助剂包括流平剂和基材润湿剂。
在本发明的一个或多个实施方式中,所述碳纳米管抗静电涂布液按重量百分比计,包括以下原料组分:
在本发明的一个或多个实施方式中,所述烯烃乳液中烯烃的熔点小于70℃,所述烯烃乳液为石蜡乳液或白油乳液。
本发明还公开了一种抗静电膜,包括基材以及形成于该基材上碳纳米管涂层,所述基材采用柔性透明材料制得,所述碳纳米管涂层的厚度为100nm-10μm。
在本发明的一个或多个实施方式中,所述烯烃乳液中烯烃的熔点小于70℃,所述烯烃乳液为石蜡乳液或白油乳液。
本发明还公开了一种抗静电膜,所述抗静电膜包括基材层以及碳纳米管涂层,所述基材层采用柔性透明材料,所述碳纳米管涂层包括单壁碳纳米管或者少壁碳纳米管,其中所述单壁碳纳米管或者少壁碳纳米管的管壁层数少于5层,且所述单壁碳纳米管或者少壁碳纳米管的直径0.4-4nm。
与现有技术相比,根据本发明实施方式的抗静电膜及其制备方法的有益效果为:
(1)利用烯烃乳液与碳纳米管在干燥固化过程的相分离作用,形成离散的油相池,推动碳纳米管形成网格图案化结构,进而通过有机萃取溶剂萃取后,获得具有图案化的碳纳米管导电网络;
(2)图案化的碳纳米管导电网络具有导电网络稳定和表面覆盖率低的特点,导电网络稳定可以提高抗静电膜的导电性,表面覆盖率低则可以提高抗静电膜的透光率,使抗静电膜具有兼顾高导电性和高透光率的性能;
(3)烯烃乳液与碳纳米管在相分离推动下形成的碳纳米管导电网络,为更长的碳纳米管管束结构,在薄膜后续裁切时候可连通上下表面,获得体积导电的特性,有效释放上下表面聚集电荷,在抗静电领域具有重要应用。
附图说明
图1是根据本发明一实施方式萃取前的碳纳米管导电网络的结构示意图;
图2是根据本发明一实施方式萃取后的碳纳米管导电网络的结构示意图。
具体实施方式
下面结合附图,对本发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。
除非另有其它明确表示,否则在整个说明书和权利要求书中,术语“包括”或其变换如“包含”或“包括有”等等将被理解为包括所陈述的元件或组成部分,而并未排除其它元件或其它组成部分。
根据本发明优选实施方式的抗静电膜的制备方法,包括以下步骤:
S1、获得碳纳米管水性分散液。
在S1中,碳纳米管水性分散液质量百分比计,可以包括以下原料组分:碳纳米管0.05~4%,分散剂0.05-10%,分散液润湿剂0.01-1%,余量为水。
在上述原料组分中,碳纳米管可以为单壁碳纳米管或者少壁碳纳米管,优选的,碳纳米管为单壁碳纳米管。分散剂可以为阳离子型表面活性剂、阴离子型表面活性剂和非离子型表面活性剂中的任意一种。优先的分散剂可以为阴离子型表面活性剂与非离子型表面活性剂,且阴离子型表面活性剂与非离子型表面活性剂的质量比为(1-10):1。
分散液润湿剂可以为聚硅氧烷类水性润湿剂,具体可以是BYK180、BYK184、BYK187、BYK190、BYK191、BYK192、BYK194、BYK151、BYK154中的任意一种。
在S1中,获得碳纳米管水性分散液的步骤可以包括:将碳纳米管、分散剂和分散液润湿剂采用纳米研磨和高压均质分散手段将其均匀分散在水中,并使用300-600目滤网过滤后,即得到碳纳米管水性分散液。
在上述步骤中,纳米研磨分散的工艺可以为:研磨分散盘线速度1-10米/秒,研磨介质为陶瓷珠,优选为氧化锆珠,直径0.4-2.0毫米,研磨次数3-10遍。高压均质分散的工艺可以为:工作压力50-200MPa,均质次数5-20遍。
在其他实施方式中,碳纳米管水性分散液也可以直接购买现有市场中类似的产品。
S2、将碳纳米管分散液、水性粘结树脂、烯烃乳液、水以及助剂混合均匀,得到碳纳米管抗静电涂布液。
在S2中,助剂可以为流平剂和基材润湿剂。碳纳米管抗静电涂布液按重量百分比计,可以包括以下原料组分:碳纳米管水性分散液50-90%,水性粘结树脂5-40%,烯烃乳液1-20%,流平剂0.1-1%,基材润湿剂0.1-1%,余量为水。
在S2中,烯烃乳液中烯烃的熔点小于70℃,烯烃乳液可以为石蜡乳液或白油乳液。水性粘结树脂可以是水性聚氨酯、水性丙烯酸、水性饱和聚酯、水性醇酸等树脂的任意一种和组合。流平剂可以为有机硅类或者有机氟类水性涂料流平剂,具体可以为BYK3410、BYK3455、BYK331、BYK333、BYK378等。基材润湿剂可以为水性涂料基材润湿剂,具体可以为BYK3400、BYK3450、BYK3451、BYK3481、BYK3499、Tego245、Tego 450等。
S3、将碳纳米管抗静电涂布液涂布于基材表面,固化后得到抗静电薄膜原膜。
在S3中,涂布的工艺可以为喷涂、滚涂、刮涂的任意一种。固化可以采用热固化的处理,热固化的处理的具体条件可以为在80-150℃下烘烤1-10min。
S4、将抗静电薄膜原膜在有机萃取溶剂中漂洗后,即获得透明抗静电薄膜。
有机萃取溶剂可以为氯仿、甲苯、二硫化碳、二甲苯、乙醇中的一种。漂洗的时间可以为5-100s。
本发明的制备方法,利用烯烃乳液与碳纳米管在干燥固化过程的相分离作用,形成离散的油相池,推动碳纳米管形成网格图案化结构,进而通过有机萃取溶剂萃取后,获得具有图案化的碳纳米管导电网络。一具体实施方式中,萃取前如图1所示,图1中的线状物可以理解为碳纳米管,椭圆形或圆形的物质可以理解为烯烃乳液在烘干后可以在基材表面形成烯烃乳胶颗粒。萃取前如图2所示,图2中的线状物可以理解为碳纳米管。基材表面经萃取处理后,由碳纳米管得到的图案化的物质,可以认为是图案化的碳纳米管导电网络。
图案化的碳纳米管导电网络具有导电网络稳定和表面覆盖率低的特点,具有兼顾高导电性和高透光率的优势;
相分离推动下形成的碳纳米管导电网络,为更长的碳纳米管管束结构,在薄膜后续裁切时候可连通上下表面,获得体积导电的特性,有效释放上下表面聚集电荷,在抗静电领域具有重要应用。
本发明还公开了一种抗静电膜。其中,该抗静电膜包括基材以及碳纳米管涂层。为了提高整个抗静电膜的透光性,基材可以采用柔性透明材料制得,使基材为透明状。碳纳米管涂层的厚度可以为100nm-10μm。
其中,碳纳米管涂层可以认为是由碳纳米管抗静电涂布液形成于基材表面,固化后,并经有机萃取溶剂漂洗后形成的。
柔性透明材料可以是聚酯(PET)、聚苯乙烯(PS)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)等柔性透明膜材。基材的厚度可以为5-150μm。
本发明的抗静电膜可作为柔性透明电热膜、电热除冰、电热除雾、智能窗膜等薄膜材料,也可以用于抗静电、屏蔽、透明感应薄膜等领域,具有高导电、高透光率、导电稳定等优势。
下面将结合具体的实施例,详细介绍本发明的抗静电膜及其制备方法。
实施例1
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径0.8毫米的氧化锆珠,分散盘线速度10米/秒,研磨10遍,进而100MPa高压均质5遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PET基材(厚度50微米)表面,120℃烘烤5分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。用四探针仪测试其表面电阻,可见光透过率测试仪测试薄膜透光率,用3M胶带测试表层碳纳米管附着力。
实施例2
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径0.4毫米的氧化锆珠,分散盘线速度4米/秒,研磨20遍,进而50MPa高压均质5遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PS基材(厚度50微米)表面,120℃烘烤10分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。用四探针仪测试其表面电阻,可见光透过率测试仪测试薄膜透光率,用3M胶带测试表层碳纳米管附着力。
实施例3
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径1.0毫米的氧化锆珠,分散盘线速度8米/秒,研磨5遍,进而100MPa高压均质5遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PC基材(厚度100微米)表面,120℃烘烤5分钟,进而用甲苯浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。用四探针仪测试其表面电阻,可见光透过率测试仪测试薄膜透光率,用3M胶带测试表层碳纳米管附着力。
实施例4
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径1.0毫米的氧化锆珠,分散盘线速度8米/秒,研磨5遍,进而150MPa高压均质8遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PET基材(厚度80微米)表面,120℃烘烤5分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。
实施例5
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径0.6毫米的氧化锆珠,分散盘线速度10米/秒,研磨10遍,进而150MPa高压均质5遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PET基材(厚度150微米)表面,120℃烘烤10分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。用四探针仪测试其表面电阻,可见光透过率测试仪测试薄膜透光率,用3M胶带测试表层碳纳米管附着力。
实施例6
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径0.8毫米的氧化锆珠,分散盘线速度10米/秒,研磨10遍,进而100MPa高压均质5遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PET基材(厚度50微米)表面,120℃烘烤5分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。用四探针仪测试其表面电阻,可见光透过率测试仪测试薄膜透光率,用3M胶带测试表层碳纳米管附着力。
实施例7
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径0.8毫米的氧化锆珠,分散盘线速度10米/秒,研磨10遍,进而100MPa高压均质5遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PET基材(厚度50微米)表面,120℃烘烤5分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。用四探针仪测试其表面电阻,可见光透过率测试仪测试薄膜透光率,用3M胶带测试表层碳纳米管附着力。
实施例8
将碳纳米管与分散剂、分散液润湿剂等按照碳纳米管分散液配方表,经纳米研磨工艺分散,研磨介质为直径1.0毫米的氧化锆珠,分散盘线速度8米/秒,研磨5遍,进而150MPa高压均质8遍,300目滤网过滤制备得到碳纳米管分散液。随后按照抗静电涂布液配方与树脂及助剂混合制备得到抗静电涂布液。将抗静电涂布液用3号线棒刮涂PET基材(厚度80微米)表面,120℃烘烤5分钟,进而用氯仿浸泡漂洗10秒,随后风干即得到本发明的抗静电膜。
对比例1
该对比例采用与实施例1相同的配方,不同之处仅是抗静电涂布液中无烯烃乳液以及有机溶剂萃取步骤。
对比例2
该对比例采用与实施例2相同的配方,不同之处仅是抗静电涂布液中无烯烃乳液以及有机溶剂萃取步骤。
对比例3
该对比例采用与实施例4基本相同,不同之处仅是选择少壁碳纳米管(管径2-5nm,管壁6-8层)作为碳纳米管。
对实施例1~8中以及对比例1-3中得到的抗静电膜进行如下的性能测试:1、用四探针仪测试其表面电阻。2、可见光透过率测试仪测试薄膜透光。3、用3M胶带测试表层碳纳米管附着力。
表1:实施例和对比例数据汇总
从表1中,实施例1的透光率和表面电阻的数据明显优于对比例1的透光率和表面电阻的数据。以及实施例2的透光率和表面电阻的数据明显优于对比例2的透光率和表面电阻的数据。可以得知,在制备抗静电膜的过程中,在抗静电液涂布液中加入烯烃乳液并在后期用有机萃取溶剂将基材层表面的烯烃乳胶颗粒溶解,利用烯烃乳液与碳纳米管在干燥固化过程的相分离作用,形成离散的油相池,推动碳纳米管形成网格图案化结构,进而通过有机萃取溶剂萃取后,获得具有图案化的碳纳米管导电网络。图案化的碳纳米管导电网络具有导电网络稳定和表面覆盖率低的特点,导电网络稳定可以提高抗静电膜的导电性,表面覆盖率低则可以提高抗静电膜的透光率,使抗静电膜具有兼顾高导电性和高透光率的性能。从表1中,实施例8的透光率优于和实施例4的透光率,实施例8的表面电阻优于和实施例4的表面电阻相近,可以得知,选择单壁碳纳米管可以明显提升抗静电膜的透光性,且还具有良好的导电性。
从表1中,实施例4透光率和表面电阻的数据都是优于对比例3的透光率和表面电阻的数据,可以的得知,当少壁碳纳米管的管壁层数大于5层时,由于单个少壁碳纳米管的导电性增强,但是单个少壁碳纳米管的重量增加,导致少壁碳纳米管的数量变少,使碳纳米管形成的导电网络不稳定,从而导致宏观上的抗静电膜的导电性变差,还会大幅度降低了抗静电膜的透光率。
需要说明的是,性能测试中表面电阻的值为范围值是由于在基材表面涂碳纳米管涂层的过程中,碳纳米管涂层的厚度会有微小差异会导致不同的测试点位的表面电阻数值不同,也有可能是因为碳纳米管分布也存在不均导致不同的测试点位的表面电阻数值不同。另外,常规的碳管分散技术,表面电阻的数据偏差更大。应该理解的是,本实施例部分仅以部分实施例进行说明,在上述各组分的质量百分数范围内以及各组分选择的具体成分的范围内,均能实现木发明的目的,即本发明的方法制备出的抗静电膜在保证优异导电性的同时获得更加优越的透光率,此处不再一一举例进行说明。
由表1的数据还可以得知,总体上抗静电膜中碳纳米管的含量越多,导电性越好,但是相应的透光率就会变差。
综上所示,本发明的方法制备出的抗静电膜在保证优异导电性的同时获得更加优越的透光率,实现高透光和高导电的结合,是一种综合性能优异的透明抗静电薄膜。
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式,并且很显然,根据上述教导,可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用,从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。
Claims (9)
1.一种抗静电膜的制备方法,其特征在于,包括以下步骤:
获得碳纳米管水性分散液;
将所述碳纳米管水性分散液、水性粘结树脂、烯烃乳液、水以及助剂混合均匀,得到碳纳米管抗静电涂布液;
将所述碳纳米管抗静电涂布液涂布于基材表面,固化后得到抗静电薄膜原膜;以及
将所述抗静电薄膜原膜在有机萃取溶剂中漂洗后,即获得所述抗静电膜;
其中,所述烯烃乳液中烯烃的熔点小于70℃,所述烯烃乳液为石蜡乳液或白油乳液。
2.如权利要求1所述的抗静电膜的制备方法,其特征在于,所述碳纳米管水性分散液按照质量百分比计,包括以下原料组分:
3.如权利要求2所述的抗静电膜的制备方法,其特征在于,所述碳纳米管为单壁碳纳米管或者少壁碳纳米管,所述少壁碳纳米管为管壁层数少于5层的碳纳米管;和/或,所述碳纳米管的直径为0.4-4nm。
4.如权利要求2所述的抗静电膜的制备方法,其特征在于,所述分散剂为阳离子型表面活性剂、阴离子型表面活性剂和非离子型表面活性剂中的一种或多种。
5.如权利要求4所述的抗静电膜的制备方法,其特征在于,所述分散剂由阴离子型表面活性剂与非离子型表面活性剂组成,且所述阴离子型表面活性剂与非离子型表面活性剂的质量比为(1-10):1。
6.如权利要求2所述的抗静电膜的制备方法,其特征在于,所述获得碳纳米管水性分散液的步骤包括:将所述碳纳米管、分散剂和分散液润湿剂采用纳米研磨和高压均质分散手段将其均匀分散在水中,并使用300-600目滤网过滤后,即得到所述碳纳米管水性分散液。
7.如权利要求1所述的抗静电膜的制备方法,其特征在于,所述助剂包括流平剂和基材润湿剂。
8.如权利要求7所述的抗静电膜的制备方法,其特征在于,所述碳纳米管抗静电涂布液按重量百分比计,包括以下原料组分:
9.一种如权利要求1-8任一项所述方法制备的抗静电膜,其特征在于,所述抗静电膜包括基材以及形成于该基材上碳纳米管涂层,所述基材采用柔性透明材料制得,所述碳纳米管涂层的厚度为100nm-10μm。
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