CN114015379A - 一种导电屏蔽胶带及其制备方法 - Google Patents
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Abstract
本发明公开了一种导电屏蔽胶带及其制备方法,导电屏蔽胶带包括基材层,底涂层和导电粘合剂层,其中导电粘合剂层有以下重量份的原料制备而成:60‑80份丙烯酸酯单体,10‑30份氨基化改性碳系导电剂,5‑10份稀释溶剂,0.1‑1份引发剂聚合反应制得。氨基化改性碳系导电剂由50‑60份环氧化碳系导电剂,10‑20份胺基改性剂和0.1‑1份促进剂组成。该导电粘合剂层采用氨基化改性碳系导电剂实现电磁屏蔽功能,能在保证优良导电性、电磁屏蔽性的功能化基础上,与高分子树脂相容性佳,避免了使用单一填料带来的相容性和分散性差,力学性能下降,易产生团聚等问题。本发明所制备的导电屏蔽胶带具有导电性能好,力学性能优异,导电填料不团聚等优点。
Description
技术领域
本发明属于导电屏蔽胶带领域,特别涉及一种复合型导电高分子粘合剂的制备方法。
背景技术
随着信息产业的高速发展,各种无线电设备例如手机、蓝牙等的广泛应用,电磁辐射问题变得日益严重。电磁辐射污染继空气污染、水污染、噪音污染之后成为第四大污染。同时随着电子产业的高速发展,各种商用家用电器的迅猛增加,这些产品内部大量的集成电路元器件在工作时会形成电磁波噪声,而且这些电子元器件正朝着小型化、数字化、高密度集成化的方向发展,这就意味着它们很容易受到外界电磁信号的干扰从而出现各种障碍,产生电磁兼容问题。为了解决电磁波辐射造成的问题,需要采用电磁屏蔽材料对保护对象进行屏蔽。
导电屏蔽技术通常使用金属及其复合材料,这些材料具有较好的屏蔽性能,但是它们存在密度大、加工性能差、成本高、生产效率低等诸多缺点。而近些年来刚刚发展起来的导电高分子材料具有电磁屏蔽性能好、质量轻、易成型、生产效率高等优点。目前常采用的工艺为填料直接掺杂填充型,包括炭黑填充型、金属填充型、纤维填充型,但填料的直接掺杂易存在与高分子基体相容性差的缺点,造成力学性能下降、易产生团聚等问题。
发明内容
本发明一种导电屏蔽胶带及其制备方法,导电屏蔽胶带包括基材层,底涂层和导电粘合剂层。其导电粘合剂层具有导电性能好,力学性能优异,导电填料不团聚等优点。
为达到上述目的,本发明采用的技术方案是:一种导电屏蔽胶带及其制备方法:导电屏蔽胶带包括基材层,底涂层和导电粘合剂层。导电粘合剂层有以下重量份的原料制备而成:60-80份丙烯酸酯单体,10-30份氨基化改性碳系导电剂,5-10份稀释溶剂,0.1-1份引发剂聚合反应制得。
优选的,所述的丙烯酸酯单体为丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸辛酯、2-甲基丙烯酸甲酯、2-甲基丙烯酸乙酯中的一种或多种的物。
优选的,所述的稀释溶剂为丙酮、丁酮、乙酸乙酯、二甲苯、二氯乙烷、乙醇中的一种。
优选的,所述的引发剂为偶氮二异丁腈、过氧化苯甲酰、过氧化苯甲酸叔丁酯、过氧化2-乙基己基酸叔丁酯、1,1-双(叔戊基过氧)环己烷、过氧化醋酸叔戊酯中的一种。
优选的,所述的氨基化改性碳系导电剂由50-60份氧化石墨烯,10-20份氨基化改性剂和0.1-1份促进剂组成。
优选的,所述的氨基化改性碳系导电剂中的氧化石墨烯为厚度0.8-1.2nm的单层氧化石墨烯。
优选的,所述的氨基化改性碳系导电剂中的氨基改性剂为1,6-己二胺、三乙烯四胺中的一种。
优选的,所述的氨基化改性碳系导电剂中的促进剂为三乙胺、三乙醇胺的一种。
优选的,所述的底涂层作用在于连接基材层和导电粘合剂层;所述的基材层为PP薄膜、PE薄膜、PET薄膜、PVC薄膜中的一种;所述的底涂层为美国3M公司生产的K-500底胶产品。
所述的氨基化改性碳系导电剂,其制备方法为将50-60份氧化石墨烯与10-20份氨基化改性剂和0.1-1份促进剂充分混合搅拌,在密闭容器中机械搅拌并控制温度50-80℃,反应2-5小时,得到氨基化改性碳系导电剂。
一种导电屏蔽胶带的制备方法,其特征在于包括以下步骤:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经80℃-120℃在线烘烤3-10分钟,得到带有底胶的基材层。
步骤二:将60-80份丙烯酸酯单体,10-30份氨基化改性碳系导电剂,5-10份稀释溶剂,加入反应釜中,恒温75℃搅拌3min,搅拌转速40-80r/min,然后加入0.1-1份引发剂,升温至80℃反应1h,后降至室温搅拌15-25min,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经80℃-120℃在线烘烤3-10分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
由于上述技术方案的运用,本发明与现有的技术相比具有下列优点:
(1)本发明通过化学接枝的方式对氧化石墨烯进行修饰改性,反应后的氧化石墨烯表面含有氨基基团,氨基基团可在丙烯酸酯单体聚合反应过程中与双键发生迈克尔加成反应,从而实现了氧化石墨烯与高分子链段的共价键连接。
(2)本发明设计合成氨基化改性碳系导电剂作为实现导电屏蔽的功能化组份,与高分子基体相容性佳,通过共价连接避免了传统导电填料易析出、易团聚等现象,所得制品导电性能好,力学性能优异。
附图说明
下面结合附图对本发明技术方案作进一步说明:
附图1为本发明的结构示意图;
其中:1、基材层;2、底涂层;3、导电粘合剂层。
具体实施方式
下面结合实施对本发明作进一步详细说明。
实施例1
氨基化改性碳系导电剂的制备:将50份厚度0.8nm的单层氧化石墨烯与10份1,6-己二胺和0.1份三乙胺充分混合搅拌,在密闭容器中机械搅拌并控制温度50℃,反应5小时,得到氨基化改性碳系导电剂。
导电屏蔽胶带的制备:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经100℃在线烘烤5分钟,得到带有底胶的基材层。
步骤二:将80份丙烯酸甲酯,30份氨基化改性碳系导电剂,10份丙酮加入反应釜中,恒温75℃搅拌3min,搅拌转速40r/min,然后加入0.1份偶氮二异丁腈,升温至80℃反应1h,当反应生成无色透明粘稠液体,降至室温搅拌15min,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经100℃在线烘烤5分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
实施例2
氨基化改性碳系导电剂的制备:将55份厚度1.2nm的单层氧化石墨烯与15份三乙烯四胺和0.5份三乙胺充分混合搅拌,在密闭容器中机械搅拌并控制温度60℃,反应2小时,得到氨基化改性碳系导电剂。
导电屏蔽胶带的制备:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经100℃在线烘烤5分钟,得到带有底胶的基材层。
步骤二:将75份丙烯酸乙酯,20份氨基化改性碳系导电剂,10份丁酮加入反应釜中,恒温75℃搅拌3min,搅拌转速80r/min,然后加入1份过氧化苯甲酰,升温至80℃反应1h,当反应生成无色透明粘稠液体,后降至室温搅拌20min后,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经100℃在线烘烤5分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
实施例3
氨基化改性碳系导电剂的制备:将58份厚度1.2nm的单层氧化石墨烯与13份三乙烯四胺和0.5份三乙醇胺充分混合搅拌,在密闭容器中机械搅拌并控制温度80℃,反应4小时,得到氨基化改性碳系导电剂。
导电屏蔽胶带的制备:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经100℃在线烘烤5分钟,得到带有底胶的基材层。
步骤二:将60份丙烯酸丁酯,25份氨基化改性碳系导电剂,8份乙酸乙酯加入反应釜中,恒温75℃搅拌3min,搅拌转速60r/min,然后加入0.6份过氧化苯甲酸叔丁酯,升温至80℃反应1h,当反应生成无色透明粘稠液体,降至室温搅拌20min后,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经100℃在线烘烤5分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
实施例4
氨基化改性碳系导电剂的制备:将55份厚度0.8nm的单层氧化石墨烯与20份1,6-己二胺和0.7份三乙醇胺充分混合搅拌,在密闭容器中机械搅拌并控制温度65℃,反应4小时,得到氨基化改性碳系导电剂。
导电屏蔽胶带的制备:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经100℃在线烘烤5分钟,得到带有底胶的基材层。
步骤二:将80份丙烯酸辛酯,28份氨基化改性碳系导电剂,10份二甲苯加入反应釜中,恒温75℃搅拌3min,搅拌转速50r/min,然后加入0.3份过氧化2-乙基己基酸叔丁酯,升温至80℃反应1h,当反应生成无色透明粘稠液体,降至室温搅拌25min后,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经100℃在线烘烤5分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
实施例5
氨基化改性碳系导电剂的制备:将60份厚度1.2nm的单层氧化石墨烯与10份三乙烯四胺和1份三乙胺充分混合搅拌,在密闭容器中机械搅拌并控制温度80℃,反应2小时,得到氨基化改性碳系导电剂。
导电屏蔽胶带的制备:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经100℃在线烘烤5分钟,得到带有底胶的基材层。
步骤二:将80份2-甲基丙烯酸甲酯,30份氨基化改性碳系导电剂,10份二氯乙烷加入反应釜中,恒温75℃搅拌3min,搅拌转速70r/min,然后加入0.8份1,1-双(叔戊基过氧)环己烷,升温至80℃反应1h,当反应生成无色透明粘稠液体,降至室温搅拌20min后,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经100℃在线烘烤5分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
对比例1
导电屏蔽胶带的制备:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经100℃在线烘烤5分钟,得到带有底胶的基材层。
步骤二:将80份丙烯酸甲酯,25份厚度0.8nm的单层氧化石墨烯,10份丙酮加入反应釜中,恒温75℃搅拌3min,搅拌转速40r/min,然后加入0.1份偶氮二异丁腈,升温至80℃反应1h,当反应生成无色透明粘稠液体,降至室温搅拌15min,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经100℃在线烘烤5分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
下表为使用导电粘合剂制备的胶带主要性能,其中电磁屏蔽效能在8~12GHz频段测试得到。
表1使用导电粘合剂制备的导电屏蔽胶带主要性能
主要性能 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对比例1 |
电导率S/cm | 3.1×10<sup>-2</sup> | 3.0×10<sup>-2</sup> | 2.8×10<sup>-2</sup> | 3.3×10<sup>-2</sup> | 3.1×10<sup>-2</sup> | 2.0×10<sup>-2</sup> |
拉伸强度MPa | 3.36 | 3.54 | 3.76 | 3.52 | 3.43 | 2.75 |
电磁屏蔽效能dB | 19 | 18 | 16 | 22 | 19 | 12 |
虽然本发明已以较佳实施例公开如上,但它们并不是用来限定本发明的,任何熟习此技艺者,在不脱离本发明之精神和范围内,自当可作各种变化或润饰,因此本发明的保护范围应当以本申请的权利要求保护范围所界定的为准。
Claims (10)
1.一种导电屏蔽胶带,包括基材层、底涂层和导电粘合剂层,其特征在于:所述的底涂层作用在于连接基材层和导电粘合剂层;所述的基材层为PP薄膜、PE薄膜、PET薄膜、PVC薄膜中的一种;所述的底涂层为美国3M公司生产的K-500底胶产品;所述的导电粘合剂层由以下重量份数的原料制备而成:60-80份丙烯酸酯单体,10-30份氨基化改性碳系导电剂,5-10份稀释溶剂,0.1-1份引发剂聚合反应制得。
2.根据权利要求1所述的氨基化改性碳系导电剂由50-60份氧化石墨烯,10-20份氨基化改性剂和0.1-1份促进剂组成。
3.根据权利要求1所述的一种导电屏蔽胶带,其特征在于:所述的丙烯酸酯单体为丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸辛酯、2-甲基丙烯酸甲酯、2-甲基丙烯酸乙酯中的一种或多种的物。
4.根据权利要求1所述的一种导电屏蔽胶带,其特征在于:所述的稀释溶剂为丙酮、丁酮、乙酸乙酯、二甲苯、二氯乙烷、乙醇中的一种。
5.根据权利要求1所述的一种导电屏蔽胶带,其特征在于:所述的引发剂为偶氮二异丁腈、过氧化苯甲酰、过氧化苯甲酸叔丁酯、过氧化2-乙基己基酸叔丁酯、1,1-双(叔戊基过氧)环己烷、过氧化醋酸叔戊酯中的一种。
6.根据权利要求2所述的氨基化改性碳系导电剂,其特征在于:所述的氧化石墨烯为厚度为0.8-1.2nm的单层氧化石墨烯。
7.根据权利要求2所述的氨基化改性碳系导电剂,其特征在于:所述的氨基改性剂为1,6-己二胺、三乙烯四胺中的一种。
8.根据权利要求2所述的氨基化改性碳系导电剂,其特征在于:所述的促进剂包括三乙胺、三乙醇胺中的一种。
9.根据权利要求2所述的氨基化改性碳系导电剂,其制备方法为将50-60份氧化石墨烯与10-20份氨基化改性剂和0.1-1份促进剂充分混合搅拌,在密闭容器中机械搅拌并控制温度50-80℃,反应2-5小时,得到氨基化改性碳系导电剂。
10.一种导电屏蔽胶带的制备方法,其特征在于包括以下步骤:
步骤一:使用印刷辊将K-500底胶涂覆在基材层的表面,然后经80℃-120℃在线烘烤3-10分钟,得到带有底胶的基材层。
步骤二:将60-80份丙烯酸酯单体,10-30份氨基化改性碳系导电剂,5-10份稀释溶剂,加入反应釜中,恒温75℃搅拌3min,搅拌转速40-80r/min,然后加入0.1-1份引发剂,升温至80℃反应1h,后降至室温搅拌15-25min,超声分散1h,即可得到导电粘合剂。
步骤三:将步骤二得到的导电粘合剂均匀涂覆在步骤一的带有底胶的基材底胶表面,然后经80℃-120℃在线烘烤3-10分钟,在底胶层上形成半固态导电粘合剂层,从而制得导电屏蔽胶带。
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