CN106432777A - 一种电磁屏蔽用复合导电薄膜及其制备方法 - Google Patents
一种电磁屏蔽用复合导电薄膜及其制备方法 Download PDFInfo
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- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 3
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- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
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Abstract
一种电磁屏蔽用复合导电薄膜,在高分子聚合物材料表面上覆有石墨烯与金属离子混合镀层。本发明的电磁屏蔽用复合导电薄膜的制备方法,将高分子聚合物材料经碱洗——改性——导电化——表面沉积石墨烯与金属离子混合镀层——纯化去膜——热处理步骤后制得,所述表面沉积石墨烯与金属离子混合镀层步骤采用等离子体电镀法、复合电镀法或多级电镀法。本发明材料具有优良导电性和阻燃性,且制备方法简单。
Description
技术领域
本发明涉及一种复合导电薄膜及其制备方法,特别涉及一种电磁屏蔽用复合导电薄膜及其制备方法。
背景技术
导电泡绵是一种集导电和电磁屏蔽功能于一体的材料,具有导电有效期长,屏蔽效果好,不受温度和湿度的影响,表面电阻值可按实际用途设定等特点,广泛应用于计算机、LED显示器、液晶电视、激光打印机、高速复印机、通讯设备、移动电话、卫星通信、医疗设备、高压机测试、仪表仪器、垫片/隔板、插板电子产品、防震导电的包装。目前,导电泡绵主要采用三维多孔聚氨酯海绵或无纺布为基材,这种以有机高分子材料为基材制备的导电泡绵材料,在电子产品超薄化的趋势下,较小的空间所产生的热量较大,多孔海绵为基体的导电泡绵因密集的孔隙而无法有效进行散热,往往受到震动及设备零部件散热的影响,经常出现热保护以及热过载,甚至发生自燃,严重危及产品使用安全。随着电子技术的快速发展,对电磁屏蔽材料功能化的要求越来越高,现在市场上以高分子材料为基体材料的导电泡绵远远无法满足现代电子技术的发展需求,因此,开发超薄、具有阻燃性能的导电薄膜材料,是电磁屏蔽材料技术发展的迫切需求。
发明内容
本发明要解决的技术问题是,克服现有技术的上述缺陷,提供一种具有优良导电性和阻燃性的电磁屏蔽用复合导电薄膜,同时还提供该电磁屏蔽用复合导电薄膜的制备方法。
本发明解决其技术问题采用的技术方案是:
一种电磁屏蔽用复合导电薄膜,在高分子聚合物材料基体表面上镀覆有石墨烯与金属离子混合层。
进一步地,所述石墨烯与金属离子混合层中,石墨烯层占5~30%,金属离子层占70~95%。所述石墨烯与金属离子混合层的总厚度优选为1.0~5.0μm。
进一步地,所述金属离子优选为镍、铜或其合金中的一种。
所述高分子聚合物材料基体一般采用PE薄膜、聚酰亚胺薄膜或无纺布薄膜中的一种,厚度优选为5~50μm。
本发明的电磁屏蔽用复合导电薄膜的制备方法,按以下步骤进行:
Ⅰ碱洗:将高分子聚合物材料基体置于温度为50~80℃、由浓度为10~60g/L的碱性溶液、浓度为10~60g/L的碱金属碳酸溶液和浓度为0.01~0.1g/L的表面活性剂混合的溶液中处理10~60min;所述碱性溶液优选为氢氧化钠溶液或氢氧化钾溶液,所述碱金属碳酸溶液优选为碳酸钠溶液或碳酸钾溶液;
Ⅱ改性:将经步骤Ⅰ处理后的高分子聚合物材料基体置于温度为50~80℃、由浓度为10~25g/L的N,N-二甲基乙酰胺溶液或N,N-二甲基甲酰胺溶液和浓度为0.1~1.0g/L表面活性剂混合的溶液中处理10~30min;
Ⅲ导电化:将经步骤Ⅱ处理后的材料采用常规的化学镀或物理气相沉积工艺进行镍或铜导电化处理,导电化层厚度一般控制为0.1~1.0μm。
Ⅳ表面镀覆石墨烯与金属离子混合层:一般采用等离子体电镀法、复合电镀法或涂覆电镀法;经比较,效果最优的为等离子体电镀法。
所述复合电镀法为常规的方法,具体为将经步骤Ⅲ处理后的材料置于电镀体系中进行表面镀覆石墨烯与金属离子混合层,所述电镀体系中的电镀溶液为10~30%的金属硫酸盐、2~5%的金属氯化盐、2~5%的硼酸和0.5~1%石墨烯粉末,所述石墨烯粉末的粒径为10~50μm,电镀溶液中采用超声波分散石墨烯粉末,电镀溶液的温度控制为20~50℃,电镀溶液的pH值为2.0~5.0,电镀的电流密度为1~5A/dm2,电镀时间为20~50min,采用金属镍、铜或钛板做催化电极;
所述涂覆电镀法为先将经步骤Ⅲ处理后的材料表面涂覆上石墨烯粉末与PVDF的混合物并烘干,再将涂覆有石墨烯粉末的材料进行表面电镀金属离子层;或者先将经步骤Ⅲ处理后的材料进行表面电镀金属离子层,再将表面镀覆有金属离子层的材料表面涂覆上石墨烯粉末与PVDF的混合物并烘干;所述混合物中石墨烯粉末与PVDF的质量比为(0.1~1.0):1.0,混合物混合后采用超声分散均匀,所述石墨烯粉末的粒径为10~50μm;烘干温度为100~300℃;表面电镀金属离子层的工艺按现有常规技术进行,现有技术中使用的电镀体系中,电镀溶液为10~30%的金属硫酸盐、2~5%的金属氯化盐和2~5%的硼酸,电镀溶液的温度控制为20~50℃,电镀溶液的pH值为2.0~5.0,电镀的电流密度为1~5A/dm2,电镀时间为20~50min,采用金属镍、铜或钛板做催化电极;可根据石墨烯层和金属离子层的镀覆顺序来调整电镀顺序;
所述等离子体电镀法为将经导电化步骤后的材料置于气相与液相混合的电镀体系中进行表面镀覆石墨烯与金属离子混合层,所述石墨烯与金属离子混合层中的金属离子层厚度以双脉冲直流电源工艺控制,其脉冲频率为100~1000KHz,占空比为10~50%,电流密度为1~5A/dm2;所述石墨烯与金属离子混合层中的石墨烯层厚度以等离子体电源工艺控制,其放电电压为1.0~5.0Kv,脉冲频率为1~5s;所述电镀体系中,电镀溶液为10~30%的金属硫酸盐、2~5%的金属氯化盐和2~5%的硼酸,5~10%的含碳气体和1~5%的氮气组成的混合气体以100~500ml/s的速度、压力控制为0.1~1.0MPa持续充入到电镀溶液中,电镀溶液的温度控制为20~50℃,电镀溶液的pH值为2.0~5.0,采用金属镍、铜或钛板做催化电极。所述含碳气体优选为乙炔、甲烷中的一种或多种。
所述石墨烯与金属离子混合层的总厚度控制为1.0~5.0μm,其中石墨烯层占总厚度的5~30%,金属离子层占总厚度的70~95%;所述金属离子优选为镍、铜或其合金中的一种;
Ⅴ纯化去膜:将经步骤Ⅳ后的材料浸于温度为50~80℃、由氢氧化钠或氢氧化钾和水以体积比1:10~20混合的溶液中10~50min;
Ⅵ热处理:将经纯化去膜步骤后的材料置于温度为100~300℃的真空炉或具有保护气氛的热处理炉中处理30~60min,即制得电磁屏蔽用复合导电薄膜。所述保护气氛为惰性气体、氮气或氩气中的一种或多种。
与现有技术相比,本发明的电磁屏蔽用复合导电薄膜,具有以下优点:1、采用石墨烯镀层对高分子聚合物材料基体进行包裹,有效增强了高分子聚合物材料作为基体的耐燃性;2、石墨烯本身具有的导电性解决了高分子聚合物材料的导电化处理,省去了高分子聚合物材料基体表面沉积后的导电化处理步骤,有效节约了生产成本;3、本发明材料具有优良导电性和阻燃性;4、本发明工艺简单,操作方便,产品实用性强,易于实现规模化生产。
具体实施方式
以下结合实施例对本发明作进一步详细说明,但本发明并不局限于实施例之表述。
实施例1
一种电磁屏蔽用复合导电薄膜的制备方法,按以下步骤进行:
Ⅰ碱洗:将厚度为5μm的聚酰亚胺薄膜基体置于温度为50℃、由浓度为10g/L的氢氧化钾溶液、浓度为10g/L的碳酸钠和浓度为0.01g/L的表面活性剂混合的溶液中处理60min;
Ⅱ改性:将经步骤Ⅰ处理后的聚酰亚胺薄膜基体置于温度为50℃、由浓度为10g/L的N,N-二甲基乙酰胺溶液和浓度为0.1g/L表面活性剂混合的溶液中处理30min;
Ⅲ导电化:将经步骤Ⅱ处理后的材料采用常规化学镀工艺进行镍导电化处理,导电化层厚度控制为0.1μm;
Ⅳ表面镀覆石墨烯与镍金属离子混合层:采用等离子体电镀法,将经步骤Ⅲ处理后的材料置于电镀体系中表面镀覆石墨烯与镍金属离子混合层,镍金属离子层厚度以双脉冲直流电源工艺控制,其脉冲频率为100KHz,占空比为10%,电流密度为1A/dm2;石墨烯层厚度以等离子体电源工艺控制,其放电电压为1.0Kv,脉冲频次为1s;电镀体系中,电镀溶液为10%的硫酸镍、2%的氯化镍和2%的硼酸,5%的甲烷和1%的氮气组成的混合气体以100ml/s的速度、压力控制为0.1MPa持续充入到电镀溶液中,电镀溶液的温度控制为20℃,电镀溶液的pH值为2.0,采用金属镍板做催化电极;石墨烯与镍金属离子混合层的总厚度控制为1.0μm,其中石墨烯层占总厚度的5%,镍金属离子层占总厚度的95%;Ⅴ纯化去膜:将经步骤Ⅳ后的材料浸于温度为50℃、由氢氧化钠和水以体积比1:10混合的溶液中50min;
Ⅵ热处理:将经纯化去膜步骤后的材料置于温度为100℃的真空炉中处理60min,即制得电磁屏蔽用复合导电薄膜。
将由上述方法制备得到的电磁屏蔽用复合导电薄膜和常规导电泡绵切成相同体积的样片,分别进行电阻率和阻燃性检测,阻燃性能的检测采用火焰直接燃烧的方法,检测材料在明火下开始燃烧的时间。其检测结果如表1所示。从表1中的数据可看出,本发明的电磁屏蔽用复合导电薄膜比常规导电泡绵的阻燃性能好,起燃时间迟缓了约96%,本发明的电磁屏蔽用复合导电薄膜的导电性能比常规导电泡绵的好。
表1
实施例2
一种电磁屏蔽用复合导电薄膜的制备方法,按以下步骤进行:
Ⅰ碱洗:将厚度为10μm的无纺布薄膜基体置于温度为65℃、由浓度为30g/L的氢氧化钠溶液、浓度为35g/L的碳酸钾和浓度为0.05g/L的表面活性剂混合的溶液中处理30min;
Ⅱ改性:将经步骤Ⅰ处理后的无纺布薄膜基体置于温度为65℃、由浓度为18g/L的N,N-二甲基甲酰胺溶液和浓度为0.5g/L表面活性剂混合的溶液中处理15min;
Ⅲ导电化:将经步骤Ⅱ处理后的材料采用常规物理气相沉积工艺进行铜导电化处理,导电化层厚度控制为0.5μm;
Ⅳ表面镀覆石墨烯与铜金属离子混合层:采用等离子体电镀法,将经步骤Ⅲ处理后的材料置于电镀体系中表面镀覆石墨烯与铜金属离子混合层,铜金属离子层厚度以双脉冲直流电源工艺控制,其脉冲频率为500KHz,占空比为30%,电流密度为2.5A/dm2;石墨烯层厚度以等离子体电源工艺控制,其放电电压为2.5Kv,脉冲频次为3s;电镀体系中,电镀溶液为15%的硫酸铜、3.5%的氯化镍和3.5%的硼酸,7.5%的乙炔和3%的氮气组成的混合气体以300ml/s的速度、压力控制为0.5MPa持续充入到电镀溶液中,电镀溶液的温度控制为35℃,电镀溶液的pH值为3.5,采用金属铜板做催化电极;石墨烯与铜金属离子混合层的总厚度控制为3μm,其中石墨烯层占总厚度的15%,铜金属离子层占总厚度的85%;
Ⅴ纯化去膜:将经步骤Ⅳ后的材料浸于温度为65℃、由氢氧化钾和水以体积比1:15混合的溶液中30min;
Ⅵ热处理:将经纯化去膜步骤后的材料置于温度为150℃且具有惰性气体的热处理炉中处理45min,即制得电磁屏蔽用复合导电薄膜。
将由上述方法制备得到的电磁屏蔽用复合导电薄膜和常规导电泡绵切成相同体积的样片,分别进行电阻率和阻燃性检测,阻燃性能的检测采用火焰直接燃烧的方法,检测材料在明火下开始燃烧的时间。其检测结果如表2所示。从表2中的数据可看出,本发明的电磁屏蔽用复合导电薄膜比常规导电泡绵的阻燃性能好,起燃时间迟缓了约93%,本发明的电磁屏蔽用复合导电薄膜的导电性能比常规导电泡绵的好。
表2
实施例3
一种电磁屏蔽用复合导电薄膜的制备方法,按以下步骤进行:
Ⅰ碱洗:将厚度为50μm的PE薄膜基体置于温度为80℃、由浓度为60g/L的氢氧化钾溶液、浓度为60g/L的碳酸钾和浓度为0.1g/L的表面活性剂混合的溶液中处理10min;
Ⅱ改性:将经步骤Ⅰ处理后的PE薄膜基体置于温度为80℃、由浓度为25g/L的N,N-二甲基乙酰胺溶液和浓度为1.0g/L表面活性剂混合的溶液中处理10min;
Ⅲ导电化:将经步骤Ⅱ处理后的材料采用常规物理气相沉积工艺进行镍导电化处理,导电化层厚度控制为1.0μm;
Ⅳ表面镀覆石墨烯与镍金属离子混合镀层:采用等离子体电镀法,将经步骤Ⅲ处理后的材料置于电镀体系中表面镀覆石墨烯与镍金属离子混合层,镍金属离子层厚度以双脉冲直流电源工艺控制,其脉冲频率为1000KHz,占空比为50%,电流密度为5A/dm2;石墨烯层厚度以等离子体电源工艺控制,其放电电压为5.0Kv,脉冲频次为5s;电镀体系中,电镀溶液为30%的硫酸镍、5%的氯化镍和5%的硼酸,10%的甲烷和5%的氮气组成的混合气体以500ml/s的速度、压力控制为1.0MPa持续充入到电镀溶液中,电镀溶液的温度控制为50℃,电镀溶液的pH值为5.0,采用金属镍板做催化电极;石墨烯与镍金属离子混合层的总厚度控制为5.0μm,其中石墨烯层占总厚度的30%,镍金属离子层占总厚度的70%;
Ⅴ纯化去膜:将经步骤Ⅳ后的材料浸于温度为80℃、由氢氧化钾和水以体积比1:20混合的溶液中10min;
Ⅵ热处理:将经纯化去膜步骤后的材料置于温度为300℃且具有氮气的热处理炉中处理30min,即制得电磁屏蔽用复合导电薄膜。
将由上述方法制备得到的电磁屏蔽用复合导电薄膜和常规导电泡绵切成相同体积的样片,分别进行电阻率和阻燃性检测,阻燃性能的检测采用火焰直接燃烧的方法,检测材料在明火下开始燃烧的时间。其检测结果如表3所示。从表3中的数据可看出,本发明的电磁屏蔽用复合导电薄膜比常规导电泡绵的阻燃性能好,起燃时间迟缓了约94%,本发明的电磁屏蔽用复合导电薄膜的导电性能比常规导电泡绵的好。
表3
实施例4
一种电磁屏蔽用复合导电薄膜的制备方法,按以下步骤进行:
Ⅰ碱洗:将厚度为20μm的聚酰亚胺薄膜基体置于温度为55℃、由浓度为35g/L的氢氧化钾溶液、浓度为35g/L的碳酸钠和浓度为0.06g/L的表面活性剂混合的溶液中处理40min;
Ⅱ改性:将经步骤Ⅰ处理后的聚酰亚胺薄膜基体置于温度为55℃、由浓度为15g/L的N,N-二甲基乙酰胺溶液和浓度为0.35g/L表面活性剂混合的溶液中处理20min;
Ⅲ导电化:将经步骤Ⅱ处理后的材料采用常规化学镀工艺进行镍导电化处理,导电化层厚度控制为0.35μm;
Ⅳ表面镀覆石墨烯与镍金属离子混合层:采用复合电镀法,将经步骤Ⅲ处理后的材料置于电镀体系中进行表面镀覆石墨烯与镍金属离子混合层,电镀体系中的电镀溶液为17%的硫酸镍、3%的氯化镍、3%的硼酸和0.8%石墨烯粉末,石墨烯粉末的粒径为35μm,电镀溶液中采用超声波分散石墨烯粉末,电镀溶液的温度控制为30℃,电镀溶液的pH值为3.0,电镀的电流密度为2.5A/dm2,电镀时间为35min,采用金属镍板做催化电极;石墨烯与镍金属离子混合层的总厚度控制为4.0μm,其中石墨烯层占总厚度的22%,镍金属离子层占总厚度的78%;
Ⅴ纯化去膜:将经步骤Ⅳ后的材料浸于温度为60℃、由氢氧化钠和水以体积比1:13混合的溶液中35min;
Ⅵ热处理:将经纯化去膜步骤后的材料置于温度为150℃的真空炉中处理50min,即制得电磁屏蔽用复合导电薄膜。
将由上述方法制备得到的电磁屏蔽用复合导电薄膜和常规导电泡绵切成相同体积的样片,分别进行电阻率和阻燃性检测,阻燃性能的检测采用火焰直接燃烧的方法,检测材料在明火下开始燃烧的时间。其检测结果如表4所示。从表4中的数据可看出,本发明的电磁屏蔽用复合导电薄膜比常规导电泡绵的阻燃性能好,起燃时间迟缓了约87%,本发明的电磁屏蔽用复合导电薄膜的导电性能比常规导电泡绵的好。
表4
实施例5
本发明的电磁屏蔽用复合导电薄膜的制备方法,按以下步骤进行:
Ⅰ碱洗:将35μm聚酰亚胺薄膜基体置于温度为68℃、由浓度为30g/L的氢氧化钠溶液、浓度为30g/L的碳酸钾溶液和浓度为0.07g/L的表面活性剂混合的溶液中处理55min;
Ⅱ改性:将经步骤Ⅰ处理后的聚酰亚胺薄膜基体置于温度为65℃、由浓度为20g/L的N,N-二甲基甲酰胺溶液和浓度为0.65g/L表面活性剂混合的溶液中处理18min;
Ⅲ导电化:将经步骤Ⅱ处理后的材料采用常规的化学镀工艺进行铜导电化处理,导电化层厚度一般控制为0.6μm。
Ⅳ表面镀覆石墨烯与铜金属离子混合层:采用涂覆电镀法,先将经步骤Ⅲ处理后的材料表面使用涂覆机涂覆上石墨烯粉末与PVDF的混合物,在200℃温度下烘干,石墨烯粉末与PVDF以质量比为0.8:1.0混合并超声分散均匀,石墨烯粉末的粒径为40μm;再将涂覆有石墨烯粉末的材料置于电镀体系中进行表面镀覆铜金属离子层;电镀体系中电镀溶液为22%的硫酸铜、3.5%的氯化铜和3.5%的硼酸,电镀溶液的温度控制为38℃,电镀溶液的pH值为3.0,电镀的电流密度为4A/dm2,电镀时间为38min,采用金属铜板做催化电极;石墨烯与金属离子混合层的总厚度控制为3.0μm,其中石墨烯层占总厚度的18%,金属离子层占总厚度的82%;
Ⅴ纯化去膜:将经步骤Ⅳ后的材料浸于温度为70℃、由氢氧化钠和水以体积比1:17混合的溶液中39min;
Ⅵ热处理:将经纯化去膜步骤后的材料置于温度为180℃且具有氩气的热处理炉中处理48min,即制得电磁屏蔽用复合导电薄膜。
将由上述方法制备得到的电磁屏蔽用复合导电薄膜和常规导电泡绵切成相同体积的样片,分别进行电阻率和阻燃性检测,阻燃性能的检测采用火焰直接燃烧的方法,检测材料在明火下开始燃烧的时间。其检测结果如表5所示。从表5中的数据可看出,本发明的电磁屏蔽用复合导电薄膜比常规导电泡绵的阻燃性能好,起燃时间迟缓了约82%,本发明的电磁屏蔽用复合导电薄膜的导电性能比常规导电泡绵的好。
表5
Claims (10)
1.一种电磁屏蔽用复合导电薄膜,其特征在于:在高分子聚合物材料基体表面上镀覆有石墨烯与金属离子混合层。
2.如权利要求1所述的一种电磁屏蔽用复合导电薄膜,其特征在于:所述石墨烯与金属离子混合层中,石墨烯层占5~30%,金属离子层占70~95%。
3.如权利要求1所述的一种电磁屏蔽用复合导电薄膜,其特征在于:所述石墨烯与金属离子混合层的总厚度为1.0~5.0μm。
4.如权利要求1~3任一所述的一种电磁屏蔽用复合导电薄膜,其特征在于:所述金属离子为镍、铜或其合金中的一种。
5.一种如权利要求1~4任一所述的电磁屏蔽用复合导电薄膜的制备方法,其特征在于:将高分子聚合物材料基体经碱洗——改性——导电化——表面镀覆石墨烯与金属离子混合层——纯化去膜——热处理步骤后制得,所述表面镀覆石墨烯与金属离子混合层步骤采用等离子体电镀法、复合电镀法或涂覆电镀法。
6.如权利要求5所述的一种电磁屏蔽用复合导电薄膜的制备方法,其特征在于:所述涂覆电镀法为先将经步骤Ⅲ处理后的材料表面涂覆上石墨烯粉末与PVDF的混合物并烘干,再将涂覆有石墨烯粉末的材料进行表面电镀金属离子层;或者先将经步骤Ⅲ处理后的材料进行表面电镀金属离子层,再将表面镀覆有金属离子层的材料表面涂覆上石墨烯粉末与PVDF的混合物并烘干;所述混合物中石墨烯粉末与PVDF的质量比为(0.1~1.0):1.0。
7.如权利要求5所述的一种电磁屏蔽用复合导电薄膜的制备方法,其特征在于:所述等离子体电镀法为将经导电化步骤后的材料置于气相与液相混合的电镀体系中进行表面镀覆石墨烯与金属离子混合层,所述石墨烯与金属离子混合层中的金属离子层厚度以双脉冲直流电源工艺控制,其脉冲频率为100~1000KHz,占空比为10~50%,电流密度为1~5A/dm2;所述石墨烯与金属离子混合层中的石墨烯层厚度以等离子体电源工艺控制,其放电电压为1.0~5.0Kv,脉冲频率为1~5s;所述电镀体系中,电镀溶液为10~30%的金属硫酸盐、2~5%的金属氯化盐和2~5%的硼酸,5~10%的含碳气体和1~5%的氮气组成的混合气体以100~500ml/s的速度、压力控制为0.1~1.0MPa持续充入到电镀溶液中,电镀溶液的温度控制为20~50℃,电镀溶液的pH值为2.0~5.0,采用金属镍、铜或钛板做催化电极。
8.如权利要求7所述的一种电磁屏蔽用复合导电薄膜的制备方法,其特征在于:所述含碳气体为乙炔、甲烷中的一种或多种。
9.如权利要求5~8任一所述的一种电磁屏蔽用复合导电薄膜的制备方法,其特征在于:所述石墨烯与金属离子混合层的总厚度控制为1.0~5.0μm,其中石墨烯层占总厚度的5~30%,金属离子层占总厚度的70~95%。
10.如权利要求5~9任一所述的一种电磁屏蔽用复合导电薄膜的制备方法,其特征在于:所述金属离子为镍、铜或其合金中的一种。
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