CN109651641A - 一种多层纳米电磁屏蔽复合膜的制备方法 - Google Patents
一种多层纳米电磁屏蔽复合膜的制备方法 Download PDFInfo
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Abstract
本发明提供了一种多层纳米电磁屏蔽复合膜的制备方法,制备步骤如下:(1)将氧化石墨制备成膨化石墨,(2)通过等离子增强化学气相沉积法在膨化石墨表面沉积碳纳米管和磁纳米颗粒,制得复合粉体,(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、复合粉体层和氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层树脂,固化后即得多层纳米电磁屏蔽复合膜。本发明制得的材料的电磁屏蔽值高达88dB,弯曲强度高达76MPa,弯曲模量高达5.3GPa,因此该材料具有良好的电磁屏蔽性能,同时具有优良的力学性能。因此本发明制得的电磁屏蔽材料具有广泛的应用前景。
Description
技术领域
本发明属于屏蔽材料技术领域,具体涉及一种多层纳米电磁屏蔽复合膜的制备方法。
背景技术
近年来,随着科学技术和电子工业的高速发展,各种数字化、高频化的电子电器设备在工作时向空间辐射了大量不同波长和频率的电磁波,从而导致了新的环境污染—电磁波干扰(Electromagnetic Interference,EMI)和放射频率干扰(Radio-FrequencyInterference,RFI)。与此同时,电子元器件也正向着小型化、轻量化、数字化和高密度集成化方向发展,灵敏度越来越高,很容易受到外界电磁干扰而出现误动、图像障碍以及声音障碍等。电磁辐射产生的电磁干扰不仅影响到电子产品的性能实现,而且由此而引起的电磁污染会对人类和其它生物体造成严重的危害。为解决电磁波辐射造成的干扰与泄漏,主要采用电磁屏蔽材料进行屏蔽,实现电子电器设备与环境相调和、相共存的电磁兼容环境(Electro-Magnetic Compatibility,EMC)。
电磁屏蔽技术通常使用标准金属及其复合材料,它们的屏蔽效能很好,但是存在重量大、价格昂贵、易腐蚀、难于调节屏蔽效能等缺点。因此制备重量轻、韧性好、易加工、低成本的电磁屏蔽材料,成为屏蔽电磁辐射的主要方法。
现有的电磁屏蔽材料的制备方法主要有两种,一种是通过喷镀的方式将屏蔽电磁的原料喷涂在基体的表面,另一种是通过原料共混的方式进行制备,喷镀的方式主要用于以金属原料作为屏蔽材料的制备,共混的方式适用于任意原料的混合,然而这种方式容易产生固体填料在混合物沉降形成原料分布不均的现象,从而影响电磁屏蔽的效果。因此,有必要对电磁屏蔽材料的制备方法进行进一步研究。
发明内容
针对以上现有技术存在的问题,本发明的目的在于提供一种多层纳米电磁屏蔽复合膜的制备方法。
为了实现上述目的,本发明提供以下技术方案:
一种多层纳米电磁屏蔽复合膜的制备方法,包括以下步骤:
(1)将氧化石墨放入到600-800℃的马弗炉中保温5-8min得到膨化石墨,将80份膨化石墨浸入1-5M的HCl溶液中,在40-50℃的温度下搅拌反应15-30min,然后通过离心去除上清液,保留下层氧化石墨,将氧化石墨放入烘箱中烘干,研磨,过50-100目筛;
(2)将步骤(1)处理后的研磨粉体置于等离子增强化学气相沉积炉中,利用等离子增强化学气相沉积工艺在膨化石墨上沉积碳纳米管和磁纳米颗粒,得到膨化石墨、碳纳米管和磁纳米颗粒的复合粉体;其中膨化石墨、碳纳米管和磁纳米颗粒的反应质量比为(5-8):5:(1-3),所述反应气体为硅烷气体、氨气和氩气的混合气体,等离子增强化学气相沉积系统使用13.56MHz、300W功率的条件,反应温度为600-800℃;将反应温度降至室温,即得复合粉体;
(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、步骤(2)制得的复合粉体层、氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层树脂,固化后即得多层纳米电磁屏蔽复合膜。
进一步的,所述聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜支撑体的厚度为5-10μm,其中聚苯胺和聚对苯二甲酸乙二醇酯起始原料的质量比为3:5。
进一步的,所述粘结剂为导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯8-14份、酚醛树脂4-8份、NaCl 1-3份、铜粉3-6份、85%乙醇10-20份。
优选的,所述粘结剂为厚度为0.5-1μm的导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯11份、酚醛树脂6份、NaCl 2份、铜粉4.5份、85%乙醇15份。
进一步的,所述的银层、复合粉体层和氧化石墨烯层的厚度均在3-15μm的范围内。
进一步的,所述树脂为氟碳树脂。
有益效果:本发明提供了一种多层纳米电磁屏蔽复合膜的制备方法,本方法通过层叠方式制备出具有层叠结构的多层纳米电磁屏蔽复合膜,首先以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,聚苯胺作为一种导电聚合物,其与具有优良力学性能的聚对苯二甲酸乙二醇酯配合制备薄膜支撑体,使得支撑体兼具导电性和优良的力学性能。通过化学气相沉积法制得膨化石墨、碳纳米管和磁纳米颗粒的复合粉体,膨化石墨具有较高的孔隙度,从而使得碳纳米管和磁纳米颗粒封填于膨化石墨的孔隙内,提高三者之间的相互作用;通过粘合剂依次将银层、复合粉体层和氧化石墨烯层进行层层粘结,最后通过氟碳树脂涂覆在氧化石墨烯层的外表面。其中粘结剂中添加有导电成分,通过与导电银层的衔接从而更加利于磁电的传导,石墨烯二维片状结构使其在少量添加下即形成导电网络,然后再与碳纳米管和磁纳米颗粒的复合,提高电磁屏蔽性能。氟碳树脂具有优良的耐候性,其涂覆在材料的外表面,对材料起到良好的保护作用。该材料在使用过程中,支撑体的一面靠近屏蔽物品的一侧。
本发明制得的材料的电磁屏蔽值高达88dB,弯曲强度高达76MPa,弯曲模量高达5.3GPa,因此该材料具有良好的电磁屏蔽性能,同时具有优良的力学性能。因此本发明制得的电磁屏蔽材料具有广泛的应用前景。
具体实施方式
下面结合具体实施例来进一步描述本发明,但实施例仅是范例性的,并不对本发明的范围构成任何限制。本领域技术人员应该理解的是,在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换,但这些修改和替换均落入本发明的保护范围内。
实施例1
一种多层纳米电磁屏蔽复合膜的制备方法,包括以下步骤:
(1)将氧化石墨放入到700℃的马弗炉中保温7min得到膨化石墨,将80份膨化石墨浸入3M的HCl溶液中,在45℃的温度下搅拌反应23min,然后通过离心去除上清液,保留下层氧化石墨,将氧化石墨放入烘箱中烘干,研磨,过80目筛;
(2)将步骤(1)处理后的研磨粉体置于等离子增强化学气相沉积炉中,利用等离子增强化学气相沉积工艺在膨化石墨上沉积碳纳米管和磁纳米颗粒,得到膨化石墨、碳纳米管和磁纳米颗粒的复合粉体;其中膨化石墨、碳纳米管和磁纳米颗粒的反应质量比为7:5:2,所述反应气体为硅烷气体、氨气和氩气的混合气体,等离子增强化学气相沉积系统使用13.56MHz、300W功率的条件,反应温度为700℃;将反应温度降至室温,即得复合粉体;
(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、步骤(2)制得的复合粉体层、氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层氟碳树脂,固化后即得多层纳米电磁屏蔽复合膜。
所述聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜支撑体的厚度为8μm,其中聚苯胺和聚对苯二甲酸乙二醇酯起始原料的质量比为3:5。
所述粘结剂为导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯11份、酚醛树脂6份、NaCl 2份、铜粉4.5份、85%乙醇15份。
所述的银层的厚度为5μm、复合粉体层的厚度为10μm、氧化石墨烯层的厚度为3μm。
实施例2
一种多层纳米电磁屏蔽复合膜的制备方法,包括以下步骤:
(1)将氧化石墨放入到600℃的马弗炉中保温5min得到膨化石墨,将80份膨化石墨浸入1M的HCl溶液中,在40℃的温度下搅拌反应15min,然后通过离心去除上清液,保留下层氧化石墨,将氧化石墨放入烘箱中烘干,研磨,过50目筛;
(2)将步骤(1)处理后的研磨粉体置于等离子增强化学气相沉积炉中,利用等离子增强化学气相沉积工艺在膨化石墨上沉积碳纳米管和磁纳米颗粒,得到膨化石墨、碳纳米管和磁纳米颗粒的复合粉体;其中膨化石墨、碳纳米管和磁纳米颗粒的反应质量比为5:5:1,所述反应气体为硅烷气体、氨气和氩气的混合气体,等离子增强化学气相沉积系统使用13.56MHz、300W功率的条件,反应温度为600℃;将反应温度降至室温,即得复合粉体;
(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、步骤(2)制得的复合粉体层、氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层氟碳树脂,固化后即得多层纳米电磁屏蔽复合膜。
所述聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜支撑体的厚度为5μm,其中聚苯胺和聚对苯二甲酸乙二醇酯起始原料的质量比为3:5。
所述粘结剂为导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯8份、酚醛树脂4份、NaCl 1份、铜粉3份、85%乙醇10份。
所述的银层的厚度为3μm、复合粉体层的厚度为5μm、氧化石墨烯层的厚度为5μm。
实施例3
一种多层纳米电磁屏蔽复合膜的制备方法,包括以下步骤:
(1)将氧化石墨放入到650℃的马弗炉中保温6min得到膨化石墨,将80份膨化石墨浸入2M的HCl溶液中,在42℃的温度下搅拌反应20min,然后通过离心去除上清液,保留下层氧化石墨,将氧化石墨放入烘箱中烘干,研磨,过60目筛;
(2)将步骤(1)处理后的研磨粉体置于等离子增强化学气相沉积炉中,利用等离子增强化学气相沉积工艺在膨化石墨上沉积碳纳米管和磁纳米颗粒,得到膨化石墨、碳纳米管和磁纳米颗粒的复合粉体;其中膨化石墨、碳纳米管和磁纳米颗粒的反应质量比为6:5:1.5,所述反应气体为硅烷气体、氨气和氩气的混合气体,等离子增强化学气相沉积系统使用13.56MHz、300W功率的条件,反应温度为650℃;将反应温度降至室温,即得复合粉体;
(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、步骤(2)制得的复合粉体层、氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层氟碳树脂,固化后即得多层纳米电磁屏蔽复合膜。
所述聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜支撑体的厚度为6μm,其中聚苯胺和聚对苯二甲酸乙二醇酯起始原料的质量比为3:5。
所述粘结剂为导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯10份、酚醛树脂5份、NaCl 1.5份、铜粉4份、85%乙醇12份。
所述的银层的厚度为5μm、复合粉体层的厚度为8μm、氧化石墨烯层的厚度为7μm。
实施例4
一种多层纳米电磁屏蔽复合膜的制备方法,包括以下步骤:
(1)将氧化石墨放入到800℃的马弗炉中保温8min得到膨化石墨,将80份膨化石墨浸入5M的HCl溶液中,在50℃的温度下搅拌反应30min,然后通过离心去除上清液,保留下层氧化石墨,将氧化石墨放入烘箱中烘干,研磨,过100目筛;
(2)将步骤(1)处理后的研磨粉体置于等离子增强化学气相沉积炉中,利用等离子增强化学气相沉积工艺在膨化石墨上沉积碳纳米管和磁纳米颗粒,得到膨化石墨、碳纳米管和磁纳米颗粒的复合粉体;其中膨化石墨、碳纳米管和磁纳米颗粒的反应质量比为8:5:3,所述反应气体为硅烷气体、氨气和氩气的混合气体,等离子增强化学气相沉积系统使用13.56MHz、300W功率的条件,反应温度为800℃;将反应温度降至室温,即得复合粉体;
(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、步骤(2)制得的复合粉体层、氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层氟碳树脂,固化后即得多层纳米电磁屏蔽复合膜。
所述聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜支撑体的厚度为10μm,其中聚苯胺和聚对苯二甲酸乙二醇酯起始原料的质量比为3:5。
所述粘结剂为导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯14份、酚醛树脂8份、NaCl 3份、铜粉6份、85%乙醇20份。
所述的银层的厚度为15μm、复合粉体层的厚度为15μm、氧化石墨烯层的厚度为5μm。
对比例1
对比例1与实施例1的区别在于,对比例1中的氧化石墨未进行膨化处理。
对比例2
对比例2与实施例1的区别在于,对比例2中未添加磁纳米颗粒。
对比例3
对比例3与实施例1的区别在于,对比例3中未添加氧化石墨烯层。
将实施例1-4以及对比例1-3制得的电磁屏蔽材料进行以下性能测试,电磁性能:按照SJ20524标准,用屏蔽效能法兰同轴测试设备测试,弯曲强度和弯曲模量:采用GB T9341-2008进行测试。测试结果如表1所示,从表1中得出,本发明制得的材料的电磁屏蔽值高达88dB,弯曲强度高达76MPa,弯曲模量高达5.3GPa,因此该材料具有良好的电磁屏蔽性能,同时具有优良的力学性能。因此本发明制得的电磁屏蔽材料具有广泛的应用前景。
表1
测试指标 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 对比例1 | 对比例2 | 对比例3 |
电磁屏蔽值(dB) | 88 | 71 | 76 | 82 | 78 | 60 | 62 |
弯曲强度(MPa) | 76 | 62 | 68 | 73 | 72 | 69 | 67 |
弯曲模量(GPa) | 5.3 | 4.2 | 4.6 | 5.1 | 4.1 | 3.8 | 3.6 |
Claims (6)
1.一种多层纳米电磁屏蔽复合膜的制备方法,其特征在于,包括以下步骤:
(1)将氧化石墨放入到600-800℃的马弗炉中保温5-8min得到膨化石墨,将80份膨化石墨浸入1-5M的HCl溶液中,在40-50℃的温度下搅拌反应15-30min,然后通过离心去除上清液,保留下层氧化石墨,将氧化石墨放入烘箱中烘干,研磨,过50-100目筛;
(2)将步骤(1)处理后的研磨粉体置于等离子增强化学气相沉积炉中,利用等离子增强化学气相沉积工艺在膨化石墨上沉积碳纳米管和磁纳米颗粒,得到膨化石墨、碳纳米管和磁纳米颗粒的复合粉体;其中膨化石墨、碳纳米管和磁纳米颗粒的反应质量比为(5-8):5:(1-3),所述反应气体为硅烷气体、氨气和氩气的混合气体,等离子增强化学气相沉积系统使用13.56MHz、300W功率的条件,反应温度为600-800℃;将反应温度降至室温,即得复合粉体;
(3)以聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜作为支撑体,通过粘结剂在支撑体的上表面依次涂覆一层银层、步骤(2)制得的复合粉体层、氧化石墨烯层,然后再于氧化石墨烯层的上表面涂覆一层树脂,固化后即得多层纳米电磁屏蔽复合膜。
2.根据权利要求1所述的一种多层纳米电磁屏蔽复合膜的制备方法,其特征在于,所述聚苯胺和聚对苯二甲酸乙二醇酯构成的薄膜支撑体的厚度为5-10μm,其中聚苯胺和聚对苯二甲酸乙二醇酯起始原料的质量比为3:5。
3.根据权利要求1所述的一种多层纳米电磁屏蔽复合膜的制备方法,其特征在于,所述粘结剂为导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯8-14份、酚醛树脂4-8份、NaCl 1-3份、铜粉3-6份、85%乙醇10-20份。
4.根据权利要求1所述的一种多层纳米电磁屏蔽复合膜的制备方法,其特征在于,所述粘结剂为厚度为0.5-1μm的导电粘结剂,所述粘结剂由以下重量份的原料混合而成:聚氧化乙烯11份、酚醛树脂6份、NaCl 2份、铜粉4.5份、85%乙醇15份。
5.根据权利要求1所述的一种多层纳米电磁屏蔽复合膜的制备方法,其特征在于,所述的银层、复合粉体层和氧化石墨烯层的厚度均在3-15μm的范围内。
6.根据权利要求1所述的一种多层纳米电磁屏蔽复合膜的制备方法,其特征在于,所述树脂为氟碳树脂。
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