CN114775297B - 一种绝缘导热-电磁屏蔽复合材料及其制备方法和用途 - Google Patents

一种绝缘导热-电磁屏蔽复合材料及其制备方法和用途 Download PDF

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CN114775297B
CN114775297B CN202210320110.0A CN202210320110A CN114775297B CN 114775297 B CN114775297 B CN 114775297B CN 202210320110 A CN202210320110 A CN 202210320110A CN 114775297 B CN114775297 B CN 114775297B
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electromagnetic shielding
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composite material
insulating
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CN114775297A (zh
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刘香兰
吕喆
孔丽菁
张献
林永兴
郑康
田兴友
包超
肖超
丁欣
王艳艳
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Hefei Institutes of Physical Science of CAS
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Abstract

本发明涉及电子封装材料领域，具体涉及一种绝缘导热‑电磁屏蔽复合材料及其制备方法和用途，应用于柔性电子封装技术领域。其制备方法包括如下步骤：(1)通过静电纺丝技术制备含有导热填料的多孔无纺布膜：(2)将液态金属分散在绝缘聚合物的溶液中，获得含有液态金属液滴的混合溶液；(3)将含有液态金属液滴的绝缘聚合物溶液涂布于导热无纺布膜上，液态金属沉积到导热无纺布的上表面，待膜表面干燥后施压处理，使液态金属液滴形成连续金属层。本发明制备的导热‑电磁屏蔽复合膜具有优异的导热性能和高的电磁屏蔽性能，在柔性电子封装领域具有广泛的应用前景，可用作柔性电子器件和可穿戴设备的封装材料。

Description

一种绝缘导热-电磁屏蔽复合材料及其制备方法和用途
技术领域
本发明涉及电子封装材料领域，具体涉及一种绝缘导热-电磁屏蔽复合材料及其制备方法和用途，应用于柔性电子封装技术领域。
背景技术
近年来，随着柔性电子技术与可穿戴设备的快速发展，电子元器件呈现出小型化、集成化、复杂化的趋势，导致电子设备运行时产生大量的积热，影响器件的可靠性和寿命。不仅如此，电子元器件在工作过程中也会产生大量的电磁辐射，如不加以约束，不仅会危害人体健康，还会影响到相邻器件的工作性能，引起仪器精度下降；甚至会导致重要信息的泄露，危及商业及国家安全。要解决上述问题，电子封装材料是其中考量的关键因素之一，目前，兼具导热性能与电磁屏蔽性能的柔性电子封装材料性能不佳，为了简单有效的解决电子设备散热及电磁辐射的问题，迫切需要一种高效的导热和电磁屏蔽双功能电子封装材料。
发明内容
为了解决现有技术中存在的兼具导热性能与电磁屏蔽性能的柔性电子封装材料性能不佳问题，本发明的目的之一是提供一种绝缘导热-电磁屏蔽复合材料的制备方法。
为实现上述目的，本发明采用了以下技术方案：一种绝缘导热-电磁屏蔽复合材料的制备方法，包括如下步骤：
S1、将电磁屏蔽材料按照1:(1-100)的质量比分散在绝缘聚合物溶液中，所述绝缘聚合物溶液中绝缘聚合物的浓度为0.1-10wt％，得到混合溶液；
S2、将混合溶液涂布于导热无纺布上，静置一段时间，待表面干燥后施压处理，即制得绝缘导热-电磁屏蔽复合材料。
作为绝缘导热-电磁屏蔽复合材料的制备方法进一步的改进：
优选的，所述电磁屏蔽材料为液态金属。
优选的，所述液态金属为镓基合金、铟基合金、铋基合金中的一种或两种以上。
优选的，所述绝缘聚合物为乙烯基聚合物、聚苯乙烯、聚酰亚胺前驱体、聚乙烯醇、聚氨酯、蚕丝、纤维素、甲壳素、壳聚糖中的一种或两种以上。
优选的，所述导热无纺布为含有40-80wt％导热填料的多孔无纺布，厚度大于10um。
优选的，所述导热无纺布的制备方法如下：
S1、将高分子聚合物和导热填料溶解于有机溶剂中，得到静电纺织液，所述导热填料在静电纺织液中的含量为40-80wt％；
S2、将静电纺织液进行静电纺织，得到导热无纺布。
优选的，所述高分子聚合物为聚氟乙烯、聚酰亚胺、聚苯乙烯、聚氨酯、聚乙烯醇、聚丙烯腈，聚氧化乙烯、聚氯乙烯、橡胶、蚕丝、纤维素、甲壳素、壳聚糖、丝蛋白中的一种或两种以上。
优选的，所述导热填料为氮化硼、氧化铝、氮化铝、碳化硅、氮化硅中的一种或两种以上。
优选的，步骤S2中涂布为刷涂、刮涂或者流延成膜法中的一种，涂布量为0.02-2ml/cm2。
本发明的目的之二是提供一种由上述任意一项的制备方法制得的绝缘导热-电磁屏蔽复合材料。
本发明的目的之三是提供一种上述绝缘导热-电磁屏蔽复合材料在柔性电子封装领域的用途。
本发明相比现有技术的有益效果在于：
1)本发明公开一种绝缘导热-电磁屏蔽双功能复合材料的制备方法，通过静电纺丝技术制备含有导热填料的多孔无纺布，无纺布的厚度可以通过控制电纺时间来调控；将液态金属分散在含有绝缘聚合物的溶液中，然后将混合溶液涂布到导热无纺布膜上，液态金属液滴在自身的重力下沉积到导热无纺布的上表面，部分液态金属渗透至导热无纺布表面的缝隙中，待膜表面干燥后施压处理，大部分液态金属形成连续金属层，压力作用也使得导热无纺布膜更加致密，进一步提高无纺布的导热性能，最终形成结合紧密的多层结构，提高了复合膜的稳定性。
2)本发明通过静电纺丝工艺制备导热无纺布，根据混合溶液的流变性能选择纺织装置的针头型号，接收电极材料为无纺布、铝箔、铜箔或者硅片，纺丝电压根据纺丝材料进行调整。
3)本发明制得的复合材料结构上包括绝缘聚合物、电磁屏蔽材料和导热无纺布，充分发挥了液态金属的电磁屏蔽性能与导热性能，提升复合材料导热性能的同时，赋予了高效电磁屏蔽性能，能满足电子封装领域导热及电磁屏蔽的实际应用需求。具有高的电磁屏蔽性能和高的热导率，可用作柔性电子器件和可穿戴设备的封装材料。
附图说明
图1为导热-电磁屏蔽双功能绝缘复合材料断面扫描电镜图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明，基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
(1)将0.2g氮化硼纳米片放入5ml六氟异丙醇(HFIP)溶液中，超声分散并磁力搅拌使氮化硼在六氟异丙醇中分散均匀后，加入0.2g蚕丝蛋白海绵，磁力搅拌4h，得到纺丝液；使用静电纺丝设备对纺丝液进行静电纺丝，纺丝电压为9kv，接收电极为硅片，纺丝完成后将纺制出的薄膜放入乙醇浸泡10min后70℃烘箱烘干并剥离，得到自支撑氮化硼-蚕丝蛋白导热无纺布；将所制无纺布裁成直径为25mm的圆片以备用，导热膜无纺布中氮化硼质量分数为50wt.％。
(2)将1.5g液态金属(镓铟合金，75％镓，25％铟)加入5.0g聚乙烯醇(PVA1788)水溶液中，使用超声粉碎机进行超声，超声时间至少9min，制备出液态金属颗粒均匀分散的分散液；其中聚乙烯醇水溶液中PVA比例为4wt.％，液态金属与PVA水溶液质量比为3:10。
(3)取步骤二所述分散液1ml均匀涂覆在步骤一所述氮化硼-蚕丝蛋白导热膜表面，于室温下干燥成膜并施压处理；成膜过程中少部分液态金属颗粒渗入导热膜并填充空隙；大部分液态金属颗粒在导热膜上层堆积形成连续相，表层残留的PVA提供绝缘性，形成了三层结构的复合材料。
对上述制得的复合材料的断面进行扫描电镜，结果如图1所示，由图1可知复合材料具有较为清晰的三层功能结构，上层为绝缘层，中间为连续的液态金属层，下层为结构致密的导热层。
制得的复合膜的导热系数3.79W/m·K，在8.2-12.4GHz范围内电磁屏蔽效能为25dB。
实施例2
(1)将0.2g氮化硼纳米片放入5ml六氟异丙醇(HFIP)溶液中，超声分散并磁力搅拌使氮化硼在六氟异丙醇中分散均匀后，加入0.2g蚕丝蛋白海绵，磁力搅拌4h，得到纺丝液；使用静电纺丝设备对纺丝液进行静电纺丝，纺丝电压为9kv，接收电极为硅片，纺丝完成后将纺制出的薄膜放入乙醇浸泡10min后70℃烘箱烘干并剥离，得到自支撑氮化硼-蚕丝蛋白导热无纺布；将所制无纺布裁成直径为25mm的圆片以备用，导热膜无纺布中氮化硼质量分数为50wt.％。
(2)将2.0g液态金属(镓铟合金，75％镓，25％铟)加入5.0g聚乙烯醇(PVA1788)水溶液中，使用超声粉碎机进行超声，超声时间至少9min，制备出液态金属颗粒均匀分散的分散液；其中聚乙烯醇水溶液中PVA比例为3wt.％，液态金属与PVA水溶液质量比为2:5。
(3)取步骤二所述分散液1ml均匀涂覆在步骤一所述氮化硼-蚕丝蛋白导热膜表面，于室温下干燥成膜并施压处理；成膜过程中少部分液态金属颗粒渗入导热膜并填充空隙；大部分液态金属颗粒在导热膜上层堆积形成连续相，表层残留的PVA提供绝缘性，形成了三层结构的复合材料。
制得的复合膜的导热系数为4.99W/m·K，在8.2-12.4GHz范围内电磁屏蔽效能为35dB。
实施例3
(1)将0.2g氮化硼纳米片放入5ml六氟异丙醇(HFIP)溶液中，超声分散并磁力搅拌使氮化硼在六氟异丙醇中分散均匀后，加入0.2g蚕丝蛋白海绵，磁力搅拌4h，得到纺丝液；使用静电纺丝设备对纺丝液进行静电纺丝，纺丝电压为9kv，接收电极为硅片，纺丝完成后将纺制出的薄膜放入乙醇浸泡10min后70℃烘箱烘干并剥离，得到自支撑氮化硼-蚕丝蛋白导热无纺布；将所制无纺布裁成直径为25mm的圆片以备用，导热膜无纺布中氮化硼质量分数为50wt.％。
(2)将2.5g液态金属(镓铟合金，75％镓，25％铟)加入5.0g聚乙烯醇(PVA1788)水溶液中，使用超声粉碎机进行超声，超声时间至少9min，制备出液态金属颗粒均匀分散的分散液；其中聚乙烯醇水溶液中PVA比例为3wt.％，液态金属与PVA水溶液质量比为5:10。
(3)取步骤二所述分散液1ml均匀涂覆在步骤一所述氮化硼-蚕丝蛋白导热膜表面，于室温下干燥成膜并施压处理；成膜过程中少部分液态金属颗粒渗入导热膜并填充空隙；大部分液态金属颗粒在导热膜上层堆积形成连续相，表层残留的PVA提供绝缘性，形成了三层结构的复合材料。
制得的复合膜的导热系数为5.68W/m·K，在8.2-12.4GHz范围内电磁屏蔽效能为50dB。
实施例4
(1)将0.2g氮化硼纳米片放入5ml六氟异丙醇(HFIP)溶液中，超声分散并磁力搅拌使氮化硼在六氟异丙醇中分散均匀后，加入0.2g蚕丝蛋白海绵，磁力搅拌4h，得到纺丝液；使用静电纺丝设备对纺丝液进行静电纺丝，纺丝电压为9kv，接收电极为硅片，纺丝完成后将纺制出的薄膜放入乙醇浸泡10min后70℃烘箱烘干并剥离，得到自支撑氮化硼-蚕丝蛋白导热无纺布；将所制无纺布裁成直径为25mm的圆片以备用，导热膜无纺布中氮化硼质量分数为50wt.％。
(2)将3g液态金属(镓铟合金，75％镓，25％铟)加入5.0g聚乙烯醇(PVA1788)水溶液中，使用超声粉碎机进行超声，超声时间至少9min，制备出液态金属颗粒均匀分散的分散液；其中聚乙烯醇水溶液中PVA比例为2wt.％，液态金属与PVA水溶液质量比为3:5。
(3)取步骤二所述分散液1ml均匀涂覆在步骤一所述氮化硼-蚕丝蛋白导热膜表面，于室温下干燥成膜并施压处理；成膜过程中少部分液态金属颗粒渗入导热膜并填充空隙；大部分液态金属颗粒在导热膜上层堆积形成连续相，表层残留的PVA提供绝缘性，形成了三层结构的复合材料。
制得的复合膜的导热系数为7.19W/m·K，在8.2-12.4GHz范围内电磁屏蔽效能为75dB。
由实施例1-4复合膜的导热系数和电磁屏蔽效能可知，通过调控液态金属在绝缘聚合物溶液中的浓度，可完善复合结构功能层的形貌，从而改善复合材料的综合性能。
本领域的技术人员应理解，以上所述仅为本发明的若干个具体实施方式，而不是全部实施例。应当指出，对于本领域的普通技术人员来说，还可以做出许多变形和改进，所有未超出权利要求所述的变形或改进均应视为本发明的保护范围。

Claims (6)

1.一种绝缘导热-电磁屏蔽复合材料的制备方法，其特征在于，包括如下步骤：
S1、将电磁屏蔽材料按照1:(1-100)的质量比分散在绝缘聚合物溶液中，所述绝缘聚合物溶液中绝缘聚合物的浓度为0.1-10wt％，得到混合溶液；
S2、将混合溶液涂布于导热无纺布上，静置一段时间，待表面干燥后施压处理，即制得绝缘导热-电磁屏蔽复合材料；
其中，所述电磁屏蔽材料为液态金属；
所述绝缘聚合物为乙烯基聚合物、聚苯乙烯、聚酰亚胺前驱体、聚乙烯醇、聚氨酯、蚕丝、纤维素、甲壳素、壳聚糖中的一种或两种以上；
所述导热无纺布为含有40-80wt％导热填料的多孔无纺布，厚度大于10um；
所述导热无纺布的制备方法如下：
S11、将高分子聚合物和导热填料溶解于有机溶剂中，得到静电纺织液，所述静电纺织液中导热填料的含量为40-80wt％；
S12、将静电纺织液进行静电纺织，得到导热无纺布。
2.根据权利要求1所述的绝缘导热-电磁屏蔽复合材料的制备方法，其特征在于，所述高分子聚合物为聚氟乙烯、聚酰亚胺、聚苯乙烯、聚氨酯、聚乙烯醇、聚丙烯腈、聚氧化乙烯、聚氯乙烯、橡胶、蚕丝、纤维素、甲壳素、壳聚糖、丝蛋白中的一种或两种以上。
3.根据权利要求1或2所述的绝缘导热-电磁屏蔽复合材料的制备方法，其特征在于，所述导热填料为氮化硼、氧化铝、氮化铝、碳化硅、氮化硅中的一种或两种以上。
4.根据权利要求1所述的绝缘导热-电磁屏蔽复合材料的制备方法，其特征在于，步骤S2中所述的涂布为刷涂、刮涂或者流延成膜法中的一种，涂布量为0.02-2ml/cm2。
5.一种权利要求1-4任意一项所述的制备方法制得的绝缘导热-电磁屏蔽复合材料。
6.一种权利要求5所述绝缘导热-电磁屏蔽复合材料在柔性电子封装领域的用途。
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