CN113831724B - 一种电磁梯度不对称导电复合材料及其制备方法 - Google Patents

一种电磁梯度不对称导电复合材料及其制备方法 Download PDF

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CN113831724B
CN113831724B CN202111241282.0A CN202111241282A CN113831724B CN 113831724 B CN113831724 B CN 113831724B CN 202111241282 A CN202111241282 A CN 202111241282A CN 113831724 B CN113831724 B CN 113831724B
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王剑
张鑫
唐健斌
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Xihua University
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Abstract

本发明涉及功能复合材料制造领域，具体为一种电磁梯度不对称导电复合材料及其制备方法。本发明首先对聚合物纤维表面进行金属化获得优异导电性，短切后作为骨架，利用短切纤维具有较大长径比、易于搭接的结构特点，实现短切金属化纤维在基体中的连续分布与网络构筑。在超声环境下将电‑磁介质纳米颗粒分散到基体中，浇注到金属化纤维骨架，在真空炉中进行烘干，而电‑磁介质纳米颗粒在重力作用下自然沉降，控制固化时间形成电磁梯度。本发明所制备的电磁梯度不对称导电复合材料，可以通过改变组分配比以及空间结构调节材料的电磁性能；所制复合材料轻质、柔性、结构稳定，可用于电磁屏蔽材料及抗静电材料等领域。

Description

一种电磁梯度不对称导电复合材料及其制备方法
技术领域
本发明涉及功能复合材料制造领域，具体为一种电磁梯度不对称导电复合材料及其制备方法。
背景技术
随着5G 、 AI 、 IoT 等新技术的出现，移动设备终端数量呈现指数增长。电子设备设施的迅速普及带来便利的同时也造成了电磁环境的日益复杂。由电磁辐射带来的电磁污染是比化学因子污染更普遍、危害更大的一种物理因子污染，会对周围环境造成广泛的危害。电磁污染不仅会对精密电子器件造成不利影响，甚至可能对人体健康产生严重危害。因此，亟需采取有效措施来屏蔽电磁波，以控制或减轻不良的电磁污染。电磁波的屏蔽主要是利用导电材料或导磁材料组成屏蔽体来阻断电磁波的传播。其中，基材的导电性是决定电磁屏蔽效能的主要指标。电磁屏蔽材料通常是由金属材料构成。尽管能够获得优异的屏蔽效果，但是其对电磁波的强反射效应会对周围器件产生二次污染。金属材料还有一些严重的缺陷，例如：耐腐蚀性差、加工困难和高密度等，限制了其作为电磁屏蔽材料的使用和发展。此外，可穿戴的小型便携智能产品迅速普及与航空航天轻量化设计对电磁屏蔽材料提出了轻质、柔性、灵活和耐久的新要求。目前，作为金属电磁屏蔽材料的取代品，高分子化合物基复合材料受到了研究者的高度关注。因为，高分子化合物基复合薄膜材料具有耐腐蚀、轻质、易加工和可调控的屏蔽性能等优点。电磁屏蔽材料在实际过程中还会面临动态弯折、空间破损和力学性能不足等问题，这些问题限制了屏蔽薄膜材料的应用领域。因此为了在严苛使用环境下实际实现电磁屏蔽，制备轻质柔性的高性能聚合物基电磁屏蔽复合材料是未来的发展趋势，也是市场的迫切需求。
发明内容
本发明旨在解决如何在聚合物复合材料中有效构筑梯度导电与轻质柔性高性能的技术问题，提供了电磁梯度不对称导电纤维基电磁屏蔽聚合物复合材料及其制备方法。
本发明解决其技术问题采用的技术方案如下。
一种电磁梯度不对称导电复合材料及其制备方法，包括具有垂直取向间隙结构的梯度导电的金属化纤维骨架和在金属化纤维骨架中垂直分布的电-磁介质纳米颗粒填料共同构筑的电-磁/金属化纤维网络，其中，梯度导电的金属化纤维与垂直分布的电-磁介质协同构筑吸收为主导的电磁屏蔽复合材料，其制备步骤为：
（1）将表面金属化后的纤维短切为0.1 mm-10 mm长度；
（2）将短切金属化纤维在去离子水中超声搅拌分散，倒入预制形状的模具中压制成型，将密度不同的单层金属化纤维按密度由高到低向上层层堆叠，然后再次压制成型；
（3）将电-磁介质纳米颗粒填料与基体在超声水浴下进行共混分散；
（4）将（3）制备的分散体按电-磁介质纳米颗粒的质量百分比由高到低分三次浇注到（2）制备的金属化纤维骨架中，每一次浇注后均在真空炉中固化。
所述纤维为芳纶纤维、碳纤维、聚酰亚胺纤维、聚对苯撑苯并二噁唑纤维或超高分子量聚乙烯纤维。
所述金属化方法为化学镀、物理镀或蒸发镀。
所述金属化纤维的单丝平均电阻为0.1 Ω/m-10 Ω/m。
所述单层金属化纤维的密度为1000 g/m2-20 g/m2。
所述电-磁介质纳米颗粒填料由具有高介电常数的电介质和具有高磁导率的磁介质的共混获得，其中高介电常数的电介质为钛酸钡，其中高磁导率的磁介质为四氧化三铁。
所述基体为水性聚氨酯、环氧树脂、聚苯胺、橡胶或聚偏氟乙烯。
所述电介质与磁介质的质量比为2：1。
所述电-磁介质纳米颗粒的总质量百分比梯度设置为50%~5%。
本发明的有益效果在于：（1）梯度导电的金属化纤维骨架孔隙可逐层捕获电磁波，包覆纤维的金属化外壳可对电磁波进行反射与衰减，同时分布于金属化纤维骨架孔隙中的电-磁介质纳米颗粒能对电磁波产生吸收，使电磁波的能量转换为热能而被彻底损耗。（2）对聚合物纤维进行表面金属化，在极大程度上保留了聚合物纤维力学性能的同时获取了优异的导电性，同时拓展了聚合物纤维的应用领域。（3）通过在具有优异透波性能的聚合物纤维表面构筑金属管状结构，极大地增加了电磁波在聚合物纤维内部的多次反射，同时，金属管覆层曲面形状有助于电磁波在复合材料内部的散射。（4）金属化聚合物纤维密度远低于传统金属材料，且导电性能相当，因此实现了电磁屏蔽材料的轻量化。（5）复合材料具有柔性，适用于不规则表面的电磁屏蔽。（6）聚合物纤维为复合材料提供了高强度的力学性能基础，从而使复合材料具备对严苛环境的适用性。
具体实施方式
以下为结合具体实施例对本发明作进一步说明。
实施例1：一种电磁梯度不对称导电复合材料及其制备方法，包括以下步骤。
步骤一，表面金属化聚合物纤维的制备：将高性能芳纶纤维在200 g/L的氢氧化钠溶液中超声处理30 min，去离子水清洗后浸入20 g/L的氯化亚锡酸性溶液3 min，去离子水清洗后浸入0.5 g/L的氯化钯酸性溶液5 min，随后化学镀金属15 min，去离子水清洗烘干后获得金属化芳纶纤维。
步骤二，金属化芳纶纤维骨架的构建：将金属化芳纶纤维短切至长度10 mm，去离子水中超声分散30 min，将分散体倒入预制模具中，过滤、干燥，最后在平板硫化机上2MPa、120 ℃热压成型，将短切金属化芳纶纤维的密度设置为1000 g/m2、800 g/m2、600 g/m2、400 g/m2、200 g/m2、100 g/m2制备金属化芳纶纤维骨架，最后将6层骨架在平板硫化机上1 MPa、120℃热压成型，以制备不对称导电骨架网络。
步骤三，电-磁介质纳米颗粒/水性聚氨酯分散体的制备：分别称取10 wt%、30wt%、50 wt%的四氧化三铁磁性纳米颗粒和钛酸钡纳米颗粒，其中电-磁介质纳米颗粒质量比为2:1，分别加入水性聚氨酯（固含量为30 wt%）中，超声分散30 min。
步骤四，电磁梯度不对称导电复合材料的制备：将步骤三制备得到的电-磁介质纳米颗粒/水性聚氨酯分散体按顺序将50 wt%、30 wt%、10 wt%三次浇注到放置有步骤二制备的不对称导电骨架网络的模具中，每一次均需超声水浴条件下辅助分散体在骨架网络的填充以及真空炉中100℃干燥固化，得到电磁梯度不对称导电复合材料。
实施例2：一种电磁梯度不对称导电复合材料及其制备方法，包括以下步骤。
步骤一，表面金属化高性能纤维的制备：将高性能聚酰亚胺纤维在200 g/L的氢氧化钠溶液中超声处理30 min，随后电磁溅射金属30 min，去离子水清洗烘干后获得金属化聚酰亚胺纤维。
步骤二，金属化聚酰亚胺纤维骨架的构建：将金属化聚酰亚胺纤维短切至长度5mm，加入去离子水中超声分散30 min，将分散体倒入预制模具中，过滤、干燥，最后在平板硫化机上1 MPa、100℃热压成型，将短切金属化聚酰亚胺纤维的密度设置为640 g/m2、320 g/m2、160 g/m2、80 g/m2、20 g/m2制备单层金属化聚酰亚胺纤维骨架，最后将5层骨架在平板硫化机上1 MPa、100℃热压成型，以制备不对称导电骨架网络。
步骤三，制备电-磁介质纳米颗粒/环氧树脂分散体的制备：分别称取5 wt%、20wt%、35 wt%的四氧化三铁磁性纳米颗粒和钛酸钡纳米颗粒，其中电-磁介质纳米颗粒质量比为2:1，分别加入环氧树脂中，超声分散30 min。
步骤四，制备电磁梯度不对称导电复合材料：将步骤三制备得到的电-磁介质纳米颗粒/环氧树脂分散体按顺序将35 wt%、20 wt%、5 wt%分三次浇注到放置有步骤二制备的不对称导电骨架网络的模具中，每一次都要超声水浴条件下辅助分散体在骨架网络的填充以及真空炉中100℃干燥固化，得到电磁梯度不对称导电复合材料。
实施例3：种电磁梯度不对称导电复合材料及其制备方法，包括以下步骤。
步骤一，表面金属化高性能纤维的制备：将高性能超高分子量聚乙烯纤维在200g/L的氢氧化钠溶液中超声处理30 min，随后蒸发镀铜金属30 min，去离子水清洗烘干后获得金属化超高分子量聚乙烯纤维。
步骤二，制备金属化超高分子量聚乙烯纤维骨架的构建：将金属化超高分子量聚乙烯纤维短切至长度0.1 mm，加入去离子中超声分散30 min，将分散体倒入预制模具中，过滤、干燥，最后在平板硫化机上1 MP a、100℃热压成型，将短切金属化超高分子量聚乙烯纤维的密度设置为800 g/m2、600 g/m2、400 g/m2、200 g/m2、100 g/m2、50 g/m2制备金属化超高分子量聚乙烯纤维骨架，最后将6层骨架在平板硫化机上1 MPa、100℃热压成型，以制备不对称导电骨架网络。
步骤三，电-磁介质纳米颗粒/聚偏氟乙烯分散体的制备：分别称取15 wt%、30wt%、45 wt%的四氧化三铁磁性纳米颗粒和钛酸钡纳米颗粒，其中电-磁介质纳米颗粒质量比为2:1，分别加入聚偏氟乙烯（固含量为20 wt%）中，超声分散30 min。
步骤四，制备电磁梯度不对称导电复合材料：将步骤三制备得到的电-磁介质纳米颗粒/聚偏氟乙烯分散体按顺序将45 wt%、30 wt%、15 wt%分三次浇注到放置有步骤二制备的不对称导电骨架网络的模具中，每一次都要超声水浴条件下辅助分散体在骨架网络的填充以及真空干燥箱中100℃干燥固化，得到电磁梯度不对称导电复合材料。

Claims (7)

1.一种电磁梯度不对称导电复合材料的制备方法，其特征在于，包括具有垂直取向间隙结构的梯度导电的金属化纤维骨架和在金属化纤维骨架中垂直分布的钛酸钡和四氧化三铁纳米颗粒填料共同构筑的钛酸钡/四氧化三铁/金属化纤维网络，其中，梯度导电的金属化纤维与垂直分布的钛酸钡/四氧化三铁协同构筑吸收为主导的电磁屏蔽复合材料，所述金属化纤维是指表面金属化后的纤维，所述表面金属化的方法为化学镀、物理镀或蒸发镀，其制备步骤为：
（1）将金属化纤维短切为0.1 mm-10 mm长度；
（2）将短切金属化纤维在去离子水中超声搅拌分散，倒入预制形状的模具中压制成型，将密度不同的单层金属化纤维按密度由高到低向上层层堆叠，然后再次压制成型；
（3）将钛酸钡和四氧化三铁纳米颗粒填料与基体在超声水浴下进行共混分散；
（4）将（3）制备的分散体按钛酸钡和四氧化三铁纳米颗粒的质量百分比由高到低分三次浇注到（2）制备的金属化纤维骨架中，每一次浇注后均在真空炉中固化。
2.根据权利要求1所述的一种电磁梯度不对称导电复合材料的制备方法，其特征在于，纤维为芳纶纤维、碳纤维、聚酰亚胺纤维、聚对苯撑苯并二噁唑纤维或超高分子量聚乙烯纤维。
3.根据权利要求1所述的一种电磁梯度不对称导电复合材料的制备方法，其特征在于，金属化纤维的单丝平均电阻为0.1 Ω/m -10 Ω/m。
4.根据权利要求1所述的一种电磁梯度不对称导电复合材料的制备方法，其特征在于，单层金属化纤维的密度为1000 g/m2-20 g/m2。
5.根据权利要求1所述的一种电磁梯度不对称导电复合材料的制备方法，其特征在于，基体为水性聚氨酯、环氧树脂、聚苯胺、橡胶或聚偏氟乙烯。
6.根据权利要求1所述的一种电磁梯度不对称导电复合材料的制备方法，其特征在于，钛酸钡与四氧化三铁的质量比为2：1。
7.根据权利要求1所述的一种电磁梯度不对称导电复合材料的制备方法，其特征在于，钛酸钡和四氧化三铁纳米颗粒的总质量百分比梯度设置为50%~5%。
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