CN106905699B - 一种限域空间微纳米精密组装法制备聚合物基导电复合材料的方法 - Google Patents

一种限域空间微纳米精密组装法制备聚合物基导电复合材料的方法 Download PDF

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CN106905699B
CN106905699B CN201710070455.4A CN201710070455A CN106905699B CN 106905699 B CN106905699 B CN 106905699B CN 201710070455 A CN201710070455 A CN 201710070455A CN 106905699 B CN106905699 B CN 106905699B
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composite material
nano
micro
polymer matrix
precise assembly
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CN106905699A (zh
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吴大鸣
高小龙
刘颖
郑秀婷
黄尧
何晓祥
萨门
许红
赵中里
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Huabo Jinggong Hebei Province Technology Co ltd
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Beijing University of Chemical Technology
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Abstract

本发明涉及一种限域空间微纳米精密组装法制备聚合物基导电复合材料的方法，属于复合材料制备技术领域；具体包括如下步骤：（1）将导电填料与聚合物基体加入到共混设备中混合均匀得到均相的聚合物/导电填料物料体系；（2）将均相物料体系加入到由两个平板组成的模具中，通过机械压缩的方式对均相共混物进行平面限域压缩；（3）利用压缩模板上设置的微纳结构阵列，对网络上的填料进行进一步压实，进行“阵列锚固”，实现网络的微纳米精密组装，得到复合材料，具有连续紧密的导电网络，同时兼具优良的拉伸性能、柔性和热稳定性。

Description

一种限域空间微纳米精密组装法制备聚合物基导电复合材料 的方法
技术领域
本发明涉及一种高性能聚合物基导电复合材料的制备方法，特别是涉及一种限域空间微纳米精密组装法制备高性能聚合物基导电复合材料的方法，属于复合材料制备技术领域。
背景技术
聚合物基导电复合材料作为重要的功能材料之一，近年来广泛的应用于制造抗静电、导电或者导热需求的电子设备、飞机配件、个人电脑、发光二极管芯片、电磁干扰屏蔽和传感材料、医疗设备、智能生物材料、汽车零部件、家用电器、管道等。大部分聚合物基体本身不导电，因此需要向聚合物基体中添加具有相当大长径比或比表面积的导电填料，形成导电网络才能制备出满足导电要求的复合材料，常用的导电填料有炭黑粒子、碳纤维、片状石墨、碳纳米管和石墨烯。原位聚合法、溶液混合法和熔体共混法是制备聚合物基导电复合材料的常用方法，其中熔体共混是制备填料均匀分散的聚合物基复合材料普遍采用的方法。理论与实践表明，形成连续紧密的导电网络是制备超高电导率聚合物基复合材料的关键，现有的提高复合材料导电性能的方法主要通过提高填料含量达到导电渗流阈值后继续添加直至饱和，即便如此，复合材料的电导率与理论值相差甚远，究其原因主要在于传统方法大多是在特定的热力学和流体动力学条件下让填料在基体中自组装形成导电网络，填料间距具有不可控性，虽然在导电渗流区域可以通过提高填料含量快速提升复合材料的导电性能，但是由于大多聚合物基体粘度高，加上填料之间排斥力，位阻等影响，填料在聚合物基体中很难自组装形成连续紧密的导电网络，距离预期的电导率相差甚远，尤其在经过导电渗流区域之后，复合材料的电导率随着填料含量变化不大，继续提高复合材料的导电性能已经无能为力。本发明采用新的技术路径限域空间微纳米精密组装来达到提高复合材料性能的目的。
发明内容
本发明的目的是提供一种限域空间高性能聚合物基导电复合材料的方法，采用该方法制备的高性能聚合物基导电复合材料具有连续紧密的导电网络，同时兼具优良的拉伸性能、柔性和热稳定性。
为实现上述发明的目的，本发明采取的技术方案如下： 一种空间限域微纳米精密组装法制备高性能聚合物基复合材料的方法，包括如下步骤： （1）将导电填料与聚合物基体按质量比为（0.5～60）： 100 的比例加入到共混设备中混合均匀，通过共混得到均相的聚合物/导电填料物料体系； （2）将步骤（1）制备的均相物料体系加入到由两个平板组成的模具中，通过机械压缩的方式对均相共混物进行平面限域压缩； （3）利用压缩模板上设置的微纳结构阵列，对网络上的填料进行进一步压实，进行“阵列锚固”，实现网络的微纳米精密组装，得到性能优异的复合材料。
步骤（1）所述的导电填料为微纳米尺度的片状填料、纤维状填料、球状导电填料中的一种或两种以上的组合物。所述的片状填料为鳞片石墨、石墨烯中的一种或两种以上的组合物；纤维状填料为碳纤维、碳纳米管中的一种或两种以上的组合物；球状导电填料为炭黑粒子、银粉或氧化镁中的一种或两种以上的组合物。
步骤（1）所述的聚合物基体为热塑性聚合物基体、热固性基体或光固化类基体。所述的热塑性聚合物基体为聚丙烯、尼龙、聚碳酸酯或聚甲基丙烯酸甲酯中的一种或两种以上的组合物；热固性基体为酚醛树脂、聚二甲基硅氧烷或环氧树脂；光固化类基体为环氧丙烯酸酯、聚氨酯丙烯酸酯或聚酯丙烯酸树脂。步骤（1）所述的共混设备包括高速搅拌器、超声分散仪、密炼机、同向双螺杆挤出机、 Buss 挤出机或行星挤出机。
步骤（2）所述的机械压缩方式包括平板压缩、履带压缩或辊压压缩。
步骤（2）所述的平面限域压缩，均相体系首先发生传统方式的自组装成网，其后共混物被进一步压缩直至设定的特征厚度，在该厚度形成过程中，自组装网络上的填料被进一步压实，填料的间距降低到设计的数值，网络密实度大幅提高。
步骤（3）所述的微纳结构阵列为 V-Cut 结构、半球型结构、半圆柱结构、棱镜结构、金字塔结构、棱锥结构或半椭圆球结构中的一种或两种以上的组合。
步骤（3）所述的复合材料的厚度为对均相样品进行机械压缩，使其厚度压缩至接近或小于自组装成网过程中的特征厚度，而特征厚度取决于填料组成网络网线的平均直径。
本发明的有益效果是： （1）通过高速搅拌器、密炼机或者双螺杆挤出机等共混的方法得到聚合物/导电填料均相体系，然后在一定热力学条件下通过机械方式对均相共混物进行平面限域压缩。在压缩过程中，均相体系首先发生传统的自组装成网；其后对共混物进一步压缩直至设定的特征厚度，在该厚度形成过程中，自组装网络上的填料被进一步压实，填料的间距降低到设定的数值，网络密实度大幅度提高。
（2）在压缩过程的后期，通过压缩模板上设置的微纳结构阵列，对网络上的填料进行“阵列锚固”最终完成导电网络的微纳米精密组装。通过这两个步骤可获得强迫组装的连续紧密的导电网络，得到导电性能优异的复合材料。
（3） 采用本发明制备的复合材料中填料形成连续紧密的导电网络，填料之间缝隙变小，尤其在锚固点，填料间距更小，在导电填料低浓度条件下复合材料可获得高电导率。该方法还可以用于制备高导热和高增强聚合物基复合材料。所制备的聚合物基导电复合材料可应用于防静电、电磁干扰屏蔽、可穿戴电子设备、弯曲显示器、柔性电子元件，智能生物材料等。
附图说明
图 1 平板上 v-cut 微结构阵列几何尺寸与排布显微图；
图 2 平板上半椭圆球微结构阵列几何尺寸与排布显微图；
图 3 平板上凸起微结构阵列的锚固作用示意图；
图 4 实验中制备的复合材料部分样品实物图；
图 5 实施例 1 制备的聚二甲基硅氧烷/0.5wt%碳纤维复合材料的断面扫描电镜图片；
图 6 实施例 2 制备的聚二甲基硅氧烷/4wt%碳纤维复合材料的断面扫描电镜图片；
图 7 实施例 3 制备的聚二甲基硅氧烷/4wt%炭黑复合材料的断面扫描电镜图片；
图 8 实施例 4 制备的聚二甲基硅氧烷/3wt%碳纤维+1wt%炭黑复合材料的断面扫描电镜图片；
图 9 实施例 5 制备的聚二甲基硅氧烷/3wt%碳纤维+1wt%碳纳米管复合材料的断面扫描电镜图片；
图 10 实施例 6 制备的聚二甲基硅氧烷/3wt%碳纤维+1wt%石墨烯复合材料的断面扫描电镜图片；
图 11 实施例 7 制备的聚丙烯/5wt%碳纤维复合材料的透射扫描电镜图片；
图 12 实施例 8 制备的聚二甲基硅氧烷/60wt%碳纤维复合材料的断面扫描电镜。
具体实施方式
下面通过实例对本发明做进一步详细说明，这些实例仅用来说明本发明，并不限制本发明的范围。
实施例 1 配置碳纤维浓度为 0.5wt%的聚二甲基硅氧烷/碳纤维混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度 30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。碳纤维几何尺寸为：直径 7um，长度 4mm。然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 1，图 5为实施例 1 制备的复合材料的横截面的扫描电镜图片。实施例 1 的复合材料测试电导率为 0.036S/m。
实施例 2 配置碳纤维浓度为 4wt%的聚二甲基硅氧烷/碳纤维混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度 30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。直径 7um，长度 4mm，然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 1，图 6 为实施例 2 制备的复合材料的横截面的扫描电镜图片。实施例 2 的复合材料测试电导率为 95.2S/m。
实施例 3 配置炭黑浓度为 4wt%的聚二甲基硅氧烷/炭黑混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度 30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。炭黑为 ORIONENGINEEREDCARBONS 公司生产，型号为： XE2-B。然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 1，图 7 为实施例 3制备的复合材料的横截面的扫描电镜图片。实施例 3 的复合材料测试电导率为 182S/m。
实施例 4 配置碳纤维浓度 3wt%，炭黑浓度为 3wt%的聚二甲基硅氧烷/碳纤维+炭黑混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度 30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。碳纤维，直径 7um，长度 4mm，炭黑为 ORION ENGINEERED CARBONS公司生产，型号为：XE2-B。然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 1，图 8 为实施例 4 制备的复合材料的横截面的扫描电镜图片。实施例 4 的复合材料测试电导率为 910S/m。
实施例 5 配置碳纤维浓度 3wt%，碳纳米管浓度为 1wt%的聚二甲基硅氧烷/碳纤维+碳纳米管混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS与固化剂均为道康宁公司生产。碳纤维，直径 7um，长度 4mm，碳纳米管几何尺寸为：直径20-30nm，长度 10-30um，电导率大于 10000S/m，北京德金岛生产。然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 2，图 9 为实施例 5 制备的复合材料的横截面的扫描电镜图片。实施例 5 的复合材料测试电导率为 727S/m。
实施例 6 配置碳纤维浓度 3wt%，石墨烯浓度为 1wt%的聚二甲基硅氧烷/碳纤维+石墨烯混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度 30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。碳纤维，直径 7um，长度 4mm，石墨烯为单层石墨烯粉末，几何尺寸为：厚度 1.0-1.77nm，片层直径 10-50um，苏州恒球科技生产。然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 2，图 10 为实施例 6制备的复合材料的横截面的扫描电镜图片。实施例 6 的复合材料测试电导率为 97.7S/m。
实施例 7 配置碳纤维浓度为 5wt%聚丙烯/碳纤维混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 100r/min 密炼温度 170℃密炼时间 15min。将混合好的物料与PDMS固化剂按照10:1的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。碳纤维，直径 7um，长度 4mm，炭黑为ORION ENGINEERED CARBONS 公司生产，型号为： XE2-B。然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 2，图 11 为实施例 7 制备的复合材料的横截面的扫描电镜图片。实施例 7 的复合材料测试电导率为 0.11S/m。
实施例 8 配置碳纤维浓度为 60wt%的聚二甲基硅氧烷/碳纤维混合物料，加入哈克密炼机中混合，密炼参数为：螺杆转速 50r/min 密炼温度 30℃密炼时间 15min。将混合好的物料与 PDMS 固化剂按照 10:1 的比例混合后放入真空干燥箱中抽真空 10 分钟去除物料中的气泡， PDMS 固化剂为八甲基环四硅氧烷， PDMS 与固化剂均为道康宁公司生产。直径 7um，长度 4mm，然后将均相体系的物料加入平板模具中，利用模压机压缩物料至设定厚度 200um，压力为 5Mpa。 加热模具至 100-130℃，固化 10 分钟，即可得到复合材料。其中一个平板上凸起的微结构阵列几何机构和尺寸如图 1，图 12 为实施例 8 制备的复合材料的横截面的扫描电镜图片。实施例 8 的复合材料测试电导率为 2650S/m。

Claims (10)

1.一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于:包括如下步骤:
(1)将导电填料与聚合物基体按质量比为0.5~60:100的比例加入到共混设备中混合均匀，通过共混得到均相的聚合物/导电填料物料体系；
(2)将步骤(1)制备的均相物料体系加入到由两个平板组成的模具中，通过机械压缩的方式对均相共混物进行平面限域压缩；
(3)利用压缩模板上设置的微纳结构阵列，对网络上的填料进行进一步压实，进行“阵列锚固”，实现网络的微纳米精密组装，得到复合材料。
2.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：步骤(1)所述的导电填料为微纳米尺度的片状填料、纤维状填料、球状导电填料中的一种或两种以上的组合物。
3.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：步骤(1)所述的聚合物基体为热塑性聚合物基体、热固性基体或光固化类基体。
4.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：步骤(1)所述的共混设备包括高速搅拌器、超声分散仪、密炼机、同向双螺杆挤出机、Buss挤出机或行星挤出机。
5.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于:步骤(2)所述的机械压缩方式包括平板压缩、履带压缩或辊压压缩。
6.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：步骤(2)所述的平面限域压缩，均相体系首先发生传统方式的自组装成网，其后共混物被进一步压缩直至设定的特征厚度，在该厚度形成过程中，自组装网络上的填料被进一步压实，填料的间距降低到设计的数值，网络密实度提高。
7.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：步骤(3)所述的微纳结构阵列为V-Cut结构、半球型结构、半圆柱结构、棱镜结构、金字塔结构、棱锥结构或半椭圆球结构中的一种或两种以上的组合。
8.根据权利要求1所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：步骤(3)所述的复合材料的厚度为对均相样品进行机械压缩，使其厚度压缩至接近或小于自组装成网过程中的特征厚度，而特征厚度取决于填料组成网络网线的平均直径。
9.根据权利要求2所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于:所述的片状填料为鳞片石墨、石墨烯中的一种或两种以上的组合物；纤维状填料为碳纤维、碳纳米管中的一种或两种以上的组合物；球状导电填料为炭黑粒子、银粉或氧化镁中的一种或两种以上的组合物。
10.根据权利要求3所述的一种空间限域微纳米精密组装法制备聚合物基复合材料的方法，其特征在于：所述的热塑性聚合物基体为聚丙烯、尼龙、聚碳酸酯或聚甲基丙烯酸甲酯中的一种或两种以上的组合物；热固性基体为酚醛树脂、聚二甲基硅氧烷或环氧树脂；光固化类基体为环氧丙烯酸酯、聚氨酯丙烯酸酯或聚酯丙烯酸树脂。
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