CN113737396A - 一种用于摩擦纳米发电机的透气可拉伸纳米纤维复合薄膜材料及其制备方法 - Google Patents
一种用于摩擦纳米发电机的透气可拉伸纳米纤维复合薄膜材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于摩擦纳米发电机的透气可拉伸纳米纤维复合薄膜材料及其制备方法。该材料由纳米纤维和弹性体微球通过静电纺丝共混形成，其中纳米纤维为聚偏氟乙烯‑六氟丙烯共聚物(PVDF‑HFP)，弹性体微球为苯乙烯‑乙烯‑丁烯‑苯乙烯嵌段共聚物。制备方法如下：(1)将纳米纤维前驱体溶解为可供静电纺丝的溶液A；(2)将弹性体微球溶解为可供静电纺丝的溶液B；(3)采用共轭静电纺丝加工技术，同步进行纳米纤维和弹性体微球的纺制，以得到纳米纤维复合薄膜。本发明制备得到的纳米纤维复合薄膜材料具有厚度可调、透气性、防水性和可拉伸性，同时具有良好的摩擦起电效应，且制备方法简单，适合工业化生产，能够作为透气可拉伸的可穿戴摩擦纳米发电机应用潜力。
Description
技术领域
本发明属于柔性电子领域，特别涉及一种用于摩擦纳米发电机的透气可拉伸纳米纤维复合膜及其制备方法。
背景技术
摩擦纳米发电机能够收集低频机械振动、液体流动、生物运动等形式的机械能，并将其转换为电能，在可穿戴电子领域具有广泛的应用前景。对于可穿戴柔性电子器件而言，具有透气、可拉伸、防水等特性是本领域工程应用所期望的；同时，针对应用于摩擦纳米发电机场景的柔性可拉伸材料，其应当位于摩擦序列表负极性或正极性两端的位置，即表面能足够低，易于摩擦起电。
目前，应用于摩擦纳米发电机的可拉伸薄膜材料主要有硅橡胶(PDMS)、EVA弹性体、脂肪族芳香族无规共聚酯(Ecoflex)、水凝胶等。但上述薄膜材料均为致密结构，透气性能较差，作为可穿戴设备应用时易引发皮肤过敏等问题。同时，EVA等材料亲电性能较差，其构建的摩擦纳米发电机输出电压较低，限制了高性能器件的研发及应用。
发明内容
针对上述技术问题，本发明提供一种用于摩擦纳米发电机的可拉伸纳米纤维复合膜及其制备方法。
本发明提供的技术方案如下：
本发明第一方面提供一种用于摩擦纳米发电机的透气可拉伸纳米纤维复合薄膜材料，由纳米纤维前驱体和弹性体通过共轭静电纺丝加工形成，纳米纤维互相堆叠交织形成网状结构，弹性体形成微球构成纳米纤维交织的结点，其中纳米纤维前驱体为聚偏氟乙烯-六氟丙烯共聚物(PVDF-HFP)，弹性体为苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物(SEBS)。
进一步，所述PVDF-HFP的分子量(Mn)为130000～200000，其中PVDF的质量分数为70％，HFP质量分数为30％；
进一步，所述SEBS的分子量(Mn)为70000～90000，其中苯乙烯的质量分数为20％，乙烯-丁烯的质量分数为80％。
进一步，所述纳米纤维前驱体溶于溶剂丙酮-二甲基甲酰胺混合溶液中进行静电纺丝。
进一步，所述弹性体溶于溶剂甲苯-二甲基甲酰胺混合溶液进行微球纺制。
本发明第二方面提供第一方面所述的纳米纤维复合薄膜材料的制备方法，包括以下步骤：
(1)将纳米纤维前驱体溶解为可供静电纺丝的溶液A；
(2)将弹性体溶解为可供静电纺丝的溶液B；
(3)采用共轭静电纺丝加工技术，同步进行纳米纤维纺丝和弹性体微球纺制，以得到纳米纤维复合薄膜。
进一步，所述纳米纤维前驱体溶于溶剂丙酮-二甲基甲酰胺混合溶液，所述弹性体溶于溶剂甲苯-二甲基甲酰胺混合溶液。所述溶剂根据聚合物的溶解性择优选择。
更进一步，所述纳米纤维前驱体占溶液A的质量百分比为15％-18％，弹性体占溶液B的质量百分比为12％-15％。
进一步，所述纳米纤维前驱体占纳米纤维前驱体与弹性体微球总质量的30％-50％。
进一步，所述共轭静电纺丝设备工作电压为负极性-2kV，正极性20kV。
进一步，所述纳米纤维复合薄膜加工时间与最终膜厚度成正比，优选4小时。
进一步，共轭静电纺丝时，纳米纤维和纳米纤维的出丝口正面相对，距离择优选择；出丝口距离收集滚筒为15-20cm。
本发明提供的制备方法能够显著提升纳米纤维机械稳定性、拉伸性和疏水性，其机理如下：共轭静电纺丝过程中，嵌段共聚物弹性体喷射产生的微米/纳米小球与聚合物电纺溶液产生的纳米纤维共同参与堆叠过程，且弹性体微米/纳米小球能够自组装覆盖于聚合物纳米纤维的结点，进而牢固焊接纤维结点，提升纤维薄膜的机械稳定性，避免纤维物理堆积所引发的脱落；另外，弹性体小球具有弹力，能够在拉伸过程中协助纳米纤维吸收机械应变，限制拉伸过程中纤维结点的滑动，改善纳米纤维薄膜拉伸性及恢复性；弹性体小球也增加了纳米纤维薄膜的粗糙度，进而提升了整个薄膜的疏水性能。
本发明的有益效果：
1、本发明制备得到的纳米纤维复合薄膜材料具有厚度可控、透气性、防水性和可拉伸性，同时具有良好的摩擦起电效应；
2、本发明制备得到的纳米纤维复合薄膜材料，弹性体嵌入到了PVDF-HFP纳米纤维中，形成了层状复合结构，弹性体微球能够自组装于纳米纤维的结点处，实现纤维结点的自焊接并抑制拉伸时纤维间的滑动，从而保证了纳米纤维复合薄膜材料的拉伸-回复性能；同时增加了表面粗糙度，提升了复合薄膜材料的疏水性。
3、本发明制备得到的纳米纤维复合薄膜加工方法简单，适合工业化生产。
附图说明
图1为共轭静电纺丝过程示意图，其中PVDF-HFP溶液和SEBS溶液所连接注射器的针尖面对面放置；
图2为实施例1制备的纳米纤维复合薄膜材料拉伸测试图；
图3为实施例3制备的纳米纤维复合薄膜材料拉伸测试图；
图4为不同PVDF-HFP含量的纳米纤维复合薄膜的应力应变曲线，其中PVDF-HFP为仅使用PVDF-HFP制备的薄膜，3-7为30％PVDF-HFP-70％SEBS制备的薄膜。
图5为实施例1制备的纳米纤维复合薄膜材料气动稳定性测试；
图6为实施例1制备的纳米纤维复合薄膜微观形貌图；
图7为实施例3制备的纳米纤维复合薄膜微观形貌图；
图8为不同PVDF-HFP含量的纳米纤维复合薄膜的输出性能，其中横坐标为PVDF-HFP与SEBS的质量比，两者质量总和为10质量份，纵坐标为电压；
具体实施方式
下面通过实施例进一步阐述本发明，本发明的内容完全不限于此。
实施例1
制备纳米纤维复合薄膜，步骤如下：
1)称取1.5g PVDF-HFP聚合物颗粒，加入20ml玻璃瓶中；再加入10ml丙酮-二甲基甲酰胺混合溶液，其中丙酮与二甲基甲酰胺的体积比为6:4，采用磁力搅拌子搅拌4h得到电纺溶液A；
2)称取1.2g SEBS弹性体颗粒，加入20ml玻璃瓶中；再加入10ml甲苯-二甲基甲酰胺混合溶液，其中甲苯与二甲基甲酰胺的体积比为85:15，采用磁力搅拌子搅拌4h得到电纺溶液B；
3)将溶液A和溶液B分别装入两个注射器，连接静电纺丝机，调节静电纺丝参数(电压为-2kV，20kV)开展共轭静电纺丝，其中溶液A的推出速度为0.7ml/h，溶液B的推出速度为2ml/h，得到纳米纤维复合薄膜材料。
实施例2
制备纳米纤维复合薄膜，步骤如下：
1)称取1.5g PVDF-HFP聚合物颗粒，加入20ml玻璃瓶中；再加入10ml丙酮-二甲基甲酰胺混合溶液，其中丙酮与二甲基甲酰胺的体积比为6:4，采用磁力搅拌子搅拌4h得到电纺溶液A；
2)称取1.2g SEBS弹性体颗粒，加入20ml玻璃瓶中；再加入10ml甲苯-二甲基甲酰胺混合溶液，其中甲苯与二甲基甲酰胺的体积比为85:15，采用磁力搅拌子搅拌4h得到电纺溶液B；
3)将溶液A和溶液B分别装入两个注射器，连接静电纺丝机，调节静电纺丝参数(电压为-2kV，20kV)开展共轭静电纺丝，其中溶液A的推出速度为1.1ml/h，溶液B的推出速度为2ml/h，得到纳米纤维复合薄膜材料。
实施例3
制备纳米纤维复合薄膜，步骤如下：
1)称取1.5g PVDF-HFP聚合物颗粒，加入20ml玻璃瓶中；再加入10ml丙酮-二甲基甲酰胺混合溶液，其中丙酮与二甲基甲酰胺的体积比为6:4，采用磁力搅拌子搅拌4h得到电纺溶液A；
2)称取1.2g SEBS弹性体颗粒，加入20ml玻璃瓶中；再加入10ml甲苯-二甲基甲酰胺混合溶液，其中甲苯与二甲基甲酰胺的体积比为15:85，采用磁力搅拌子搅拌4h得到电纺溶液B；
3)将溶液A和溶液B分别装入两个注射器，连接静电纺丝机，调节静电纺丝参数(电压为-2kV，20kV)开展共轭静电纺丝，其中溶液A的推出速度为1.6ml/h，溶液B的推出速度为2ml/h，得到纳米纤维复合薄膜材料。
实施例4
性能和表观测试：
(1)拉伸测试：
图2和图3为实施例1和实施例3制备的纳米纤维复合薄膜材料的拉伸测试结果。从图2、图3中可以看出薄膜宏观颜色为白色，拉伸后能保持良好的机械结构，并不发生断裂。
图4给出了实施例1得到的复合纤维薄膜与传统PVDF-HFP电纺薄膜的应力应变曲线，可以看到传统PVDF-HFP薄膜的断裂伸长率为270％；而本实施例1得到的复合薄膜断裂伸长率达到490％，显著优于传统PVDF-HFP电纺薄膜。
(2)机械结构稳定性测试
图5给出了实施例1制备的纳米纤维复合薄膜材料和传统PVDF-HFP薄膜材料的机械结构稳定性测试结果，可以看到传统PVDF-HFP纤维薄膜在高速气流的吹动下会出现明显的脱层；而经本发明制备的PVDF-HFP/SEBS薄膜在高速气流吹动下能够保持良好的机械结构稳定性。
(3)表观测试：
图6和图7为实施例1、实施例3制备的纳米纤维复合薄膜材料的微观形貌图。从图中可以看到SEBS弹性体嵌入了PVDF-HFP纳米纤维，形成了复合结构。
(4)输出性能测试：
图8为实施例1-3制备的纳米纤维复合薄膜以及纯SEBS弹性体薄膜在相同机械能摩擦下的输出电压。从图8可以看出，随着复合材料中PVDF-HFP含量由30％逐步增加至50％，薄膜的摩擦输出电压从75V增加至约130V，接近纯PVDF-HFP的140V。在PVDF-HFP含量为30％(3:7)和40％(4:6)时，摩擦纳米发电机的输出电压相比较于SEBS弹性体薄膜提升近10倍。
以上所述，仅为本发明较佳的具体实施方式，但本发明保护的范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内所做的任何修改，等同替换和改进等，均应包含在发明的保护范围之内。
Claims (10)
1.一种用于摩擦纳米发电机的透气可拉伸纳米纤维复合薄膜材料及其制备方法，其特征在于：
由纳米纤维前驱体溶液和弹性体溶液通过共轭静电纺丝加工形成，纳米纤维互相堆叠交织形成网状结构，弹性体形成微球并实现纳米纤维交织结点的自焊接，其中纳米纤维前驱体为聚偏氟乙烯-六氟丙烯共聚物(PVDF-HFP)，弹性体为苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物。
2.根据权利要求1所述的纤维复合薄膜材料，其特征在于：所述PVDF-HFP的分子量为130000～200000，其中PVDF的质量分数为70％，HFP质量分数为30％。
3.根据权利要求1所述的纤维复合薄膜材料，其特征在于：所述苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物分子量为70000～90000，其中苯乙烯的质量分数为20％，乙烯-丁烯的质量分数为80％。
4.根据权利要求1所述的纤维复合薄膜材料，其特征在于：所述纳米纤维前驱体溶于溶剂丙酮-二甲基甲酰胺混合溶液中进行纳米纤维纺丝；所述弹性体溶于溶剂甲苯-二甲基甲酰胺混合溶液进行弹性体微球纺制。
5.权利要求1-4任一项所述的纳米纤维复合薄膜材料的制备方法，其特征在于，包括以下步骤：
(1)将纳米纤维前驱体溶解为可供静电纺丝的溶液A；
(2)将弹性体溶解为可供静电纺丝的溶液B；
(3)采用共轭静电纺丝加工技术，同步进行纳米纤维和弹性体微球纺制，以得到纳米纤维复合薄膜。
6.根据权利要求5所述的方法，其特征在于：所述纳米纤维前驱体溶于溶剂丙酮-二甲基甲酰胺混合溶液中进行纳米纤维纺丝，所述弹性体溶于溶剂甲苯-二甲基甲酰胺混合溶液进行弹性体微球纺制。
7.根据权利要求6所述的方法，其特征在于：所述纳米纤维前驱体占溶液A的质量百分比为15％-18％，弹性体占溶液B的质量百分比为12％-15％。
8.根据权利要求5所述的方法，其特征在于：所述纳米纤维前驱体占纳米纤维前驱体与弹性体微球总质量的30％-50％。
9.根据权利要求5所述的方法，其特征在于：所述共轭静电纺丝设备工作电压为负极性-2kV，正极性20kV。
10.根据权利要求5所述的方法，其特征在于：所述纳米纤维前驱体占溶液A和弹性体溶液B通过推进泵控制流速喷丝，其中溶液A和溶液B的流速可根据需求设置。
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