CN110078976B - 一种压电传感材料的制备方法及制备的材料 - Google Patents

一种压电传感材料的制备方法及制备的材料 Download PDF

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CN110078976B
CN110078976B CN201910378733.1A CN201910378733A CN110078976B CN 110078976 B CN110078976 B CN 110078976B CN 201910378733 A CN201910378733 A CN 201910378733A CN 110078976 B CN110078976 B CN 110078976B
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CN110078976A (zh
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李国栋
刘温霞
宋兆萍
王慧丽
于得海
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Hefei Pilot Micro System Integration Co ltd
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Abstract

本发明涉及一种利用聚偏氟乙烯（PVDF）/纤维素/纳米导电颗粒制备压电传感材料的制备方法，属于功能材料及压电传感器制备技术领域。本发明的方法是将PVDF、纤维素、纳米导电颗粒和成孔剂等原料经高温熔接、置换造孔和干燥固化等工艺，制备一种新型压电传感材料。该技术成本较为低廉、生产工艺简单，产品强度大、柔韧性好、灵敏度高，在电子皮肤、虚拟现实、健康监测等智能可穿戴设备方面具有极大的应用潜能。

Description

一种压电传感材料的制备方法及制备的材料
技术领域
本发明涉及压电传感材料的制备方法及制备的材料，属于功能材料及压电传感器制备技术领域。
背景技术
随着信息社会的发展，物联网与智能终端等技术得到了迅速发展，人们对周边环境信息的采集深度与广度不断提升，传感器作为一类十分重要的信息采集器件，正逐渐被广泛应用在机器人、可穿戴电子设备、医疗器械、人机交互和智能蒙皮等领域。柔性压电传感器具有轻薄便携、电学性能优异和集成度高等特点，逐渐成为近年来的研究热点。
专利CN106370290B公开了一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器及其制备方法，该技术利用表面包覆石墨烯的化学纤维与PVDF通过静电纺丝技术制备一种压电传感器。专利CN105527014A公开了一种基于PVDF纳米纤维的柔性振动传感器的制造方法，该技术首先利用磁控溅射将叉指电极溅射在PVDF纳米纤维，再对其进行PDMS封装，得到一种自供电振动传感器。专利CN106805954A披露了一种穿戴式柔性压力传感器及其制备方法，该传感器由上支撑基体、超柔软Ecoflex压力探测头、PVDF压电薄膜、阵列化微凸台支撑结构和下支撑基体五个部分组成，能够灵敏感知测量人体微弱的脉搏跳动力。
然而，上述发明或利用静电纺丝、磁控溅射等技术，制备工艺相对较为复杂，需要特殊制造设备，耗费大量能源，且成本相对较高，大规模工业生产较难实现；或制备的产品结构组成较为复杂、体积相对较大，且柔韧性较差、适应性不强，无法大规模应用于可穿戴电子设备。
发明内容
针对现阶段压电传感材料的制备工艺复杂，且性能不好的问题，本发明提供了一种压电传感材料的制备方法及制备的材料。
一种压电传感材料的制备方法，包括如下步骤：
（1）将PVDF、纤维素、纳米导电颗粒和成孔剂充分混合；
（2）将步骤（1）得到的混合物进行高温处理，利用熔融的PVDF将纤维素、纳米导电颗粒和成孔剂熔接在一起；
（3）将步骤（2）得到的产物进行溶剂置换；
（4）将步骤（3）得到的产物进行干燥脱水得压电传感材料。
所述步骤（1）的成孔剂为：氯化锂、氯化钠、碘化钠、硫酸钠、氯化钾以及硫酸钾中的一种或多种。
所述步骤（1）的原料中PVDF含量为0.1～15%，纤维素含量为0.1～15%，纳米导电颗粒含量为0.1～5%，成孔剂含量为70～85%。
所述步骤（1）的原料需经研磨处理后过200目筛子。
所述步骤（2）的高温处理的温度为150 ℃～300 ℃，优选的温度为180 ℃～250℃。
所述步骤（3）的置换所用溶剂为去离子水或乙醇。
所述步骤（3）的溶剂置换的条件为：置换次数为6～15次，置换间隔时间为1～5小时。
所述步骤（4）的干燥温度为-80 ℃～80 ℃，干燥方式包括：冷冻干燥、烘箱干燥、真空干燥以及超临界干燥中的一种。
所述步骤（1）的纤维素为改性纤维素粉末，包括：甲基纤维素、羧甲基纤维素、羟甲基纤维素、羟乙基纤维素、羟丙基甲基纤维素、微纤化纤维素、纤维素纳米晶以及纳米纤维素中的至少一种。
上述任一方法制备的纤维素基柔性压力传感材料。
所用的纳米导电颗粒为具备导电性能的纳米颗粒，包括：石墨烯、碳纳米管、银纳米线、纳米银粉、纳米铜粉、纳米镍粉、纳米金粉以及MXene中的至少一种。
本发明的有益效果：
1、工艺简单
本发明是将PVDF、纤维素、纳米导电颗粒和成孔剂等原料混合后，经高温熔接、置换造孔和干燥固化等工艺，制备一种新型压电传感材料。本发明以PVDF、纤维素和纳米导电颗粒为原料，通过高温熔接、置换造孔和干燥固化等工艺，制备一种新型压电传感器材。该技术成本较为低廉、生产工艺简单，产品强度大、柔韧性好、灵敏度高，在电子皮肤、虚拟现实、健康监测等智能可穿戴设备方面具有极大的应用潜能。
2、成本较低
本发明的制备工艺简单、原料来源广泛，所制备的压电传感材料环保无毒，密度低、灵敏度高、柔韧性好。
3、应用潜能大
该产品密度较低、灵敏度较高、柔韧性较大、适应性较强等优点，在电子皮肤、虚拟现实、健康监测等智能可穿戴设备方面具有极大的应用潜能。
附图说明
图1为实施例1所制备的PVDF/纤维素/纳米导电颗粒压电传感材料；
图2为实施例1所制备的PVDF/纤维素/纳米导电颗粒压电传感器材扫描电镜图。
具体实施方式
下面结合具体实施例对本发明作进一步说明；除另有指明，实施例中的所述份数均以质量计。
实施例1
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将0.1份PVDF、85份氯化锂、15份纳米纤维素、0.1份MXene加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换12次(每次置换时间为1小时)；最后将上述产品置于50℃真空干燥箱中干燥6小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
实施例2
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将12份PVDF、80份碘化钠、0.1份纳米纤维素、1份纳米镍粉加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换15次(每次置换时间为5小时)；最后将上述产品置于50℃真空干燥箱中干燥10小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
实施例3
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将15份PVDF、70份氯化钾、14份纳米纤维素、1份银纳米线加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换8次(每次置换时间为2小时)；最后将上述产品置于50℃真空干燥箱中干燥12小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
实施例4
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将15份PVDF、70份氯化钠、12份纳米纤维素、3份碳纳米管加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换8次(每次置换时间为2小时)；最后将上述产品置于50℃真空干燥箱中干燥12小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
实施例5
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将15份PVDF、82份氯化钠、1份纳米纤维素、5份石墨烯加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换10次(每次置换时间为2小时)；最后将上述产品置于50℃真空干燥箱中干燥10小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
实施例6
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将15份PVDF、82份氯化钠、1份纳米纤维素、5份石墨烯加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在无水乙醇中溶剂置换10次(每次置换时间为2小时)；最后将上述产品置于-80℃冷冻干燥箱中干燥30小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
对比例1
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将15份PVDF、1份纳米纤维素、3份石墨烯加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换10次(每次置换时间为2小时)；最后将上述产品置于50℃真空干燥箱中干燥10小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
对比例2
一种基于PVDF/纤维素/纳米导电颗粒的压电传感材料的制备方法，包括如下步骤：将15份PVDF、40份氯化钠、1份纳米纤维素、5份石墨烯加入到球磨机中进行研磨；将充分研磨后的产品装入模具置于200 ℃的马弗炉中处理30分钟；将上述产品浸没在80 ℃的去离子水中溶剂置换10次(每次置换时间为2小时)；最后将上述产品置于50℃真空干燥箱中干燥10小时得到基于PVDF/纤维素/纳米导电颗粒的压电传感材料成品。
实施效果例
将实施例1-6及对比例1、2制备的材料的性质比较如下：
Figure DEST_PATH_IMAGE001
因此，本发明制备的复合导电材料，密度较低、回弹率高，制备成压电传感器，在较小压力条件下，灵敏度较高、柔韧性较大等优点，在电子皮肤、虚拟现实、健康监测等智能可穿戴设备方面具有极大的应用潜能。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。

Claims (9)

1.一种压电传感材料的制备方法，其特征在于，包括如下步骤：
（1）将PVDF、纤维素、纳米导电颗粒和成孔剂充分混合；
（2）将步骤（1）得到的混合物进行高温处理，利用熔融的PVDF将纤维素、纳米导电颗粒和成孔剂熔接在一起；
（3）将步骤（2）得到的产物进行溶剂置换；
（4）将步骤（3）得到的产物进行干燥脱水得压电传感材料；
所述步骤（1）的原料中PVDF含量为0.1～15%，纤维素含量为0.1～15%，纳米导电颗粒含量为0.1～5%，成孔剂含量为70～85%。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）的成孔剂为：氯化锂、氯化钠、碘化钠、硫酸钠、氯化钾以及硫酸钾中的一种或多种。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）的原料需经研磨处理后过200目筛子。
4.根据权利要求1所述的制备方法，其特征在于，所述步骤（2）的高温处理的温度为150℃～300 ℃。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤（3）的置换所用溶剂为去离子水或乙醇。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤（3）的溶剂置换的条件为：置换次数为6～15次，置换间隔时间为1～5小时。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤（4）的干燥温度为-80 ℃～80 ℃。
8.根据权利要求1所述的制备方法，其特征在于，所述步骤（1）的纤维素为改性纤维素粉末。
9.一种权利要求1-8任一方法制备的纤维素基柔性压力传感材料。
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