CN106370290A - 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 - Google Patents
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 Download PDFInfo
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Abstract
本发明涉及一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器及其制备方法,所述压电传感器的结构为:石墨烯/弹性纤维外表覆盖着PVDF纳米纤维,石墨烯包覆弹性纤维。制备方法,包括:将弹性纤维浸入到氧化石墨烯分散液中,放置,取出后烘干,得到表面包覆氧化石墨烯的弹性纤维,还原,清洗,烘干,得到表面包覆石墨烯的弹性纤维;然后和PVDF纺丝液置于静电纺丝仪中,静电纺丝,即得。本发明的制备方法简单,得到的PVDF纳米纤维/石墨烯/弹性纤维压电传感器力学性能稳定,不需要额外的电源支持,即可准确、灵敏监测动态变形信号,循环稳定好;在柔性电子、可穿戴传感器领域具有广阔的应用前景。
Description
技术领域
本发明属于石墨烯复合纤维及其制备领域,特别涉及一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器及其制备方法。
背景技术
石墨烯是由sp2杂化碳原子组成的,呈现出正六边形周期蜂窝点阵结构,具有极薄的厚度。自2004年首次被科学家成功制备出以来,其独特的二维结构和优异的性能受到众多学者的广泛关注。石墨烯常见的制备方法有机械剥离法、氧化还原法、SiC外延生长法和化学气相沉积法(CVD),它具有非同寻常的导电性能,是最坚硬的纳米材料,而且具有极高的光透性、优异的导热能、极高的比表面积、极快的电子迁移速率等特性,这些特性使石墨烯在超级电容器、应变传感器、智能服装领域等方面具有广泛的应用。
传感器是一种检测器件,能察觉到被测物的信息,并能将察觉到的信息,按一定规律变换成为电信号或其他所需形式的信息输出,以达到对检测物的监测。随着科学技术的进步,单靠人们自身的感觉器官来研究事物的规律以及功能已经远远不够了,传感器应运而生。其中可穿戴式传感器发展的最为迅速,它们被用于监测环境、健康等方面,监测的技术越来越成熟、范围越来越广、精密度越来越高。比如智能心率仪,智能体温计等智能便携可穿戴式传感器对于儿童和老人的健康监测有很大的辅助作用。近年来随着可穿戴式传感器的兴起,越来越多的材料用在此类传感器的制备中,其中石墨烯基的可穿戴式传感器近年来得到了很高的关注。
石墨烯基纤维传感器是近年来新兴的传感器,相比于基于金属箔和半导体等的传统传感器,其具有良好的灵敏度、较宽的检测范围、循环稳定性等特性。石墨烯基纤维作为传感器可以充分发挥出纤维的柔韧性、可拉伸性,亦可弯曲扭转,但现有的石墨烯基纤维传感器在应用时都需要对其提供额外的电源以保证其在监测时具有相应的信号,这很大程度上限制了石墨烯基复合纤维在应变传感器领域的应用。
发明内容
本发明所要解决的技术问题是提供一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器及其制备方法,该方法制得的石墨烯/弹性纤维压电传感器在应用时不需要额外的电源支持,即可准确、灵敏监测动态变形信号,循环稳定好,力学性能稳定,在柔性电子、可穿戴传感器领域具有广阔的应用前景。
本发明的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器,所述压电传感器的结构为:石墨烯/弹性纤维外表覆盖着PVDF纳米纤维,石墨烯包覆弹性纤维。
所述弹性纤维为由质量分数1~15%氨纶+99~85%涤纶组成。
本发明的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,包括:
(1)将弹性纤维浸入到氧化石墨烯分散液中,放置,取出后烘干,得到表面包覆氧化石墨烯的弹性纤维;
(2)将步骤(1)中表面包覆氧化石墨烯的弹性纤维进行还原,清洗,烘干,得到表面包覆石墨烯的弹性纤维;
(3)将步骤(2)中的弹性纤维和聚偏氟乙烯PVDF纺丝液置于静电纺丝仪中,弹性纤维置于纺丝液收集处,静电纺丝,得到PVDF纳米纤维/石墨烯/弹性纤维压电传感器;其中,PVDF纺丝液的组成为:质量比为丙酮:N,N-二甲基甲酰胺:PVDF=4~10:8~2:1~1.5。
所述步骤(1)中氧化石墨烯分散液的制备方法:室温下,将氧化石墨溶于去离子水中,得到氧化石墨分散液,超声,得到分散均匀的氧化石墨烯分散液;其中,氧化石墨烯分散液的浓度为1~50mg/mL;超声时间为1~72h。
所述步骤(1)中弹性纤维使用前进行表面改性前处理;其中,前处理的目的在于:使弹性纤维更利于纤维与氧化石墨烯的结合。
所述前处理的方式为:将弹性纤维用去离子水清洗后放置于酒精溶液中,超声处理10~60min,然后氧等离子处理10~60min。
所述步骤(1)中放置的时间为1~60min。
所述步骤(1)中烘干的条件为:40~70℃保温1~5h。
所述步骤(2)中还原的方式为:表面包覆氧化石墨烯的弹性纤维浸入氢碘酸中进行还原,还原时间为1~3h。
所述步骤(2)中清洗为分别用乙醇和去离子水多次清洗;烘干的条件为:40~70℃保温1~5h。
所述步骤(3)中静电纺丝的条件为:电压为10~20kV,静电纺丝时间为1~15min,接收距离为5~20cm。
有益效果
(1)本发明的制备方法简单,无需复杂工艺,制作成本低廉;
(2)本发明通过氧化石墨包覆弹性纤维上还原得到石墨烯/弹性纤维复合物,使石墨烯有一个优异弹性的基底,石墨烯和弹性纤维两者的优点充分的结合在一起,达到了一加一大于二的效果。
(3)本发明所制备的PVDF纳米纤维/石墨烯/弹性纤维压电传感器在应用时不需要额外的电源,弹性纤维在应变时由于PVDF的压电效应使制备的传感器可以自动产生电信号,使传感器摆脱了对外界电源的依赖,能监测出微弱、不同方向的震动,在医用领域、智能穿戴、应变等领域有着广阔的应用前景。
附图说明
图1为实施例1制备PVDF纳米纤维/石墨烯/弹性纤维压电传感器的扫描电镜图;
图2为实施例1制备PVDF纳米纤维/石墨烯/弹性纤维压电传感器的细节扫描电镜图;
图3为实施例1制备PVDF纳米纤维/石墨烯/弹性纤维压电传感器在无外加电源时循环应变2%作用下的时间-电流曲线;
图4为实施例2制备PVDF纳米纤维/石墨烯/弹性纤维压电传感器的扫描电镜图;
图5为实施例3制备PVDF纳米纤维/石墨烯/弹性纤维压电传感器的扫描电镜图。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
在室温下,称取氧化石墨270mg,置于50mL的烧杯中,然后加去离子水30mL配成浓度为9mg/mL的氧化石墨分散液,然后将烧杯放入超声仪中超声处理8h,得到氧化石墨烯分散液。
将由质量分数5%氨纶+95%涤纶组成的弹性纤维用去离子水清洗后放置酒精溶液中,然后超声处理30min,再用氧等离子体处理30min。将处理后的弹性纤维浸入上述氧化石墨烯分散液中,浸泡时间为20min。将浸有氧化石墨烯分散液的弹性纤维放入设置为60℃的烘箱中,时间为2h,得到氧化石墨烯基弹性纤维(氧化石墨烯包覆弹性纤维)。对获得的氧化石墨烯基弹性纤维用氢碘酸还原,时间为1h。将还原后的复合纤维分别用乙醇和去离子水进行多次洗涤除去残留氢碘酸,放入设置为60℃的烘箱中,时间为3h,得到石墨烯基弹性纤维。将按质量比为丙酮:N,N-二甲基甲酰胺:PVDF=6:4:1.12的PVDF静电纺丝溶液用静电纺法纺于石墨烯基弹性纤维上,得到PVDF纳米纤维/石墨烯/弹性纤维压电传感器;其中,静电纺的使用高压为18kV,纺丝时间为3min,接受距离为15cm;石墨烯基弹性纤维置于纺丝液收集处。
图1为制备的PVDF纳米纤维/石墨烯/弹性纤维压电传感器的扫描电镜图,可以看出:石墨烯/弹性纤维外表覆盖着PVDF纳米纤维。图2为制备的PVDF纳米纤维/石墨烯/弹性纤维压电传感器的细节扫描电镜图,可以看出:PVDF纳米纤维、石墨烯和弹性纤维的分层结构。图3为制备的PVDF纳米纤维/石墨烯/弹性纤维压电传感器在无外加电源时循环应变2%作用下的时间-电流曲线,可以明看出:在没有外界电压得支持下,石墨烯/弹性纤维压电传感器发生定量的形变时,依然能产生电信号,并且在多次循环后响应电流依然稳定。
实施例2
在室温下,称取氧化石墨270mg,置于50mL的烧杯中,然后加去离子水30mL配成浓度为9mg/mL的氧化石墨分散液,然后将烧杯放入超声仪中超声处理8h,得到氧化石墨烯分散液。
将由质量分数5%氨纶+95%涤纶组成的弹性纤维用去离子水清洗后放置酒精溶液中,然后超声处理30min,再用氧等离子体处理30min。将处理后的弹性纤维浸入上述氧化石墨烯分散液中,浸泡时间为20min。将浸有氧化石墨烯分散液的弹性纤维放入设置为60℃的烘箱中,时间为2h,得到氧化石墨烯基弹性纤维(氧化石墨烯包覆弹性纤维)。对获得的氧化石墨烯基弹性纤维用氢碘酸还原,时间为1h。将还原后的复合纤维分别用乙醇和去离子水进行多次洗涤除去残留氢碘酸,放入设置为60℃的烘箱中,时间为3h,得到石墨烯基弹性纤维。将按质量比为丙酮:N,N-二甲基甲酰胺:PVDF=6:4:1.12的PVDF静电纺丝溶液用静电纺法纺于石墨烯基弹性纤维上,得到PVDF纳米纤维/石墨烯/弹性纤维压电传感器;其中,静电纺的使用高压为18kV,纺丝时间为9min,接受距离为15cm;石墨烯基弹性纤维置于纺丝液收集处。
图4为制备的PVDF纳米纤维/石墨烯/弹性纤维压电传感器的扫描电镜图,可以看出石墨烯/弹性纤维复合体外裹覆的PVDF纳米纤维较实施例1的样品多了很多。
实施例3
在室温下,称取氧化石墨270mg,置于50mL的烧杯中,然后加去离子水30mL配成浓度为9mg/mL的氧化石墨分散液,然后将烧杯放入超声仪中超声处理8h,得到氧化石墨烯分散液。
将由质量分数5%氨纶+95%涤纶组成的弹性纤维用去离子水清洗后放置酒精溶液中,然后超声处理30min,再用氧等离子体处理30min。将处理后的弹性纤维浸入上述氧化石墨烯分散液中,浸泡时间为20min。将浸有氧化石墨烯分散液的弹性纤维放入设置为60℃的烘箱中,时间为2h,得到氧化石墨烯基弹性纤维(氧化石墨烯包覆弹性纤维)。对获得的氧化石墨基弹性纤维用氢碘酸还原,时间为1h。将还原后的复合纤维分别用乙醇和去离子水进行多次洗涤除去残留氢碘酸,放入设置为60℃的烘箱中,时间为3h,得到石墨烯基弹性纤维。将按质量比为丙酮:N,N-二甲基甲酰胺:PVDF=6:4:1.12的PVDF静电纺丝溶液用静电纺法纺于石墨烯基弹性纤维上,得到PVDF纳米纤维/石墨烯/弹性纤维压电传感器;其中,静电纺的使用高压为18kV,纺丝时间为15min,接受距离为15cm;石墨烯基弹性纤维置于纺丝液收集处。
图5为PVDF纳米纤维/石墨烯/弹性纤维压电传感器的扫描电镜图,可以看出石墨烯/弹性纤维复合体外已经完全被PVDF纳米纤维裹覆,较实施例2样品表面的PVDF纳米纤维多。
Claims (10)
1.一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器,其特征在于,所述压电传感器的结构为:石墨烯/弹性纤维外表覆盖着PVDF纳米纤维,石墨烯包覆弹性纤维。
2.根据权利要求1所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器,其特征在于,所述弹性纤维由1~15wt%氨纶+99~85wt%涤纶组成。
3.一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,包括:
(1)将弹性纤维浸入到氧化石墨烯分散液中,放置,取出后烘干,得到表面包覆氧化石墨烯的弹性纤维;
(2)将步骤(1)中表面包覆氧化石墨烯的弹性纤维进行还原,清洗,烘干,得到表面包覆石墨烯的弹性纤维;
(3)将步骤(2)中的弹性纤维和聚偏氟乙烯PVDF纺丝液置于静电纺丝仪中,弹性纤维置于纺丝液收集处,静电纺丝,得到PVDF纳米纤维/石墨烯/弹性纤维压电传感器;其中,PVDF纺丝液的组分及其质量比为:丙酮:N,N-二甲基甲酰胺:PVDF=4~10:8~2:1~1.5。
4.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(1)中氧化石墨烯分散液的制备方法:室温下,将氧化石墨溶于去离子水中,得到氧化石墨分散液,超声1~72h,得到氧化石墨烯分散液;其中,氧化石墨烯分散液的浓度为1~50mg/mL。
5.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(1)中弹性纤维使用前进行前处理;其中,前处理的方式为:将弹性纤维用去离子水清洗后放置于酒精溶液中,超声处理10~60min,然后氧等离子表面改性处理10~60min。
6.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(1)中放置的时间为1~60min。
7.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(1)和步骤(2)中烘干的条件为:40~70℃保温1~5h。
8.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(2)中还原的方式为:表面包覆氧化石墨烯的弹性纤维浸入氢碘酸中进行还原,还原时间为1~3h。
9.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(2)中清洗为分别用乙醇和去离子水清洗。
10.根据权利要求3所述的一种PVDF纳米纤维/石墨烯/弹性纤维压电传感器的制备方法,其特征在于,所述步骤(3)中静电纺丝的条件为:电压为10~20kV,静电纺丝时间为1~15min,接收距离为5~20cm。
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