CN106370221B - 一种自响应pvdf/石墨烯/弹性织物复合传感器的制备方法 - Google Patents
一种自响应pvdf/石墨烯/弹性织物复合传感器的制备方法 Download PDFInfo
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Abstract
本发明涉及一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,包括:将经过前处理的弹性织物浸入氧化石墨烯分散液中,静置,取出弹性织物,烘干,得到氧化石墨烯/弹性织物复合物,然后进行还原,清洗,烘干,得到石墨烯/弹性织物复合物;浸入聚偏氟乙烯PVDF溶液中,取出复合物,烘干,10~20kV极化4~15h,得到自响应PVDF/石墨烯/弹性织物复合传感器。本发明的方法简单,所得到的自响应PVDF/石墨烯/弹性织物传感器不需要额外的电源支持,具有高灵敏度、可拉伸性和循环稳定性,在智能服装上有很大的应用前景。
Description
技术领域
本发明属于石墨烯复合材料的制备领域,特别涉及一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法。
背景技术
“衣食住行”,作为居于人类本能社会活动之首的“衣”,现在远不止“包裹身躯”那么简单了,服装不只是款式的美观与得体,更是讲究穿着的舒适和个性的表达以及多功能的一体化。服装行业的科技发展在今后若干年最主要的任务就是利用高新技术和信息技术改变和提升传统的服装功能,这将主要体现在智能服装的研究和开发上。智能服装是随着科学技术的发展应运而生的产物,它是集多种功能于一体,可以快速、便捷、智能化的服务于人们。智能服装的应用在不断的渗透到每个领域,包括通讯、医疗、运动、军事、娱乐等等,比如:变色军装、保温袜、情绪手套、音乐外套等等。在智能服装中,智能传感器的应用越来越广泛,比如智能心率仪,智能体温计等智能服装,这些服饰对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,其中石墨烯基可穿戴式传感器近年来在智能服装领域得到了很高的关注。
石墨烯是一种由碳原子以sp2杂化轨道组成六角型呈蜂巢晶格的平面薄膜,只有一个碳原子厚度的二维材料。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。石墨烯中各碳原子之间的连接非常柔韧,当施加外部作用力时,碳原子面就会弯曲变形,从而使碳原子不必重新排列来适应外力,保持了结构稳定,这种稳定的晶格结构还使石墨烯具有优秀的导电性。除此外石墨烯还具有优异的导热能、极高的比表面积、高透光性和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、太阳能电池、生物医学、应变传感器、微电子和智能服装领域等方面具有广泛的应用。
石墨烯基的可穿戴式传感器是近年来新兴的传感器,多数具有良好的灵敏度、较宽的检测范围和可重复性。但现在的石墨烯基的可穿戴式传感器在智能服装上测试时都需要额外的电源,使其在应用时很不方便,且大多数石墨烯基的可穿戴式传感器都是有少量裹有石墨烯的线与大片织物结合在一起,这就局限了石墨烯材料在智能服装上的应用,这些附加的因素不利于充分发挥出石墨烯的特性,不能充分的发挥出复合体各自的优势。
发明内容
本发明所要解决的技术问题是提供一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,该方法制得的自响应PVDF/石墨烯/弹性织物复合传感器在应用时不需要额外的电源,即可准确、灵敏监测动态变形信号,循环稳定好;在心率、脉搏等监测上有着广阔的应用前景。
本发明的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,包括:
(1)将经过前处理的弹性织物浸入氧化石墨烯分散液中,静置,取出弹性织物,烘干,得到氧化石墨烯/弹性织物复合物;
(2)将步骤(1)中的氧化石墨烯/弹性织物复合物进行还原,清洗,烘干,得到石墨烯/弹性织物复合物;
(3)将步骤(2)种石墨烯/弹性织物复合物浸入聚偏氟乙烯PVDF溶液中充分吸附,取出复合物,烘干,10~20kV高压极化4~15h,得到自响应PVDF/石墨烯/弹性织物复合传感器;其中,PVDF溶液的组分及其质量比为:丙酮:N,N-二甲基甲酰胺:PVDF=3~10:8~2:0.8~1.5。
所述步骤(1)中弹性织物为由质量分数1~20%氨纶+99~80%涤纶组成。
所述步骤(1)中前处理的方式为:将弹性织物用去离子水清洗后放置于酒精溶液中,然后超声处理10~60min,再用氧等离子体表面改性处理10~120min,利于氧化石墨烯有效的浸渍在织物表面。
所述步骤(1)中氧化石墨烯分散液的浓度为1~60mg/mL。
所述氧化石墨烯分散液的制备方法为:在室温下,将氧化石墨加入去离子水中,超声,得到氧化石墨烯分散液;其中,超声的时间为1~96h。
所述步骤(1)中静置的时间为1~60min。
所述步骤(1)中烘干的条件为:40~80℃保温1~5h,优选40~75℃保温1~5h。
所述步骤(2)中还原的方式为:氢碘酸还原1~3h。
所述步骤(2)中清洗的条件为:乙醇和去离子水分别清洗;烘干的条件为:40~80℃保温1~5h。
所述步骤(3)中浸入的时间为10~120min。
所述步骤(3)中烘干的条件为:40~80℃保温1~5h,优选50~80℃保温1~5h。
有益效果
(1)本发明的制备方法简单,制作成本低廉,工艺简便;
(2)本发明通过石墨烯和弹力织物的结合,使石墨烯有一个优异弹性的基底,石墨烯和弹性织物两者的优点充分的结合在一起,并且石墨烯和弹性织物不易分开,并可以水洗;
(3)本发明所制备的自响应PVDF/石墨烯/弹性织物复合传感器在应用时不需要额外的电源,弹性织物由于具有压电效应的PVDF的存在,在受到外部刺激时产生应变后可以自响应产生电信号,摆脱了对外界电源的依赖,在心率、脉搏等智能穿戴方面有着广阔的应用前景。
附图说明
图1为实施例1制备自响应PVDF/石墨烯/弹性织物复合传感器的扫描电镜图;
图2为实施例1制备自响应PVDF/石墨烯/弹性织物复合传感器在无外加电源时循环应变1%作用下的时间-电流曲线;
图3为实施例1制备石墨烯/弹性织物复合物的扫描电镜图;
图4为实施例2制备石墨烯/弹性织物复合物的扫描电镜图;
图5为实施例3制备石墨烯/弹性织物复合物的扫描电镜图。
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6h,得到氧化石墨烯分散液。
将由质量分数5%氨纶+95%涤纶组成的弹性织物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60min。将处理后的弹性织物浸入上述氧化石墨烯分散液中,浸泡时间为20min。将浸有氧化石墨分散液的弹性织物放入设置为60℃的烘箱中,时间为2h,得到氧化石墨烯/弹性织物复合物。对获得的氧化石墨烯/弹性织物复合物用氢碘酸还原,时间为1.5h。将还原后的织物用乙醇和去离子水进行多次洗涤,放入设置为60℃的烘箱中,时间为3h,得到石墨烯/弹性织物复合物。将上述复合物浸入PVDF(聚偏氟乙烯)溶液中,时间为30min,充分吸附后将其放入设置为70℃的烘箱中,时间为3h,烘干后用10kV高压极化5h,得到自响应PVDF/石墨烯/弹性织物复合传感器;其中,PVDF溶液的各组分及其质量比为:丙酮:N,N-二甲基甲酰胺:PVDF=6:4:1.12。
图1为制备自响应PVDF/石墨烯/弹性织物复合传感器的扫描电镜图,可以看出:在石墨烯/弹性织物表面浸渍了一定量的PVDF溶液,这样的组件在高压极化后可以作为自响应传感器使用。图2为制备自响应PVDF/石墨烯/弹性织物复合传感器在无外加电源时循环应变1%作用下的时间-电流曲线,可以看出:在无外加电源的支持下,在多次循环后响应电流依然稳定。图3为制备石墨烯/弹性织物复合物的扫描电镜图,可以看出:弹性织物表面覆盖有石墨烯。
实施例2
在室温下,称取氧化石墨90mg,置于50mL的烧杯中,然后加去离子水30mL配成浓度为3mg/mL的氧化石墨分散液,然后将烧杯放入超声仪中超声处理6h,得到氧化石墨烯分散液。
将由质量分数5%氨纶+95%涤纶组成的弹性织物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60min。将处理后的弹性织物浸入上述氧化石墨烯分散液中,浸泡时间为20min。将浸有氧化石墨分散液的弹性织物放入设置为60℃的烘箱中,时间为2h,得到氧化石墨烯/弹性织物复合物。对获得的氧化石墨/弹性织物复合物用氢碘酸还原,时间为1.5h。将还原后的织物用乙醇和去离子水进行多次洗涤,放入设置为60℃的烘箱中,时间为3h,得到石墨烯/弹性织物复合物。将上述复合物浸入PVDF(聚偏氟乙烯)溶液中,时间为30min,充分吸附后将其放入设置为70℃的烘箱中,时间为3h,烘干后用10kV高压极化5h后得到自响应PVDF/石墨烯/弹性织物复合传感器;其中,PVDF溶液的各组分及其质量比为:丙酮:N,N-二甲基甲酰胺:PVDF=6:4:1.12。
图4为制备仅有石墨烯/弹性织物复合物的扫描电镜图,可以看出:由于初始的氧化石墨分散液的浓度相较实施例1的低,所以弹性织物表面覆盖的石墨烯的量较实施例1的少。
实施例3
在室温下,称取氧化石墨450mg,置于50mL的烧杯中,然后加去离子水30mL配成浓度为15mg/mL的氧化石墨分散液,然后将烧杯放入超声仪中超声处理6h,得到氧化石墨烯分散液。
将由质量分数5%氨纶+95%涤纶组成的弹性织物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60min。将处理后的弹性织物浸入上述氧化石墨烯分散液中,浸泡时间为20min。将浸有氧化石墨分散液的弹性织物放入设置为60℃的烘箱中,时间为2h,得到氧化石墨烯/弹性织物复合物。对获得的氧化石墨/弹性织物复合物用氢碘酸还原,时间为1.5h。将还原后的织物用乙醇和去离子水进行多次洗涤,放入设置为60℃的烘箱中,时间为3h,得到石墨烯/弹性织物复合物。将上述复合物浸入PVDF(聚偏氟乙烯)溶液中,时间为30min,充分吸附后将其放入设置为70℃的烘箱中,时间为3h,烘干后用10kV高压极化5h后得到自响应PVDF/石墨烯/弹性织物复合传感器;其中,PVDF溶液的各组分及其质量比为:丙酮:N,N-二甲基甲酰胺:PVDF=6:4:1.12。
图5为制备仅有石墨烯/弹性织物复合物的扫描电镜图,可以看出:由于初始的氧化石墨分散液的浓度较实施例1的高,所以弹性织物表面覆盖的石墨烯的量较实施例1的多。
Claims (9)
1.一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,包括:
(1)将经过前处理的弹性织物浸入氧化石墨烯分散液中,静置,取出弹性织物,烘干,得到氧化石墨烯/弹性织物复合物,其中前处理的方式为:将弹性织物用去离子水清洗后放置于酒精溶液中,然后超声处理10~60min,再用氧等离子体表面改性处理10~120min;
(2)将步骤(1)中的氧化石墨烯/弹性织物复合物进行还原,清洗,烘干,得到石墨烯/弹性织物复合物,其中还原是用氢碘酸;
(3)将步骤(2)种石墨烯/弹性织物复合物浸入聚偏氟乙烯PVDF溶液中,取出复合物,烘干,10~20kV极化4~15h,得到自响应PVDF/石墨烯/弹性织物复合传感器;其中,PVDF溶液的组分及其质量比为:丙酮:N,N-二甲基甲酰胺:PVDF=3~10:8~2:0.8~1.5。
2.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(1)中弹性织物为由1~20wt%氨纶+99~80wt%涤纶组成。
3.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(1)氧化石墨烯分散液的浓度为1~60mg/mL。
4.根据权利要求1或3所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述氧化石墨烯分散液的制备方法为:在室温下,将氧化石墨加入去离子水中,超声1~96h,得到氧化石墨烯分散液。
5.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(1)中静置的时间为1~60min。
6.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(2)中还原的时间为1~3h。
7.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(2)中清洗的条件为:乙醇和去离子水分别清洗。
8.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(1)、步骤(2)和步骤(3)中烘干的条件为:40~80℃保温1~5h。
9.根据权利要求1所述的一种自响应PVDF/石墨烯/弹性织物复合传感器的制备方法,其特征在于,所述步骤(3)中浸入的时间为10~120min。
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