CN113463438A - 一种超疏水纸基双功能柔性传感材料及其制备方法和应用 - Google Patents
一种超疏水纸基双功能柔性传感材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种超疏水纸基双功能柔性传感材料及其制备方法和应用,所述方法包括如下步骤:步骤1,将打浆后的纤维、增强剂与石墨烯分散液打浆至抄纸要求,所述纤维、石墨烯分散液中的石墨烯和增强剂的质量比为(60~85):(15~40):(1~10),得到混合浆料;步骤2,将混合浆料制备成石墨烯纸后浸入在造纸施胶剂里,然后干燥,得到超疏水纸基双功能柔性传感材料。本发明以天然高分子纤维素为原料,得到的传感材料价格低廉、可降解、易处理、不会污染环境。
Description
技术领域
本发明涉及传感器制备技术领域,具体为一种超疏水纸基双功能柔性传感材料及其制备方法和应用。
背景技术
柔性传感器能够应用到人体运动检测、人体健康检测、软体机器人、人工智能、可穿戴智能设备、人机界面等领域。因此,柔性传感器受到广泛关注。但是近几年来,随着科技的快速进步以及电子产业的快速发展,产生了大量的电子垃圾,并且这些电子垃圾大多数不可降解,会对环境产生很大的威胁。
为了解决电子垃圾污染环境的问题,研究者使用一些可降解材料,如天然纤维素、淀粉和蛋白质,作为基底去制备柔性传感器。由于纤维素是自然界最丰富的天然高分子,具有价格低廉、可再生、可降解等优点。而纸张最主要的成分是纤维素。因此,以纸作为柔性传感器基材的研究更为广泛。例如:浸涂法(Gao,L.;Zhu,C.;Li,L.;Zhang,C.;Liu,J.;Yu,H.D.;Huang,W.All Paper-Based Flexible and Wearable Piezoresistive PressureSensor.ACS Appl Mater Interfaces 2019,11(28),25034-25042.),激光打印法(Long,Y.;He,P.;Xu,R.;Hayasaka,T.;Shao,Z.;Zhong,J.;Lin,L.Molybdenum-carbide-graphenecomposites for paper-based strain and acoustic pressure sensors.Carbon 2020,157,594-601.)等。
但是,以纸作为柔性传感器的基材在应用时,由于纤维素表面富含大量的羟基,导致其不能在有水存在的环境中进行正常工作,而且纸张的强度有限,进一步限制了其应用。
发明内容
针对现有技术中存在的问题,本发明提供一种超疏水纸基双功能柔性传感材料及其制备方法和应用,得到性能优异、价格低廉、超疏水的纸基双功能柔性传感材料。
本发明是通过以下技术方案来实现:
一种超疏水纸基双功能柔性传感材料的制备方法,包括如下步骤:
步骤1,将打浆后的纤维、增强剂与石墨烯分散液打浆至抄纸要求,所述纤维、石墨烯分散液中的石墨烯和增强剂的质量比为(60~85):(15~40):(1~10),得到混合浆料;
步骤2,将混合浆料制备成石墨烯纸后浸入在造纸施胶剂里,然后干燥,得到超疏水纸基双功能柔性传感材料。
优选的,步骤1先将打浆后的纤维和石墨烯分散液使用标准浆料疏解机打浆至抄纸要求,在此过程中加入增强剂,得到混合浆料。
优选的,步骤1使用天然纤维进行打浆,得到打浆后的纤维,天然纤维采用针叶木纤维、阔叶木纤维和棉浆纤维的一种或多种。
优选的,步骤1所述石墨烯分散液中的石墨烯采用氧化还原法或机械法制备得到。
优选的,步骤1中所述的增强剂为阳离子淀粉、纳米纤维素或纳米纤维素晶。
优选的,步骤2所述的造纸施胶剂为松香胶、烷基烯酮二聚体乳液或烯基琥珀酸酐。
优选的,步骤2将浸入在造纸施胶剂里的石墨烯纸干燥后,再室温放置,得到超疏水纸基双功能柔性传感材料。
进一步,步骤2将浸入在造纸施胶剂里的石墨烯纸干燥后,室温放置24~48h,得到超疏水纸基双功能柔性传感材料。
一种由上述任意一项所述的超疏水纸基双功能柔性传感材料的制备方法得到的超疏水纸基双功能柔性传感材料。
超疏水纸基双功能柔性传感材料在应变传感或压力传感中的应用,其特征在于,当所述传感材料作为应变传感器来使用时,其应变系数GF可达19.54,相应时间为0.3s,并且能在滴水的环境中检测到人体手指的弯曲;
当所述传感材料作为压力传感器来使用时,能检测0~1421kPa范围内的压力,响应时间为0.48s。
与现有技术相比,本发明具有以下有益的技术效果:
本发明一种超疏水纸基双功能柔性传感材料的制备方法,先通过造纸的方法将石墨烯和打浆后纤维结合起来,在这个过程中添加增强剂增强,可以增加纸张的强度,将制备出来的石墨烯纸浸入在造纸施胶剂当中可赋予其疏水性能,同时,以天然高分子纤维素为原料,价格低廉、可降解、易处理、不会污染环境。该柔性传感材料在弯曲的过程中,石墨烯层会受到弯曲挤压的作用而紧密连接在一起,使得柔性传感材料的电阻发生改变,而在按压的过程中,按压区域的石墨烯层与层之间的接触更加紧密,使得柔性传感材料整体的电阻发生变化,同时由于其具有疏水的性能,因此该柔性传感材料也可以在有水存在的环境中进行正常工作。
附图说明
图1为本发明石墨烯纸基柔性传感器传感原理图。
图2为本发明石墨烯纸基柔性传感器结构示意图。
图3为本发明实施例2中石墨烯纸照片。
图4a为本发明实施例2中石墨烯纸在200μm下的扫描电镜图。
图4b为本发明实施例2中石墨烯纸在20μm下的扫描电镜图。
图5为本发明实施例2中石墨烯纸中石墨烯含量与电阻率的关系。
图6为本发明实施例2中应变传感器的应变指数图。
图7为本发明实施例2中应变传感器的传感效果图。
图8为本发明实施例2中应变传感器的响应时间。
图9为本发明实施例2中应变传感器在有水存在的环境中进行工作。
图10为本发明实施例2中压力传感器的灵敏度。
图11为本发明实施例2中压力传感器的传感效果图。
图12为本发明实施例2中压力传感器的响应时间。
具体实施方法
下面结合具体的实施例对本发明做进一步的详细说明,所述是对本发明的解释而不是限定。
本发明一种可以水中工作的超疏水纸基应变压力双功能柔性传感材料的制备方法,包括如个步骤:
步骤1,将打浆后的纤维与石墨烯分散液使用标准浆料疏解机混合,打浆至抄纸要求,在这个过程中加入增强剂,得到混合浆料,通过这种方式提高纸张的强度,天然纤维、石墨烯和增强剂的质量比为(60~85):(15~40):(1~10);
天然纤维采用针叶木纤维、阔叶木纤维和棉浆纤维的一种或多种,石墨烯采用不同方法制备的石墨烯:氧化还原法制备的石墨烯,机械法制备的石墨烯,增强剂为阳离子淀粉、纳米纤维素(简写为CNF)、纳米纤维素晶(简写为CNC);
步骤2,将混合浆料经过现有造纸的过程进行成型、压榨和干燥,制备出石墨烯纸;
步骤3,将石墨烯纸剪成纸条,然后浸入在造纸施胶剂里,造纸施胶剂为松香胶、烷基烯酮二聚体乳液(简写为AKD)、烯基琥珀酸酐(简写为ASA),烘箱干燥后,室温下放置24~48h,从而制备出超疏水石墨烯纸基传感材料,记为复合纸条。
如图2所示,用导电铜胶2将制备出来的复合纸条1和导线3连接起来,即得到应变或压力传感器。即不仅可以作为应变传感器来使用,也可以作为压力传感器来使用。
如图1所示,作为应变传感器的基本原理为:在弯曲的过程中,石墨烯层受到弯曲挤压的作用而紧密连接在一起,使得传感器的电阻发生改变,作为压力传感器的基本原理为:在按压的过程中,按压区域的石墨烯层与层之间的接触更加紧密,使得传感器整体的电阻发生变化。同时,由于其具有疏水的性能,因此也可以在有水存在的环境中进行正常工作。
当作为应变传感器来使用时,应变系数GF可达19.54,响应时间为0.3s,并且可以在滴水的环境中检测手指的弯曲,同时可以在有水存在的环境中正常工作;当作为压力传感器来使用时,可以检测0~1421kPa范围内的压力,响应时间为0.48s。
实施例1
一种可以水中工作的超疏水纸基应变压力双功能柔性传感材料的制备方法,包括如个步骤:
步骤(1):将已打浆的针叶木纤维与已超声分散的机械法制备的石墨烯分散液使用标准浆料疏解机混合。在这个过程中加入阳离子淀粉来提高纸张的强度。纤维、石墨烯和增强剂的质量比为80:20:2。
浆料的打浆度可以为35度。
步骤(2):将混合的浆料经过现有造纸的过程,成型、压榨、干燥的过程制备出石墨烯纸,纸张的定量为80g/m2。
步骤(3):将制备出来的石墨烯纸剪成纸条,然后浸入在AKD乳液里,烘箱干燥后,室温下放置24h,从而制备出疏水的石墨烯纸基传感材料。
步骤(4):用导电铜胶将制备出来的石墨烯纸基传感材料和导线连接起来,即得到应变、压力传感器。
实施例2
一种可以水中工作的超疏水纸基应变压力双功能柔性传感材料的制备方法,包括如个步骤:
步骤(1):将已打浆的针叶木纤维与已超声分散的机械法制备的石墨烯分散液使用标准浆料疏解机混合。在这个过程中加入CNF来提高纸张的强度。纤维、石墨烯和增强剂的质量比为78:22:2。
步骤(2):将混合的浆料经过现有造纸的过程,成型、压榨、干燥的过程制备出石墨烯纸。
步骤(3):将制备出来的石墨烯纸剪成纸条,然后浸入在AKD乳液里,烘箱干燥后,室温下放置24h,从而制备出疏水的石墨烯纸基传感材料。
步骤(4):用导电铜胶将制备出来的石墨烯纸基传感材料和导线连接起来,即得到应变、压力传感器。
从图3石墨烯纸的照片可以看到其颜色为浅黑色,这主要是由于石墨烯本身的颜色引起的。
图4a和图4b体现了石墨烯纸的微观形貌。从图4a中可以看到,纤维与纤维之间交错分布,形成三维网络状结构,石墨烯填充在纤维之间形成的孔隙中。从图4b中可以看到片层状的石墨烯,石墨烯和纤维之间缠结在一起。
在图5当中可以看到,一开始随着石墨烯的添加,石墨烯纸的电阻率的减小是非常快的,当石墨烯的添加量达到25%之后,石墨烯纸的电阻率虽然也在减小,但是减小速率变慢。
从图6相对电阻随着应变的变化曲线可以看出,当其作为应变传感器来使用时,其应变系数可以达到19.54。
将步骤(4)得到的应变传感器贴在手上,手指动,得到如图7所示的传感效果图,图7显示了随着手指的不断弯曲,应变传感器会产生一个同步的电信号,表明其可以用来进行应变传感。
图8为图7局部放大图,表明传感器的响应时间可以达到0.3s。
图9是将传感器贴在手指上,用其检测手指弯曲,然后在传感器表面滴水,同样会产生一个同步的电信号。
从图10相对电阻随着压力的变化曲线可以看出,当其作为压力传感器来使用时,在压力范围为0~316.5kPa时,其灵敏度为0.019kPa-1;在压力范围为316.5~1421kPa时,其灵敏度为0.01kPa-1。
图11为不断地以100kPa压力按压传感器,会产生一个同步的电信号,表明其可以用来进行压力传感。
图12是图11的一个局部放大图,可以看到其响应时间为0.48s。总之,制备出来的传感器不仅可以实现应变传感和压力传感,而且可以在有水存在的环境中进行应变传感。
实施例3
一种可以水中工作的超疏水纸基应变压力双功能柔性传感材料的制备方法,包括如个步骤:
步骤(1):将已打浆的针叶木纤维与已超声分散的机械法制备的石墨烯分散液使用标准浆料疏解机混合。在这个过程中加入CNC来提高纸张的强度。纤维、石墨烯和增强剂的质量比为70:30:2。
步骤(2):将混合的浆料经过现有造纸的过程,成型、压榨、干燥的过程制备出石墨烯纸。
步骤(3):将制备出来的石墨烯纸剪成纸条,然后浸入在AKD乳液里,烘箱干燥后,室温下放置24h,从而制备出疏水的石墨烯纸基传感材料。
步骤(4):用导电铜胶将制备出来的石墨烯纸基传感材料和导线连接起来,即得到应变、压力传感器。
实施例4
一种可以水中工作的超疏水纸基应变压力双功能柔性传感材料的制备方法,包括如个步骤:
步骤(1):将已打浆的针叶木纤维与已超声分散的氧化还原法制备的石墨烯分散液使用标准浆料疏解机混合。在这个过程中加入CNF来提高纸张的强度。纤维、石墨烯和增强剂的质量比为60:40:2。
步骤(2):将混合的浆料经过现有造纸的过程,成型、压榨、干燥的过程制备出石墨烯纸。
步骤(3):将制备出来的石墨烯纸剪成纸条,然后浸涂在在AKD乳液里,烘箱干燥后,室温下放置24h,从而制备出疏水的石墨烯纸基传感材料。
步骤(4):用导电铜胶将制备出来的石墨烯纸基传感材料和导线连接起来,即得到应变、压力传感器。
实施例5
一种可以水中工作的超疏水纸基应变压力双功能柔性传感材料的制备方法,包括如个步骤:
步骤(1):将已打浆的针叶木纤维与已超声分散的氧化还原法制备的石墨烯分散液使用标准浆料疏解机混合。在这个过程中加入CNF来提高纸张的强度。纤维、石墨烯和增强剂的质量比为85:15:2。
步骤(2):将混合的浆料经过现有造纸的过程,成型、压榨、干燥的过程制备出石墨烯纸。
步骤(3):将制备出来的石墨烯纸剪成纸条,然后浸涂在在AKD乳液里,烘箱干燥后,室温下放置24h,从而制备出疏水的石墨烯纸基传感材料。
步骤(4):用导电铜胶将制备出来的石墨烯纸基传感材料和导线连接起来,即得到应变、压力传感器。
Claims (10)
1.一种超疏水纸基双功能柔性传感材料的制备方法,其特征在于,包括如下步骤:
步骤1,将打浆后的纤维、增强剂与石墨烯分散液打浆至抄纸要求,所述纤维、石墨烯分散液中的石墨烯和增强剂的质量比为(60~85):(15~40):(1~10),得到混合浆料;
步骤2,将混合浆料制备成石墨烯纸后浸入在造纸施胶剂里,然后干燥,得到超疏水纸基双功能柔性传感材料。
2.根据权利要求1所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤1先将打浆后的纤维和石墨烯分散液使用标准浆料疏解机打浆至抄纸要求,在此过程中加入增强剂,得到混合浆料。
3.根据权利要求1所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤1使用天然纤维进行打浆,得到打浆后的纤维,天然纤维采用针叶木纤维、阔叶木纤维和棉浆纤维的一种或多种。
4.根据权利要求1所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤1所述石墨烯分散液中的石墨烯采用氧化还原法或机械法制备得到。
5.根据权利要求1所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤1中所述的增强剂为阳离子淀粉、纳米纤维素或纳米纤维素晶。
6.根据权利要求1所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤2所述的造纸施胶剂为松香胶、烷基烯酮二聚体乳液或烯基琥珀酸酐。
7.根据权利要求1所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤2将浸入在造纸施胶剂里的石墨烯纸干燥后,再室温放置,得到超疏水纸基双功能柔性传感材料。
8.根据权利要求7所述的超疏水纸基双功能柔性传感材料的制备方法,其特征在于,步骤2将浸入在造纸施胶剂里的石墨烯纸干燥后,室温放置24~48h,得到超疏水纸基双功能柔性传感材料。
9.一种由权利要求1~8中任意一项所述的超疏水纸基双功能柔性传感材料的制备方法得到的超疏水纸基双功能柔性传感材料。
10.如权利要求9所述的超疏水纸基双功能柔性传感材料在应变传感或压力传感中的应用,其特征在于,当所述传感材料作为应变传感器来使用时,其应变系数GF可达19.54,相应时间为0.3s,并且能在滴水的环境中检测到人体手指的弯曲;
当所述传感材料作为压力传感器来使用时,能检测0~1421kPa范围内的压力,响应时间为0.48s。
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