CN111043950A - 一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器及其制备方法 - Google Patents

一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器及其制备方法 Download PDF

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CN111043950A
CN111043950A CN201911331884.8A CN201911331884A CN111043950A CN 111043950 A CN111043950 A CN 111043950A CN 201911331884 A CN201911331884 A CN 201911331884A CN 111043950 A CN111043950 A CN 111043950A
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mxenes
polymer
fiber composite
conductive fiber
strain sensor
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贾志欣
李彰杰
张文强
陈勇军
贾德民
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South China University of Technology SCUT
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Abstract

本发明公开了一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器及其制备方法。本发明采用静电纺丝法制备高分子纤维膜，再将得到的高分子纤维膜浸入过渡金属碳化物MXenes的分散液中超声，取出、干燥，得到MXenes/高分子导电纤维复合膜。在MXenes/高分子导电纤维复合膜的两端接上导线固定单元和导线，即得到基于MXenes/高分子导电纤维复合膜的柔性应变传感器。本发明的柔性应变传感器具有原料成本低、产品性能优良、工艺操作简单、应变测试范围广和灵敏度高等优点，在柔性可穿戴设备、仿人体电子皮肤、智能机器人、物联网以及健康监测等领域具有重要的运用前景。

Description

一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器 及其制备方法
技术领域
本发明涉及到应变传感器领域，具体涉及一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器及其制备方法。
背景技术
近年来，柔性应变传感器因其在电子皮肤，机器人技术和运动检测等领域的巨大潜力而备受关注。传统的基于金属或半导体材料的应变传感器因应变范围窄(通常低于5％)且刚度较大而无法满足智能可穿戴式设备的要求。因此，亟待开发具有优异的灵敏度和高拉伸性的柔性应变传感器，以满足日益增长的需求。
目前，柔性应变传感器的主流方式是在拉伸过程中把传感器的形变转化为电阻值的变化。普遍的做法是将导电纳米材料(例如炭黑，石墨烯，碳纳米管等)引入作为柔性可拉伸基底的弹性聚合物中作为传感活性材料。通过该方法，目前已实现了相比于传统传感器具有更可控的感测范围的柔性传感器。然而，目前常采用的导电纳米材料(如炭黑，石墨烯，碳纳米管等)与弹性聚合物基底的相互作用通常较弱，为了实现低电阻高灵敏度的柔性传感器，往往需要加大导电纳米材料的用量，这又带来了成本上问题。如何在减少昂贵的导电纳米材料的用量的同时，制备具备较大感测范围和较高灵敏度的柔性传感器仍然是一大挑战。
MXenes是一种二维层状过渡金属碳化物，其化学式为Mn+1Xn，n＝1、2、3(M为早期过渡金属元素，X为碳元素或氮元素)。MXenes可以通过对从MAX相(这里的M、X、n与上述一样，A为III A族元素或IV A族元素)中选择性刻蚀掉A层得到。MXenes在拥有可与石墨烯媲美的电导率的同时，又拥有亲水的表面，使其在应变传感领域表现出极大的应用前景。
发明内容
本发明的目的是针对目前柔性传感器的制备工艺复杂，成本高，导电纳米材料与柔性基材相互作用力弱的等问题，提供一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器及其制备方法。
本发明的目的通过以下技术方案实现。
一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器的制备方法，包括以下步骤：
(1)将高分子材料溶于溶剂中，得到高分子纺丝液；
(2)将步骤(1)得到的高分子纺丝液进行静电纺丝，得到高分子纤维膜；
(3)将步骤(2)得到的高分子纤维膜剪成所需大小，浸入步骤(1)MXenes纳米片层分散液中超声，取出、干燥，得到MXenes/高分子导电纤维复合膜；
(4)将步骤(3)得到的MXenes/高分子导电纤维复合膜的两端接上导线固定单元和导线，即得到基于MXenes/高分子导电纤维复合膜的柔性应变传感器。
优选的，步骤(1)所述高分子材料为聚酯、聚酰胺、聚乙烯醇、聚丙烯腈、聚丙烯、聚氯乙烯、或聚氨酯中的至少一种；进一步优选为热塑性聚氨酯和聚丙烯腈中的至少一种。
优选的，步骤(1)所述溶剂为丙酮、N，N-二甲基甲酰胺、N-甲基吡咯烷酮和四氢呋喃中的至少一种；进一步优选为N，N-二甲基甲酰胺。
优选的，步骤(1)所述高分子溶剂中溶质的质量分数为10-15wt％。
优选的，步骤(2)所述静电纺丝的工艺条件如下：温度为室温，湿度为50％-70％，电压为20-30kV，注射器针头与接收板之间的距离为10-15cm，接收板为铝箔或锡箔中的一种，进样速度为0.5-2ml/h，纺丝时间为6-8h。
优选的，步骤(2)所述高分子纤维膜具有网络结构；所述高分子纤维膜的厚度为100-300μm。
优选的，步骤(2)所述高分子纤维膜的单根纤维直径为100-2000nm。
优选的，步骤(3)所述MXenes纳米片层为Ti3C2，Ti2C，Ti4C3，V3C2，V2C中的一种或几种，进一步优选为Ti3C2。
优选的，步骤(3)所述MXenes纳米片层分散液的液相为去离子水、乙醇、N，N-二甲基甲酰胺和四氢呋喃中的至少一种；优选为去离子水。
优选的，步骤(3)所述MXenes纳米片层分散液的浓度为0.5-3mg/mL。
优选的，步骤(3)所述超声的时间为30-120分钟；所述超声温度控制在10-40℃。
优选的，步骤(3)所述干燥为真空干燥；所述干燥的时间为30-120min；所述干燥的温度为40-70℃。
优选的，步骤(4)所述导线固定单元为银胶、双组份环氧胶或无机材料导电胶中的至少一种，进一步优选为银胶；所述导线与测量仪器相连，导线通过导线固定单元固定于导电层上。
由以上任一项所述方法制得的基于MXenes/高分子导电纤维复合膜的柔性应变传感器，该柔性应变传感器的拉伸度70％以上，灵敏度达到25.52。
与现有技术相比，本发明具有如下优点：
1、感测范围广：本发明的柔性应变传感器可以检测并分辨0.1％-70％的应变。
2、响应时间短：本发明的柔性应变传感器对0.1％的瞬阶应变的响应时间低至140.6ms。
3、多功能：本发明的柔性应变传感器可应用于人体关节运动，脉搏震动，声带震动等多种活动的检测。
4、导电纳米材料与柔性基底间的作用力强：利用MXene纳米片层表面的活性基团与所使用的高分子分子链上官能团形成的氢键，有效提高了MXene纳米片层与柔性基底的相互作用力，显著降低了MXenes/高分子导电纤维复合膜的表面电阻。
5、节省原料，节约成本：本发明采用浸涂法制备柔性应变传感器，浸涂液可多次反复使用，而导电纳米材料一般价格昂贵，这一优点显著降低了制备柔性应变传感器的成本。
附图说明
图1是本发明基于MXenes/高分子导电纤维复合膜的柔性应变传感器的制备流程示意图。
图2是实施例1中制备的MXenes/高分子导电纤维复合膜表面的扫描电子显微镜图像。
图3是实施例1中制备的柔性应变传感器在1％、2％、3％、4％以及5％拉伸应变下各3个循环的时间-相对电阻曲线图。
图4是实施例1中制备的柔性应变传感器在50％、60％、70％拉伸应变下的各3个循环的时间-相对电阻曲线图。
图5是实施例2中制备的MXenes/高分子导电纤维复合膜表面的扫描电子显微镜图。
图6是实施例2所得应变传感器在1％、2％、3％、4％以及5％拉伸应变下各3个循环的时间-相对电阻曲线图。
图7是实施例2所得应变传感器在60％、70％、80％拉伸应变下的各3个循环的时间-相对电阻曲线图。
图8是实施例3中制备的MXenes/高分子导电纤维复合膜表面的扫描电子显微镜图像。
图9是实施例3所得应变传感器在1％、2％、3％、4％以及5％拉伸应变下各3个循环的时间-相对电阻曲线图。
图10是实施例3所得应变传感器在50％、60％、70％拉伸应变下的各3个循环的时间-相对电阻曲线图。
图11是MXenes纳米片层分散液经过反复多次使用，使用1次后到使用7次后所得MXenes/高分子导电纤维复合膜的表面电阻
具体实施方式
以下结合实例及附图对本发明的具体实施作进一步的说明，但本发明的实施方式不限于此。
实施例1
(1)制备高分子纺丝液：将2.40g TPU和0.13g加入到15ml的N，N-二甲基甲酰胺中，常温下磁力搅拌直至充分溶解，即得均匀的高分子纺丝液。
(2)制备高分子纤维膜：对步骤(1)制备的高分子纺丝液进行静电纺丝，静电纺丝参数如下：温度为室温，湿度为60％，电压为25kV，注射器针头与接收板之间的距离为10cm，接收板为铝箔，进样速度为1ml/h，纺丝时间为8h。最后得到单根纤维直径为300nm，厚度为200μm的高分子纤维膜。
(3)制备MXenes/高分子导电纤维复合膜：将0.5g Ti3C2纳米片层加入到50g去离子水中，超声处理30min，即得质量分数为1wt％的MXenes纳米片层分散液；将步骤(2)所得高分子纤维膜置入上述MXenes纳米片层分散液中超声处理60min，取出，在50℃下真空干燥90min，即得MXenes/高分子导电纤维复合膜。
(4)制备基于MXenes/高分子导电纤维复合膜的柔性应变传感器：通过银胶将导线固定在步骤(3)得到的MXenes/高分子导电纤维复合膜的两端，即得基于MXenes/高分子导电纤维复合膜的柔性应变传感器。
实施例2
(1)制备高分子纺丝液：将2.3g TPU和0.23g PAN加入到15ml的N，N-二甲基甲酰胺中，常温下磁力搅拌直至充分溶解，即得均匀的高分子纺丝液。
(2)制备高分子纤维膜：对步骤(1)制备的高分子纺丝液进行静电纺丝，静电纺丝参数如下：温度为室温，湿度为60％，电压为25kV，注射器针头与接收板之间的距离为10cm，接收板为铝箔，进样速度为1ml/h，纺丝时间为8h。
(3)制备MXenes/高分子导电纤维复合膜：将0.5g Ti3C2纳米片层加入到50g去离子水中，超声处理30min，即得质量分数为1wt％的MXenes纳米片层分散液；将步骤(2)所得高分子纤维膜置入上述MXenes纳米片层分散液中超声处理60min，取出，在50℃下真空干燥90min，即得MXenes/高分子导电纤维复合膜。
(4)制备基于MXenes/高分子导电纤维复合膜的柔性应变传感器：通过银胶将导线固定在步骤(3)得到的MXenes/高分子导电纤维复合膜的两端，即得基于MXenes/高分子导电纤维复合膜的柔性应变传感器。
实施例3
(1)制备高分子纺丝液：将2.02g TPU和0.51g PAN加入到15ml的N，N-二甲基甲酰胺中，常温下磁力搅拌直至充分溶解，即得均匀的高分子纺丝液。
(2)制备高分子纤维膜：对步骤(1)制备的高分子纺丝液进行静电纺丝，静电纺丝参数如下：温度为室温，湿度为60％，电压为25kV，注射器针头与接收板之间的距离为12cm，接收板为铝箔，进样速度为1ml/h，纺丝时间为8h。
(3)制备MXenes/高分子导电纤维复合膜：将0.5g Ti3C2纳米片层加入到50g去离子水中，超声处理30min，即得质量分数为1wt％的MXenes纳米片层分散液；将步骤(2)所得高分子纤维膜置入上述MXenes纳米片层分散液中超声处理60min，取出，在50℃下真空干燥90min，即得MXenes/高分子导电纤维复合膜。
(4)制备基于MXenes/高分子导电纤维复合膜的柔性应变传感器：通过银胶将导线固定在步骤(3)得到的MXenes/高分子导电纤维复合膜的两端，即得基于MXenes/高分子导电纤维复合膜的柔性应变传感器。
图1为本发明基于MXenes/高分子导电纤维复合膜的柔性应变传感器的制备流程示意图。由图1可知，该传感器制备方法简单，生产成本低，便于大规模生产。
图2为实施例1中制备的MXenes/高分子导电纤维复合膜表面的扫描电子显微镜图像。由图2可知，MXenes纳米片层与高分子纤维结合良好，MXenes纳米片层很好地附着在高分子纤维上。
图3为实施例1所得应变传感器在1％、2％、3％、4％以及5％拉伸应变下各3个循环的时间-相对电阻曲线图。结果表明应变传感器可以检测区分非常小的拉伸应变。
图4为实施例1所得应变传感器在50％、60％、70％拉伸应变下的各3个循环的时间-相对电阻曲线图。这表明本发明制备的应变传感器可以在很大的应变范围内工作。
图5为实施例2中制备的MXenes/高分子导电纤维复合膜表面的扫描电子显微镜图像。由图5可见，MXenes纳米片层像丝绸一样将高分子纤维包裹起来，这说明MXenes纳米片层与高分子纤维之间有较强的相互作用力。
图6为实施例2所得应变传感器在1％、2％、3％、4％以及5％拉伸应变下各3个循环的时间-相对电阻曲线图。结果同样表明应变传感器可以检测区分非常小的拉伸应变。
图7为实施例2所得应变传感器在60％、70％、80％拉伸应变下的各3个循环的时间-相对电阻曲线图。这表明本发明制备的应变传感器的感测范围可以达到80％。
图8为实施例3中制备的MXenes/高分子导电纤维复合膜表面的扫描电子显微镜图像。
图9为实施例3所得应变传感器在1％、2％、3％、4％以及5％拉伸应变下各3个循环的时间-相对电阻曲线图。结果同样表明应变传感器可以检测区分非常小的拉伸应变。
图10为实施例3所得应变传感器在50％、60％、70％拉伸应变下的各3个循环的时间-相对电阻曲线图。结果同样表明本发明制备的应变传感器可以在很大的应变范围内工作。
图11为实施例2所得MXenes纳米片层分散液经过反复多次使用，使用1次后到使用7次后所得MXenes/高分子导电纤维复合膜的表面电阻；由图8可知，第7次使用MXenes纳米片层分散液进行浸涂处理所得的MXenes/高分子导电纤维复合膜的表面电阻与第1次使用其进行浸涂处理导电纤维复合膜的表面电阻仍在一个数量级，且仍未超过200Ω/sqr。这也是MXenes纳米片层与实施例1所得高分子纤维膜相互作用力较强带来的益处。基于此，本发明极大地节省了昂贵的导电纳米材料的用量，进而节省了成本。
表1
应变 1％ 2％ 3％ 4％ 5％ 50％ 60％ 70％
灵敏度系数 25.52 13.94 12.42 13.22 14.74 8.16 8.27 8.41
表1为实施例1所得应变传感器在不同拉伸应变下的灵敏度系数(GF，Gaugefactor)，可以看到本发明制备的应变传感器在小应变和大应变下都具有较高的灵敏度。
表2
应变 1％ 2％ 3％ 4％ 5％ 60％ 70％ 80％
灵敏度系数 7.01 6.33 5.59 4.91 4.50 4.89 8.37 9.69
表2为实施例2所得应变传感器在不同拉伸应变下的灵敏度系数。可以看到本发明制备的应变传感器在小应变和大应变下都具有较高的灵敏度。
表3
应变 1％ 2％ 3％ 4％ 5％ 50％ 60％ 70％
灵敏度系数 5.69 3.16 2.91 2.74 2.84 1.82 1.79 6.81
表3为实施例3所得应变传感器在不同拉伸应变下的灵敏度系数。可以看到本发明制备的应变传感器在小应变和大应变下都具有较高的灵敏度。
综上所述,本发明所制备基于MXenes/高分子导电纤维复合膜的柔性应变传感器解决了现有方案中，导电纳米材料与柔性基底间相互作用力较弱的问题，通过调整高分子纤维膜的成分，有效提高了MXenes纳米片层与高分子纤维膜的相互作用力，提高了价格昂贵的导电纳米材料的利用率。由于其感测范围广、响应时间短、多功能同时又节省原料，节约成本，因此所展示的柔性应变传感器在电子皮肤、生物医学监测和运动检测方面具有巨大的潜力。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种基于MXenes/高分子导电纤维复合膜的柔性应变传感器的制备方法，其特征在于，包括以下步骤：
(1)将高分子材料溶于溶剂中，得到高分子纺丝液；
(2)将步骤(1)得到的高分子纺丝液进行静电纺丝，得到高分子纤维膜；
(3)将步骤(2)得到的高分子纤维膜浸入MXenes纳米片层分散液中超声，取出、干燥，得到MXenes/高分子导电纤维复合膜；
(4)将步骤(3)得到的MXenes/高分子导电纤维复合膜的两端接上导线固定单元和导线，即得到基于MXenes/高分子导电纤维复合膜的柔性应变传感器。
2.根据权利要求1所述的制备方法，其特征在于，步骤(1)所述高分子材料为聚酯、聚酰胺、聚乙烯醇、聚丙烯腈、聚丙烯、聚氯乙烯和聚氨酯中的至少一种；所述溶剂为丙酮、N，N-二甲基甲酰胺、N-甲基吡咯烷酮和四氢呋喃中的至少一种。
3.根据权利要求1所述的制备方法，其特征在于，步骤(2)所述静电纺丝的工艺条件包括：温度为室温、湿度为50％-70％、电压为20-30kV、注射器针头与接收板之间的距离为10-15cm、接收板为铝箔或锡箔中的一种；所述纺丝的时间为6-8h。
4.根据权利要求1所述的制备方法，其特征在于，步骤(2)所述高分子纤维膜具有网络结构；所述高分子纤维膜的厚度为100-300μm；所述高分子纤维膜的单根纤维直径为100-2000nm。
5.根据权利要求1所述的制备方法，其特征在于，步骤(3)所述的MXenes的化学式为Mn+ 1Xn，其中，n＝1、2、3，M为早期过渡金属元素，X为碳和氮元素中的一种或两种；所述MXenes为Ti3C2，Ti2C，Ti4C3，V3C2和V2C中的一种或几种。
6.根据权利要求1所述的制备方法，其特征在于：步骤(3)所述MXenes纳米片层分散液的液相为去离子水、乙醇、N，N-二甲基甲酰胺和四氢呋喃中的至少一种；所述分散液的浓度为0.5-3mg/mL。
7.根据权利要求1所述的制备方法，其特征在于：步骤(3)所述超声的时间为30-120分钟；所述超声温度控制在10℃-40℃。
8.根据权利要求1所述的制备方法，其特征在于：步骤(3)所述干燥为真空干燥；所述干燥的时间为30-120min；所述干燥的温度为40-70℃。
9.根据权利要求1所述的制备方法，其特征在于：步骤(4)所述导线固定单元为银胶、双组份环氧胶和无机材料导电胶中的至少一种；所述导线与测量仪器相连，导线通过导线固定单元固定于导电层上。
10.由权利要求1-9任一项所述方法制得的基于MXenes/高分子导电纤维复合膜的柔性应变传感器。
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CN113733697A (zh) * 2021-08-11 2021-12-03 哈尔滨理工大学 一种高灵敏度宽传感范围的柔性复合薄膜及其应用
CN113758986A (zh) * 2021-09-14 2021-12-07 湖北大学 基于Ti3C2-MXene沟道的电化学晶体管传感器及制备方法、检测亚硝酸盐的方法
CN114001637A (zh) * 2021-10-29 2022-02-01 上海应用技术大学 双模芯鞘结构弹性应力发光导电应变传感器的制备方法
CN114993527A (zh) * 2022-05-31 2022-09-02 电子科技大学 基于碳化静电纺丝纤维的柔性电阻式压力传感器及制备
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CN113733697B (zh) * 2021-08-11 2023-05-19 哈尔滨理工大学 一种高灵敏度宽传感范围的柔性复合薄膜及其应用
CN113733697A (zh) * 2021-08-11 2021-12-03 哈尔滨理工大学 一种高灵敏度宽传感范围的柔性复合薄膜及其应用
CN113758986A (zh) * 2021-09-14 2021-12-07 湖北大学 基于Ti3C2-MXene沟道的电化学晶体管传感器及制备方法、检测亚硝酸盐的方法
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