CN110306354A - 一种高热导率可拉伸应变传感器的制备方法 - Google Patents

一种高热导率可拉伸应变传感器的制备方法 Download PDF

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CN110306354A
CN110306354A CN201910438722.8A CN201910438722A CN110306354A CN 110306354 A CN110306354 A CN 110306354A CN 201910438722 A CN201910438722 A CN 201910438722A CN 110306354 A CN110306354 A CN 110306354A
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蔡铭凯
孙彬
朱宏泽
谭岑孝
郭向欣
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Yantai Qibin New Material Technology Co ltd
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Abstract

本发明属于柔性可穿戴电子技术领域，公开了一种高热导率可拉伸应变传感器的制备方法，包含如下步骤：(1)制备掺杂有导热导电纳米材料和高分子材料的静电纺丝前驱体溶液、制备掺杂有导热绝缘纳米材料和高分子材料的涂膜前驱体溶液；(2)以静电纺丝前驱体溶液进行静电纺丝；(3)以涂膜前驱体溶液在静电纺丝纤维膜的上、下表面各形成一层封装层薄膜，进行封装、压紧，并制备电极，即得到高热导率可拉伸应变传感器。本发明的传感器具有高导热率和稳定性好的特点，克服了现有应变传感器在运行过程中产生的多余热量不易散发出去，从而影响传感器精度、稳定性和使用寿命的缺点。

Description

一种高热导率可拉伸应变传感器的制备方法
技术领域
本发明属于柔性可穿戴电子技术领域，特别涉及一种高热导率的可拉伸应变传感器的制备方法。
背景技术
柔性应变式传感器可以将位移、力、压力、加速度、形变等非电物理量转换为电阻值变化，在冶金、电力、交通、石化、商业、生物医学和国防等行业有着广泛应用。尤其随着科技发展和柔性电子技术的兴起，对于柔性可拉伸功能的应变传感器的需求日渐高涨。柔性可拉伸应变传感器可以承受较大形变，从而使得传感器可以测量的范围得以大大拓宽。目前，对于可拉伸应变传感器的研究主要是集中在两种途径上：一种是研究和探索新的可拉伸材料，例如一维纳米线和二维纳米片；另一种是发展材料的可拉伸结构。
在柔性可拉伸应变传感器的制备过程中，必须将制备的材料或者结构放置到柔性高分子衬底上进行封装。同时，当传感器运行时，纳米材料之间以及纳米材料和高分子衬底之间存在巨大的接触电阻，会使得传感器产生大量的焦耳热；而受到高分子本身较差的导热性影响，这些产生的热量不易被及时散发出去，从而使得传感器的精度和稳定性受到影响，也危及整个电路的安全寿命。所以制备具有高热导率的应变传感器势在必行。而具有封装功能的导热层必须与外界环境相接触才能将热量快速散发出去，因此其绝缘性也至关重要。
发明内容
本发明的目的在于克服现有的应变传感器在运行过程中产生的焦耳热不易散发出去，从而影响传感器精度、稳定性和使用寿命的缺点，提供一种具有高导热率、稳定性好、且制备简单的应变传感器的制备方法。
为解决上述技术问题，本发明的实施方式所提供的高热导率可拉伸应变传感器的制备方法，包含如下步骤：
(1)制备静电纺丝前驱体溶液和涂膜前驱体溶液：将导热导电纳米材料均匀分散到有机溶剂中，再加入高分子材料，搅拌均匀后得到静电纺丝前驱体溶液；将导热绝缘纳米材料均匀分散到有机溶剂中，再加入高分子材料，搅拌均匀后得到涂膜前驱体溶液；
(2)制备静电纺丝纤维膜：以静电纺丝前驱体溶液进行静电纺丝，得到静电纺丝纤维膜，并引出导线；
(3)制备封装层薄膜；以涂膜前驱体溶液在静电纺丝纤维膜的上、下表面各形成一层封装层薄膜，进行封装、压紧，并制备电极，即得到高热导率可拉伸应变传感器。
相对于现有技术而言，本发明的实施方式中，不但在静电纺丝纤维膜中掺杂了具有导热性能的纳米材料；同时也在位于静电纺丝纤维膜上下表面的两个封装层薄膜中掺杂了具有导热性能的纳米材料，因此，封装薄膜层可以与静电纺丝纤维膜之间形成良好的导热通路，从而使得传感器运行过程中产生的热量能够快速散发出去，使传感器保持较高的稳定性，且响应快速、可承受应变范围广。此外，静电纺丝纤维膜以及位于静电纺丝纤维膜上下表面的两个封装层薄膜之间接触紧密所形成的三明治结构，使得传感器的各方面功能得以相互促进，具有多种功能的同时不需要增加额外的部件，节省了器件所占空间。
优选地，所述导热导电纳米材料选自一维纳米材料、二维纳米片、二维纳米带中的至少一种。进一步优选地，所述一维纳米材料选自金属纳米线或碳纳米管，所述金属纳米线例如金纳米线、银纳米线、铜纳米线；所述二维纳米片选自石墨烯纳米片；所述二维纳米带选自石墨烯纳米带。相比零维纳米材料，上述材料更易形成三维导电网络结构，且机械性能也较零维纳米材料更优。
优选地，所述导热绝缘纳米材料选自氮化硼纳米片、氮化铝纳米片、氮化硅纳米片、二硫化钼纳米片和氧化铍纳米片中的至少一种。
优选地，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所加入的高分子材料各自独立地选自热塑性聚氨酯弹性体橡胶(TPU)、苯乙烯类弹性体(例如苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS))、或聚二甲基硅氧烷(PDMS)，上述这些优选的高分子材料具有优异的弹性、疏水性、抗腐蚀性和机械性能。另外，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所加入的高分子材料可以相同，也可以不同。
优选地，所述导热导电纳米材料在所述静电纺丝纤维膜中的质量百分含量为0.5～4％；所述导热绝缘纳米材料在所述封装层薄膜中的质量百分含量为10～40％。
优选地，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所用的有机溶剂各自独立地选自二甲基甲酰胺、四氢呋喃、丙酮、甲醇、乙醇、甲酸、乙酸等中的一种或者多种的混合物。
优选地，所述静电纺丝纤维膜中的纤维形貌为二维无纺布结构、扭曲结构、有序结构和图案化结构中的一种或几种。
优选地，所述封装层薄膜的形成方式为流延成膜或者旋涂成膜。
优选地，所述制备封装层薄膜过程中，抽去静电纺丝纤维膜和封装层薄膜之间的空气，并干燥。制备封装层薄膜的步骤中，所述的压紧采用干压或热压。
附图说明
图1为实施例1制备的静电纺丝纤维膜的扫描电镜图；
图2为实施例1制备的静电纺丝纤维膜的透射电镜图；
图3为实施例1制备的封装层薄膜的断面扫描电镜图；
图4为实施例1制备的柔性可拉伸传感器反复拉伸及响应性能测试图；
图5为实施例2制备的静电纺丝纤维膜的光学照片。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将对本发明的各实施方式进行详细的阐述。然而，本领域的普通技术人员可以理解，在本发明各实施方式中，为了使读者更好地理解本申请而提出了许多技术细节。但是，即使没有这些技术细节和基于以下各实施方式的种种变化和修改，也可以实现本申请各权利要求所要求保护的技术方案。
本发明的具体实施例提供了一种压电传感器的制备方法，包含如下步骤：(1)制备静电纺丝前驱体溶液和涂膜前驱体溶液：将导热导电纳米材料均匀分散到有机溶剂中，再加入高分子材料，搅拌均匀后得到静电纺丝前驱体溶液；将导热绝缘纳米材料均匀分散到有机溶剂中，再加入高分子材料，搅拌均匀后得到涂膜前驱体溶液；(2)制备静电纺丝纤维膜：以静电纺丝前驱体溶液进行静电纺丝，得到掺杂有导热导电纳米材料的静电纺丝纤维膜，并引出导线；(3)制备封装层薄膜；以涂膜前驱体溶液在静电纺丝纤维膜的上、下表面各形成一层掺杂有导热绝缘纳米材料的封装层薄膜，进行封装、压紧，并制备电极，即得到高热导率可拉伸应变传感器。
在本发明的一些具体实施方式中，所述导热导电纳米材料选自一维纳米材料、二维纳米片、二维纳米带中的至少一种。
在本发明的一些具体实施方式中，所述一维纳米材料选自金属纳米线或碳纳米管；所述二维纳米片选自石墨烯纳米片；所述二维纳米带选自石墨烯纳米带。在本发明的一些具体实施方式中，所述一维纳米材料选自金属纳米线或碳纳米管，所述金属纳米线例如金纳米线、银纳米线、铜纳米线；所述二维纳米片选自石墨烯纳米片；所述二维纳米带选自石墨烯纳米带。
在本发明的一些具体实施方式中，所述导热绝缘纳米材料选自氮化硼、氮化铝、氮化硅、二硫化钼中的至少一种。
在本发明的一些具体实施方式中，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所加入的高分子材料各自独立地选自热塑性聚氨酯弹性体橡胶(TPU)、苯乙烯类弹性体(例如苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS))、或聚二甲基硅氧烷(PDMS)，上述这些优选的高分子材料具有优异的弹性、疏水性、抗腐蚀性和机械性能。另外，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所加入的高分子材料可以相同，也可以不同。
在本发明的一些具体实施方式中，所述导热导电纳米材料在所述静电纺丝纤维膜中的质量百分含量为0.5～4％；所述导热绝缘纳米材料在所述封装层薄膜中的质量百分含量为10～40％。
在本发明的一些具体实施方式中，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所用的有机溶剂各自独立地选自二甲基甲酰胺、四氢呋喃、丙酮、甲醇、乙醇、甲酸、乙酸等中的一中或者多种的混合物。
在本发明的一些具体实施方式中，静电纺丝纤维膜中的纤维形貌为二维无纺布结构、扭曲结构、有序结构和图案化结构中的一种或几种。
在本发明的一些具体实施方式中，封装层薄膜的形成方式为流延成膜或者旋涂成膜。
在本发明的一些具体实施方式中，在所述制备封装层薄膜过程中还包括如下步骤：抽去静电纺丝纤维膜和封装层薄膜之间的空气，并干燥。
在本发明的一些具体实施方式中，在制备封装层薄膜的步骤中，所述的压紧采用干压或热压。
以下为本发明的具体实施方式的举例，其中的原料均为已知化合物，可以由商业途径获得，或可按本领域已知方法制备。
实施例1
本实施例涉及一种以热塑性聚氨酯弹性体橡胶(TPU)和碳纳米管制备静电纺丝纤维膜，以热塑性聚氨酯弹性体橡胶(TPU)和氮化硼纳米片制备封装层薄膜的可拉伸应变传感器的制备方法，具体包括如下步骤：
第一步：制备静电纺丝前驱体溶液和涂膜前驱体溶液
将碳纳米管(CNTs)加入到二甲基甲酰胺(DMF)和四氢呋喃(THF)混合溶剂中，超声振荡之后搅拌10小时，使得碳纳米管均匀分散在混合溶剂中。然后将TPU颗粒加入到上述溶液中，磁力搅拌5小时，得到静电纺丝前驱体溶液A。
将剥离好的单层氮化硼纳米片加入到DMF和THF混合溶剂中，超声振荡之后搅拌10小时，使得氮化硼纳米片均匀分散在混合溶剂中。然后将TPU颗粒加入到上述溶液中，磁力搅拌5小时，得到涂膜前驱体溶液B。
第二步：制备TPU/碳纳米管静电纺丝纤维膜
将上述静电纺丝前驱体溶液A吸入到5毫升针管中，进行静电纺丝，调节纺丝条件(例如电压10kV、纺丝距离12cm等)收集到携带碳纳米管的纤维膜。本实施例中碳纳米管在静电纺丝纤维膜中的质量百分含量为2.5％之间。
图1和图2分别是掺杂碳纳米管的二维无纺布结构静电纺丝纤维膜的扫描电镜(SEM)和透射电镜(TEM)图，可以看出电纺纤维形貌均匀，并且碳纳米管均沿着纤维的轴向排列。
第三步：制备高介电封装层薄膜
将制备好的涂膜前驱体溶液B流延成膜或者旋涂成膜；将静电纺丝纤维膜从收集极上揭下后覆于前驱体溶液B所形成的流延膜或旋涂膜上，真空干燥10小时，抽去静电纺丝纤维膜以及前驱体溶液B所形成的流延膜或旋涂膜之间的空气，并使之充分干燥；在静电纺丝纤维膜相对两端制备电极，再在静电纺丝纤维膜的没有前驱体溶液B所形成流延膜或旋涂膜的表面上，再形成一层前驱体溶液B的流延膜或旋涂膜，从而形成中间层为静电纺丝纤维膜、上下层分别为流延膜或旋涂膜(即封装层薄膜)的三明治结构，然后将其置于真空干燥箱中，真空干燥10小时。本实施例中氮化硼纳米片在封装层薄膜中的质量百分含量为35％。
图3为封装层薄膜的断面扫描电镜图。从图3中可见，氮化硼纳米片相互接触，形成有效的导热通路。
第四步：干压、热压。
利用干压、热压等方法将制备好的样品压紧，使得各层物质间接触紧密。
第五步：性能测试。
将制备好的柔性可拉伸应变传感器进行热学、电学等测试。
结果表明，本实施例中制备的样品可以在拉伸应变达到160％时，仍保持稳定的电学性能。同时，本发明方法制备的可拉伸应变传感器稳定性和灵敏度极好。图4为传感器在可拉伸应变范围内反复拉伸的性能测试图(保持变压为5伏)，可以看出，随着封装层薄膜及静电纺丝纤维膜的拉伸，其电流迅速变化。
此外，本实施例所制备的柔性可拉伸应变传感器的导热系数为1.192W/m·K，远高于基于纯TPU封装层的传感器的导热系数0.42W/m·K，因此，本发明提出的可拉伸应变传感器导热性能得到极大提高。
实施例2
本实施例中，将实施例1中的碳纳米管替换为石墨烯纳米片，静电纺丝纤维膜中的纤维形貌改有序排列扭曲结构的纤维阵列；此外，使石墨烯纳米片在静电纺丝纤维膜中的质量百分含量为3％；使氮化硼纳米片在封装层薄膜中的质量百分含量为35％，其他条件与实施例1类似，制备柔性可拉伸应变传感器。
图5为本实施例制备的掺杂石墨烯纳米片的有序排列扭曲结构静电纺丝纤维膜的光学照片。
测试结果表明，本实施例所制备的柔性可拉伸应变传感器可以在拉伸应变达到150％时，仍保持稳定的电学性能；柔性可拉伸应变传感器的导热系数为1.43W/m·K，导热性得到大大增强。
实施例3
本实施例中，将实施例1中的碳纳米管替换为银纳米线，将氮化硼纳米片替换成氮化硅纳米片，将封装层薄膜材料换成聚二甲基硅氧烷。此外，使银纳米线在静电纺丝纤维膜中的质量百分含量为2.5％，使氮化硅纳米片在封装层薄膜中的质量百分含量为30％，其他条件与实施例1类似，制备柔性可拉伸应变传感器。
测试结果表明，本实施例制备的柔性可拉伸应变传感器可以在拉伸应变达到120％时，仍保持稳定的电学性能。柔性可拉伸应变传感器的导热系数为1.01W/m·K，导热性得到大大增强。
本领域的普通技术人员可以理解，上述各实施方式是实现本发明的具体实施例，而在实际应用中，可以在形式上和细节上对其作各种改变，而不偏离本发明的精神和范围。

Claims (10)

1.一种高热导率可拉伸应变传感器的制备方法，其特征在于，包含如下步骤：
(1)制备静电纺丝前驱体溶液和涂膜前驱体溶液：
将导热导电纳米材料均匀分散到有机溶剂中，再加入高分子材料，搅拌均匀后得到静电纺丝前驱体溶液；
将导热绝缘纳米材料均匀分散到有机溶剂中，再加入高分子材料，搅拌均匀后得到涂膜前驱体溶液；
(2)制备静电纺丝纤维膜：
以所述静电纺丝前驱体溶液进行静电纺丝，得到静电纺丝纤维膜，并引出导线；
(3)制备封装层薄膜；
以所述涂膜前驱体溶液在所述静电纺丝纤维膜的上、下表面各形成一层封装层薄膜，封装、压紧，并制备电极，即得到高热导率可拉伸应变传感器。
2.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述导热导电纳米材料选自一维纳米材料、二维纳米片、二维纳米带中的至少一种。
3.根据权利要求2所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述一维纳米材料选自金属纳米线或碳纳米管；所述二维纳米片选自石墨烯纳米片；所述二维纳米带选自石墨烯纳米带。
4.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述导热绝缘纳米材料选自氮化硼纳米片、氮化铝纳米片、氮化硅纳米片、二硫化钼纳米片和氧化铍纳米片中的至少一种。
5.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所加入的高分子材料各自独立地选自热塑性聚氨酯弹性体橡胶、苯乙烯类弹性体或聚二甲基硅氧烷。
6.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述导热导电纳米材料在所述静电纺丝纤维膜中的质量百分含量为0.5～4％；所述导热绝缘纳米材料在所述封装层薄膜中的质量百分含量为10～40％。
7.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，制备所述静电纺丝前驱体溶液和所述涂膜前驱体溶液时所用的有机溶剂各自独立地选自二甲基甲酰胺、四氢呋喃、丙酮、甲醇、乙醇、甲酸、乙酸等中的一中或者多种的混合物。
8.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述静电纺丝纤维膜中的纤维形貌为二维无纺布结构、扭曲结构、有序结构和图案化结构中的一种或几种。
9.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述封装层薄膜的形成方式为流延成膜或者旋涂成膜。
10.根据权利要求1所述的高热导率可拉伸应变传感器的制备方法，其特征在于，所述制备封装层薄膜的过程中，抽去静电纺丝纤维膜和封装层薄膜之间的空气，并干燥。
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CN115450054A (zh) * 2022-09-19 2022-12-09 陕西科技大学 一种超疏水柔性导热薄膜及其制备方法
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