CN114396868A - 一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料及其制备方法 - Google Patents
一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种a‑MWCNTs/MgAl‑LDH/皮革柔性可穿戴应变传感材料及其制备方法,主要技术特点为利用具有特殊微观结构的皮革材料为柔性基底,首次通过一维和二维纳米材料的协同作用在皮革的纤维表面构建高效的电子传输通道,使该传感器具有优于同类产品的高灵敏度。所述的皮革基柔性可穿戴传感材料具有可呼吸、可降解、应变范围宽、响应时间短等技术特点。与采用PDMS、PET等作为柔性基底的传统柔性传感材料相比,本发明在保证材料力学性能的前提下还具有很好的透水透气性,大大提升了穿戴舒适感。
Description
技术领域
本发明属于可穿戴传感器领域,涉及一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料及其制备方法。
背景技术
近年来,柔性可穿戴电子器件由于具有舒适、可穿戴、可远程操作和及时反馈等优点,在医疗设备领域得到了快速发展。它是一类能够对外部信号作出相应反应的智能设备。传感器作为柔性可穿戴电子器件的主要部件,能够将各种生理信号转换成可视化的电信号,比如人体关节弯曲等运动幅度大的信号和血压、心跳等运动幅度小的信号。一般来说,传统的电子传感器大多基于金属或半导体材料,其灵敏度和可拉伸性受到很大限制,不适合监测生理信号。与传统的电子传感器相比,柔性传感器克服了以上缺点,大多表现出良好的生物相容性、可拉伸性、实时监控等优点。应变传感器由于其结构简单,在各种柔性电子传感器中应用最广泛。到目前为止,柔性应变传感器的制备及应用己经取得了显著进展,但如何快速制备出兼具高灵敏度和宽检测范围的高性能柔性应变传感器仍然是一项挑战。
此外,传统的柔性应变传感器所用基底材料为高分子膜。虽然其具有生物相容性,但由于其较差的透水透气性,使得人体皮肤分泌的汗液很难挥发到空气中,不适合长时间佩戴。而且高分子膜很难降解,对环境造成了压力。因此,开发一种具有良好透气性和可降解的柔性基底并通过简单的制备工艺以获得兼具高灵敏度和宽检测范围的高性能可穿戴应变传感器具有重要科学意义。
发明内容
本发明提供了一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料及其制备方法。
为达到上述目的,本发明的技术方案如下:
一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,采用酸化后的多壁碳纳米管a-MWCNTs作为一维导电纳米材料,与二维材料MgAl-LDH物理共混,制备a-MWCNTs/MgAl-LDH复合材料;通过抽滤的工艺将a-MWCNTs/MgAl-LDH复合材料负载在皮革的纤维表面用于构建传感器所必需的电子传输通道,然后在a-MWCNTs/MgAl-LDH复合材料包覆的皮革表面连接电极,制备得到柔性可穿戴应变传感材料。
所述皮革为绵羊坯革,厚度为0.5-0.8 mm。
所述a-MWCNTs在复合材料中的质量浓度为0.5-2 g/L。
所述MgAl-LDH的横向尺寸为2-3 um。
具体步骤为:
步骤一、分别制备a-MWCNTs和MgAl-LDH:
将MWCNTs加入烧瓶中,倒入浓硫酸后机械搅拌,缓慢滴加浓硝酸,滴加完成后在50℃下回流2h,得到分散液,将分散液用去离子水水洗至滤液PH=7,所得滤饼在60 ℃下真空干燥,即得a-MWCNTs;
将硝酸镁、硝酸铝、尿素溶解在去离子水中,搅拌、超声,在110 ℃下加热24 h,冷却后离心、水洗,真空干燥,获得MgAl-LDH;
步骤二、制备a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料:
分别取a-MWCNTs和MgAl-LDH分散在一定体积的去离子水中,超声处理,获得a-MWCNTs/MgAl-LDH水分散液;
将a-MWCNTs/MgAl-LDH水分散液抽滤到绵羊坯革上(D=100 mm),60 ℃下干燥后即得a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
步骤一中,所述MWCNTs在浓硫酸和浓硝酸混合溶液中的质量浓度为8-12 g/L;所述浓硫酸和浓硝酸的体积比为3:1。
步骤一中,所述硝酸镁与硝酸铝的摩尔比为2:1;所述尿素的浓度为0.3-1.0 mol/L。
步骤二中,所述MgAl-LDH的加入量为a-MWCNTs的8 wt%-24 wt%。
如上述制备方法制得的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
与现有技术相比,本发明具有以下有益的技术效果:
本发明将具有优异电学性能和力学性能的a-MWCNTs和具有阻燃性能的MgAl-LDH同时引入到透气性良好的皮革基底中,获得了一种在宽应变范围下具有高灵敏度(GF=7238.92)和宽检测范围(0%-60%)、可应用于人体运动监测的多功能新型皮革基传感材料。该传感材料具有可呼吸、可降解、响应时间短(小于300 ms)、稳定性与重复性好等技术特点。与PDMS、PET等作为柔性基底的传统柔性传感材料相比,本发明在保证材料力学性能的前提下还具有很好的透水透气性,提升了穿戴舒适感。
附图说明
图1为实施例3的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的相对电阻变化-应变曲线图。
图2为实施例3的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的响应时间图。
图3为实施例3的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料分别在循环拉伸1000次和重复压缩1000次下的相对电阻变化图
图4为实施例3的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料实时监测人体运动图。
具体实施方式
下面通过具体实施例对本发明作进一步的描述,但本发明的保护范围并不仅限于此。
实施例1
一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法:
步骤a:取1 g的MWCNTs粉末加入250 mL三口烧瓶,将67.5 mL浓硫酸倒入三口烧瓶,机械搅拌一段时间。然后缓慢滴加22.5 mL浓硝酸,滴加完成后在50 ℃下回流2 h。获得的分散液用大量去离子水水洗至滤液PH=7,将滤饼在60 ℃下真空干燥,即得a-MWCNTs。
步骤b:分别取3.33g硝酸镁、2.44g硝酸铝与4.68g尿素一起溶于80mL去离子水,搅拌、超声一段时间后,放入反应釜中,在110 ℃下加热24 h,待其冷却之后离心、水洗,将得到的沉淀于烘箱中干燥,获得MgAl-LDH。
步骤c:分别取0.05 g的a-MWCNTs和0.004 gMgAl-LDH分散在50 mL去离子水中,超声处理20 min后,形成均匀的水分散液;将a-MWCNTs/MgAl-LDH水分散液抽滤到绵羊坯革上(D=100 mm),60 ℃下干燥后即得a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
传感材料性能测试:将上述实施例1制备得到的a-MWCNTs/MgAl-LDH/皮革传感材料进行拉伸应变测试,方法为:将制备的一定长宽高的柔性传感材料两端夹持在拉伸运动滑台上,以导电铜胶带作为电极,两端导线连接Keithley 2450型数字源表,测试拉伸应变与传感材料的电阻之间的关系。灵敏度计算公式为GF=(ΔR/R0)/ε,GF为灵敏系数,ε为应变变化,ΔR为电阻变化量,R0为初始电阻。其中,传感材料的长宽高分别为40 mm、10 mm和0.7mm。传感材料的初始距离为20 mm,每次拉伸应变为2 mm。
实施例2
步骤a:取1 g的MWCNTs粉末加入250 mL三口烧瓶,将67.5 mL浓硫酸倒入三口烧瓶,机械搅拌一段时间。然后缓慢滴加22.5 mL浓硝酸,滴加完成后在50 ℃下回流2 h。获得的分散液用大量去离子水水洗至滤液PH=7,将滤饼在60 ℃下真空干燥,即得a-MWCNTs。
步骤b:分别取3.33g硝酸镁、2.44g硝酸铝与4.68g尿素一起溶于80mL去离子水,搅拌、超声一段时间后,放入反应釜中,在110 ℃下加热24 h,待其冷却之后离心、水洗,将得到的沉淀于烘箱中干燥,获得MgAl-LDH。
步骤c:分别取0.05 g的a-MWCNTs和0.006 gMgAl-LDH分散在50 mL去离子水中,超声处理20 min后,形成均匀的水分散液;将a-MWCNTs/MgAl-LDH水分散液抽滤到绵羊坯革上(D=100 mm),60 ℃下干燥后即得a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
实施例3
步骤a:取1 g的MWCNTs粉末加入250 mL三口烧瓶,将67.5 mL浓硫酸倒入三口烧瓶,机械搅拌一段时间。然后缓慢滴加22.5 mL浓硝酸,滴加完成后在50 ℃下回流2 h。获得的分散液用大量去离子水水洗至滤液PH=7,将滤饼在60 ℃下真空干燥,即得a-MWCNTs。
步骤b:分别取3.33g硝酸镁、2.44g硝酸铝与4.68g尿素一起溶于80mL去离子水,搅拌、超声一段时间后,放入反应釜中,在110 ℃下加热24 h,待其冷却之后离心、水洗,将得到的沉淀于烘箱中干燥,获得MgAl-LDH。
步骤c:分别取0.05 g的a-MWCNTs和0.012 gMgAl-LDH分散在50 mL去离子水中,超声处理20 min后,形成均匀的水分散液;将a-MWCNTs/MgAl-LDH水分散液抽滤到绵羊坯革上(D=100 mm),60 ℃下干燥后即得a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
参见图1,上述实施例3制备得到的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料经应变-电阻测试,在30%-60%应变范围内灵敏度可达7238.92。
参见图2,上述实施例3制备得到的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料响应时间较短,其拉伸响应时间和压缩响应时间分别为270 ms、230 ms。图中,(a)拉伸响应时间;(b)压缩响应时间。
参见图3,上述实施例3制备得到的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料在循环拉伸1000次和重复压缩1000次后,相对电阻变化保持稳定。图中,(a)拉伸1000次;(b)压缩1000次。
参见图4,上述实施例3制备得到的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料可用于实时监测人体运动,包括人体较大应变的运动(手指弯曲、肘部弯曲、手腕弯曲、走路、跑步、跳跃)和人体运动的微妙信号(吞咽、脸部表情)。图中(a)手指弯曲;(b)肘部弯曲;(c)手腕弯曲;(d)走路;(e)跑步;(f)跳跃;(g)吞咽;(h)张嘴;(i)脸部鼓起。
本发明的内容不限于实施例所列举,本领域普通技术人员通过阅读本发明说明书而对本发明技术方案采取的任何等效的变换,均为本发明的权利要求所涵盖。
Claims (9)
1.一种a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于:
采用酸化后的多壁碳纳米管a-MWCNTs作为一维导电纳米材料,与二维材料MgAl-LDH物理共混,制备a-MWCNTs/MgAl-LDH复合材料;通过抽滤的工艺将a-MWCNTs/MgAl-LDH复合材料负载在皮革的纤维表面用于构建传感器所必需的电子传输通道,然后在a-MWCNTs/MgAl-LDH复合材料包覆的皮革表面连接电极,制备得到柔性可穿戴应变传感材料。
2.根据权利要求1所述的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于,所述皮革为绵羊坯革,厚度为0.5-0.8 mm。
3.根据权利要求1所述的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于,所述a-MWCNTs在复合材料中的质量浓度为0.5-2 g/L。
4.根据权利要求1所述的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于,所述MgAl-LDH的横向尺寸为2-3 um。
5.根据权利要求1所述的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于:
具体步骤为:
步骤一、分别制备a-MWCNTs和MgAl-LDH:
将MWCNTs加入烧瓶中,倒入浓硫酸后机械搅拌,缓慢滴加浓硝酸,滴加完成后在50 ℃下回流2h,得到分散液,将分散液用去离子水水洗至滤液PH=7,所得滤饼在60 ℃下真空干燥,即得a-MWCNTs;
将硝酸镁、硝酸铝、尿素溶解在去离子水中,搅拌、超声,在110 ℃下加热24 h,冷却后离心、水洗,真空干燥,获得MgAl-LDH;
步骤二、制备a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料:
分别取a-MWCNTs和MgAl-LDH分散在一定体积的去离子水中,超声处理,获得a-MWCNTs/MgAl-LDH水分散液;
将a-MWCNTs/MgAl-LDH水分散液抽滤到绵羊坯革上(D=100 mm),60 ℃下干燥后即得a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
6.根据权利要求5所述a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于,步骤一中,所述MWCNTs在浓硫酸和浓硝酸混合溶液中的质量浓度为8-12g/L;所述浓硫酸和浓硝酸的体积比为3:1。
7.根据权利要求5所述a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于,步骤一中,所述硝酸镁与硝酸铝的摩尔比为2:1;所述尿素的浓度为0.3-1.0 mol/L。
8.根据权利要求5所述a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料的制备方法,其特征在于,步骤二中,所述MgAl-LDH的加入量为a-MWCNTs的8 wt%-24 wt%。
9.如权利要求1-8任一项权利要求所述制备方法制得的a-MWCNTs/MgAl-LDH/皮革柔性可穿戴应变传感材料。
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