CN113483796B - 一种新型“三明治”结构柔性传感器复合膜的制备方法 - Google Patents
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Abstract
本发明公开了一种新型“三明治”结构柔性传感器复合膜的制备方法。采用剑麻纤维、桃胶多糖、聚酰亚胺石墨烯炭化膜为原料,利用自组装方法制备羧基/桃胶多糖柔性膜,并与聚酰亚胺石墨烯炭化膜复合,通过模压成型方法制备具有“三明治”结构柔性传感器复合膜。本发明方法具有制备工艺简单,附着力强,传感性能显著等特点,电阻式弯曲传感器在(0°~90°~0°)800次重复快速弯曲循环后,仍然能提供稳定的电子信号。
Description
技术领域
本发明属于柔性导电膜传感器领域,尤其涉及一种新型“三明治”结构柔性传感器复合膜的制备方法。
背景技术
柔性传感器是指采用柔性材料制成的传感器,具有良好的柔韧性、延展性、能自由弯曲甚至折叠,而且结构形式灵活多样,可根据测量条件的要求任意布置,能够非常方便地对复杂被测量进行检测。新型柔性传感器在电子皮肤、医疗保健、电子、电工、运动器材、纺织品、航天航空、环境监测等领域得到了广泛的应用。柔性可穿戴压力传感器主要由导电纳米材料和柔性塑料基板的组合制备。目前使用较多的导电纳米材料有单层石墨烯、碳纳米管、金属银纳米线、金属铜纳米线及其复合材料。其中,石墨烯因具有特殊的二维表面结构,独特电子学、热学、机械性能和优异的导电性等,使其在柔性导电薄膜电子产品中有广阔的应用前景。然而,石墨烯材料难以在其他聚合物基体中分散,是制约其大规模应用的难点。
聚酰亚胺(PI)树脂是一种具有高模量、高强度、低吸水率、耐水解、耐辐射,优异绝缘性及耐热氧化稳定性的工程塑料。对聚酰亚胺薄膜进行高温石墨化处理可获得结构规整的石墨烯炭化膜,不仅解决了石墨烯材料在聚合物基体中分散性,同时使其既具有传统炭材料密度低、耐高温、耐腐蚀且高强高模等特点,又具有优异的传导性能,在柔性可穿戴压力传感器中具有潜在的应用前景。
纤维素具有很好的亲水性、生物降解性、柔韧性及出色的机械强度等多种优势,被广泛应用于各类柔性基材和增强相填料。纤维上丰富的官能团提供了相互作用的位点,可通过强氢键与功能化石墨烯炭化膜结合,从而构建了连续的导电路径。然而,当前开发的柔性传感器大多由不可生物降解的原材料(如某些塑料)组成,当在使用结束后,这些废弃电子设备可能对环境造成不利影响。将生物可降解材料应用到柔性传感器上,可减少电子污染,实现柔性传感器优异的性能特性和低廉的生产制造成本。本发明利用剑麻纳米纤维和功能化石墨烯炭化膜复合制备柔性传感器膜,该传感器膜的制备方法目前未见报道。
发明内容
本发明的目的在于克服现有技术的不足,以剑麻纤维为原料,通过一种工艺简单,操作方便,绿色环保的方法制备剑麻纳米纤维/功能化石墨烯炭化膜/剑麻纳米纤维复合的“三明治”结构柔性导电薄膜。该薄膜具有优良的柔韧性和导电性,良好的生物相容性以及力学性能。为了实现上述发明目的,本发明采用的技术方案如下:
1、羧甲基剑麻纤维(MSF-g-COOH)的制备:将50~60克剑麻纤维(1~3cm)、70~100毫升5wt%NaOH和300~350毫升去离子水置于特氟龙高压釜中,于180℃温度下加热3~4小时后,过滤,水洗除去剑麻纤维中的半纤维素、木质素和果胶,于60℃温度下真空干燥12小时得到产物A;取20~25克产物A、5~6克氯乙酸、(40~50mL)10wt%NaOH溶液混合,在180℃温度下搅拌反应3小时后,过滤,水洗至中性,于60℃温度下真空干燥10小时得到产物B;将产物B加入500毫升去离子水中,在均质机中高速搅拌(28000r/min)2~3小时,即得到固含量为0.3wt%的MSF-g-COOH溶液。
2、MSF-g-COOH/桃胶多糖柔性膜的制备:利用自组装方法,取50克固含量为0.3wt%桃胶多糖溶液与50克固含量为0.3wt%的MSF-g-COOH溶液、0.25~0.30克甘油混合搅拌30分钟后,真空脱气,倒入15cm×15cm聚四氟乙烯板中,于60℃温度下真空干燥12小时,得到MSF-g-COOH/桃胶多糖复合膜,将该复合膜放入10wt%柠檬酸溶液中交联,即可得到MSF-g-COOH/桃胶多糖柔性膜。
3、功能化石墨烯炭化膜的制备:先将聚酰亚胺薄膜在真空下,加热至1300~1500℃进行炭化,然后在高纯氩气下升温至2500~3000℃进行石墨化,得到聚酰亚胺石墨烯薄膜,最后将聚酰亚胺石墨烯薄膜在30ml盐酸多巴胺碱性溶液(50mM,pH 8.0)中进行表面功能化改性,即可得到功能化石墨烯炭化膜。
4、“三明治”柔性传感器膜的制备:将上述两类薄膜裁剪成10cm×10cm的正方形小片,将MSF-g-COOH/桃胶多糖柔性膜放在上下层,功能化石墨烯炭化膜放中间层,在室温下压力1MPa平板硫化机压5分钟,即可得到本发明的“三明治”柔性传感器膜。
优选地,所述桃胶多糖的分子量为35000g/mol~38000g/mol。
优选地,所述聚酰亚胺石墨烯薄膜的电导率大于1.5×105S/m,导热率大于1400W/m·k。
本发明具有以下优点:
(1)柔性传感器制备原料来源广泛,工艺简单。
(2)所制备功能化石墨烯碳化膜电导率高,适合做各种传感器膜材料。
(3)所制备的三明治柔性传感器膜附着力强,传感性能显著,能够快速检测弯曲-释放的重复信号,电阻式弯曲传感器在(0°~90°~0°)800次重复快速弯曲循环后,仍然提供稳定的电子信号。
附图说明
图1“三明治”柔性传感器膜断面扫描电镜图;
图2为“三明治”柔性传感器膜的制备及其电阻式弯曲传感性能循环测试试验结果。其中:(a)剑麻纤维素/桃胶多糖复合膜;(b)剑麻纤维素/桃胶多糖复合膜与功能化石墨烯碳化膜封装的三明治膜;(c)三明治膜结构示意图;(d)三明治膜电阻率变化与弯曲耐久性试验示意图。
具体实施方式
实施例合成超分散剂的主要原料如下:石墨烯炭化膜(桂林电器科学研究院有限公司提供),桃胶(食品纯),剑麻纤维(工业级),氯乙酸(化学纯),多巴胺(化学纯),柠檬酸(化学纯),氢氧化钠(化学纯)。
实施例1:
(1)羧甲基剑麻纤维(MSF-g-COOH)的制备:将50克剑麻纤维(1~3cm)、70毫升5wt%NaOH和300毫升去离子水置于特氟龙高压釜中,于180℃温度下加热3小时后,过滤,水洗除去剑麻纤维中的半纤维素、木质素和果胶,于60℃温度下真空干燥12小时得到产物A;取20克产物A、5克氯乙酸、(40mL)10wt%NaOH溶液混合,在180℃温度下搅拌反应3小时后,过滤,水洗至中性,于60℃温度下真空干燥10小时得到产物B;将产物B加入500毫升去离子水中,在均质机中高速搅拌(28000r/min)2小时,即得到固含量为0.3wt%的MSF-g-COOH溶液。
(2)MSF-g-COOH/桃胶多糖柔性膜的制备:利用自组装方法,取50克固含量为0.3wt%桃胶多糖溶液与50克固含量为0.3wt%的MSF-g-COOH溶液、0.25克甘油混合搅拌30分钟后,真空脱气,倒入15cm×15cm聚四氟乙烯板中,于60℃温度下真空干燥12小时,得到MSF-g-COOH/桃胶多糖复合膜,将该复合膜放入10wt%柠檬酸溶液中交联,即可得到MSF-g-COOH/桃胶多糖柔性膜。
(3)功能化石墨烯炭化膜的制备:先将聚酰亚胺薄膜在真空下,加热至1300~1500℃进行炭化,然后在高纯氩气下升温至2500~3000℃进行石墨化,得到聚酰亚胺石墨烯薄膜,最后将聚酰亚胺石墨烯薄膜在30ml盐酸多巴胺碱性溶液(50mM,pH 8.0)中进行表面功能化改性,即可得到功能化石墨烯炭化膜。
(4)“三明治”柔性传感器膜的制备:将上述两类薄膜裁剪成10cm×10cm的正方形小片,将MSF-g-COOH/桃胶多糖柔性膜放在上下层,功能化石墨烯炭化膜放中间层,在室温下压力1MPa平板硫化机压5分钟,即可得到本发明的“三明治”柔性传感器膜。
实施例2:
(1)羧甲基剑麻纤维(MSF-g-COOH)的制备:将50~60克剑麻纤维(1~3cm)、70~100毫升5wt%NaOH和300~350毫升去离子水置于特氟龙高压釜中,于180℃温度下加热3小时后,过滤,水洗除去剑麻纤维中的半纤维素、木质素和果胶,于60℃温度下真空干燥12小时得到产物A;取20~25克产物A、5克氯乙酸、(40~50mL)10wt%NaOH溶液混合,在180℃温度下搅拌反应3小时后,过滤,水洗至中性,于60℃温度下真空干燥10小时得到产物B;将产物B加入500毫升去离子水中,在均质机中高速搅拌(28000r/min)2.5小时,即得到固含量为0.3wt%的MSF-g-COOH溶液。
(2)MSF-g-COOH/桃胶多糖柔性膜的制备:利用自组装方法,取50克固含量为0.3wt%桃胶多糖溶液与50克固含量为0.3wt%的MSF-g-COOH溶液、0.30克甘油混合搅拌30分钟后,真空脱气,倒入15cm×15cm聚四氟乙烯板中,于60℃温度下真空干燥12小时,得到MSF-g-COOH/桃胶多糖复合膜,将该复合膜放入10wt%柠檬酸溶液中交联,即可得到MSF-g-COOH/桃胶多糖柔性膜。
(3)功能化石墨烯炭化膜的制备:先将聚酰亚胺薄膜在真空下,加热至1300~1500℃进行炭化,然后在高纯氩气下升温至2500~3000℃进行石墨化,得到聚酰亚胺石墨烯薄膜,最后将聚酰亚胺石墨烯薄膜在30ml盐酸多巴胺碱性溶液(50mM,pH 8.0)中进行表面功能化改性,即可得到功能化石墨烯炭化膜。
(4)“三明治”柔性传感器膜的制备:将上述两类薄膜裁剪成10cm×10cm的正方形小片,将MSF-g-COOH/桃胶多糖柔性膜放在上下层,功能化石墨烯炭化膜放中间层,在室温下压力1MPa平板硫化机压5分钟,即可得到本发明的“三明治”柔性传感器膜。
实施例3:
(1)羧甲基剑麻纤维(MSF-g-COOH)的制备:将50~60克剑麻纤维(1~3cm)、70~100毫升5wt%NaOH和300~350毫升去离子水置于特氟龙高压釜中,于180℃温度下加热4小时后,过滤,水洗除去剑麻纤维中的半纤维素、木质素和果胶,于60℃温度下真空干燥12小时得到产物A;取20~25克产物A、6克氯乙酸、(40~50mL)10wt%NaOH溶液混合,在180℃温度下搅拌反应3小时后,过滤,水洗至中性,于60℃温度下真空干燥10小时得到产物B;将产物B加入500毫升去离子水中,在均质机中高速搅拌(28000r/min)3小时,即得到固含量为0.3wt%的MSF-g-COOH溶液。
(2)MSF-g-COOH/桃胶多糖柔性膜的制备:利用自组装方法,取50克固含量为0.3wt%桃胶多糖溶液与50克固含量为0.3wt%的MSF-g-COOH溶液、0.30克甘油混合搅拌30分钟后,真空脱气,倒入15cm×15cm聚四氟乙烯板中,于60℃温度下真空干燥12小时,得到MSF-g-COOH/桃胶多糖复合膜,将该复合膜放入10wt%柠檬酸溶液中交联,即可得到MSF-g-COOH/桃胶多糖柔性膜。
(3)功能化石墨烯炭化膜的制备:先将聚酰亚胺薄膜在真空下,加热至1300~1500℃进行炭化,然后在高纯氩气下升温至2500~3000℃进行石墨化,得到聚酰亚胺石墨烯薄膜,最后将聚酰亚胺石墨烯薄膜在30ml盐酸多巴胺碱性溶液(50mM,pH 8.0)中进行表面功能化改性,即可得到功能化石墨烯炭化膜。
(4)“三明治”柔性传感器膜的制备:将上述两类薄膜裁剪成10cm×10cm的正方形小片,将MSF-g-COOH/桃胶多糖柔性膜放在上下层,功能化石墨烯炭化膜放中间层,在室温下压力1MPa平板硫化机压5分钟,即可得到本发明的“三明治”柔性传感器膜。
以上所述的实施例仅是本发明的较优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进,这些改进也应视为本发明的保护范围。
Claims (3)
1.一种新型“三明治”结构柔性传感器复合膜的制备方法,其特征在于,具体步骤为:
(1)羧甲基剑麻纤维(MSF-g-COOH)的制备:将50~60克的1~3cm剑麻纤维、70~100毫升5wt%NaOH和300~350毫升去离子水置于特氟龙高压釜中,于180℃温度下加热3~4小时后,过滤,水洗除去剑麻纤维中的半纤维素、木质素和果胶,于60℃温度下真空干燥12小时得到产物A;取20~25克产物A、5~6克氯乙酸、40~50mL的10wt%NaOH溶液混合,在180℃温度下搅拌反应3小时后,过滤,水洗至中性,于60℃温度下真空干燥10小时得到产物B;将产物B加入500毫升去离子水中,在28000r/min均质机中高速搅拌2~3小时,即得到固含量为0.3wt%的MSF-g-COOH溶液;
(2)MSF-g-COOH/桃胶多糖柔性膜的制备:利用自组装方法,取50克固含量为0.3wt%桃胶多糖溶液与50克固含量为0.3wt%的MSF-g-COOH溶液、0.25~0.30克甘油混合搅拌30分钟后,真空脱气,倒入15cm×15cm聚四氟乙烯板中,于60℃温度下真空干燥12小时,得到MSF-g-COOH/桃胶多糖复合膜,将该复合膜放入10wt%柠檬酸溶液中交联,即可得到MSF-g-COOH/桃胶多糖柔性膜;
(3)功能化石墨烯炭化膜的制备:先将聚酰亚胺薄膜在真空下,加热至1300~1500℃进行炭化,然后在高纯氩气下升温至2500~3000℃进行石墨化,得到聚酰亚胺石墨烯薄膜,最后将聚酰亚胺石墨烯薄膜在30ml盐酸多巴胺碱性溶液50mM,pH 8.0中进行表面功能化改性,即可得到功能化石墨烯炭化膜;
(4)“三明治”柔性传感器膜的制备:将上述两类薄膜裁剪成10cm×10cm的正方形小片,将MSF-g-COOH/桃胶多糖柔性膜放在上下层,功能化石墨烯炭化膜放中间层,在室温下压力1MPa平板硫化机压5分钟,即可得到“三明治”柔性传感器膜。
2.根据权利要求1所述的制备的方法,其特征在于,所述桃胶多糖的分子量为35000g/mol~38000g/mol。
3.根据权利要求1所述的制备方法,其特征在于,所述的聚酰亚胺石墨烯薄膜的电导率大于1.5×105S/m,导热率大于1400W/m·k。
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