CN110735323A - 导电复合纳米纤维膜的制备方法 - Google Patents

导电复合纳米纤维膜的制备方法 Download PDF

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CN110735323A
CN110735323A CN201810807572.9A CN201810807572A CN110735323A CN 110735323 A CN110735323 A CN 110735323A CN 201810807572 A CN201810807572 A CN 201810807572A CN 110735323 A CN110735323 A CN 110735323A
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nanofiber membrane
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冯章启
杜丽娟
吴方方
袁旭
严珂
金飞
李�瑞
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Nanjing Tech University
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Abstract

本发明公开了一种导电复合纳米纤维膜的制备方法。所述方法先采用静电纺丝技术，制备具有能与磺酸基形成氢键的基团的聚合物纳米纤维膜，然后将聚合物纳米纤维膜平整的置于铜网上，滴加PEDOT：PSS溶液，使之均匀铺展在纳米纤维膜上，静置，除去表面多余的溶液，在100～160℃退火，稀硫酸处理，得到PEDOT：PSS包覆的导电复合纳米纤维。本发明的制备工艺简单，充分利用了PEDOT：PSS电化学和氧化稳定性，制得的导电纳米纤维的导电率达到了3.28ⅹ10‑2S cm‑1。

Description

导电复合纳米纤维膜的制备方法
技术领域
本发明属于静电纺丝技术领域，涉及一种导电复合纳米纤维膜的制备工艺。
背景技术
导电聚合物具有高导电性、特殊的光学性能和高机械灵活性，在生物传感器、组织工程支架、神经探针、药物输送装置和生物致动器等领域具有重要应用。由于其具有高电导率，可以促进生物化学反应产生的电荷转移到电子电路，能够提高生物传感器的响应速度，灵敏度和多功能性。
在导电聚合物中，聚(3,4-亚乙基二氧噻吩)(PEDOT)常作为如神经系统，心脏和骨骼肌中的电极或活性物质。现有的聚3，4-乙烯二氧噻吩/聚苯乙烯磺酸盐(PEDOT:PSS)纳米复合纤维膜多采用原位聚合法。但是采用原位聚合法需要控制多个条件，较为复杂。Wang等(Wang S,et al.Chitosan/gelatin porous scaffolds assembled with conductivepoly(3,4-ethylenedioxythiophene)nanoparticles for neural tissue engineering[J].Journal of Materials Chemistry B,2017,5(24).)通过原位聚合法得到的PEDOT/壳聚糖明胶支架的导电率只有4.95×10-4S cm-1。
发明内容
本发明的目的在于提供了一种导电复合纳米纤维膜的制备方法。该方法采用简单的非原位渗透法，将导电高分子PEDOT:PSS包覆聚合物静电纺丝纳米纤维膜，制成导电复合纳米纤维膜。
实现本发明目的的技术方案如下：
导电复合纳米纤维膜的制备方法，具体步骤如下：
步骤1，采用静电纺丝技术，制备具有能与磺酸基(﹣SO3H)形成氢键的基团的聚合物纳米纤维膜；
步骤2，将聚合物纳米纤维膜平整的置于铜网上，滴加PEDOT：PSS溶液，使之均匀铺展在纳米纤维膜上，静置，除去表面多余的溶液，在100～160℃退火，稀硫酸处理，得到PEDOT：PSS包覆的导电复合纳米纤维。
优选地，步骤1中，所述的具有能与磺酸基(﹣SO3H)形成氢键的基团的聚合物选自聚丙烯腈、聚己内酯、聚乳酸、聚乳酸-羟基乙酸共聚物或聚乙烯吡咯烷酮。
优选地，步骤2中，所述的PEDOT：PSS溶液的质量分数为0.2wt％～1.4wt％，静置时间为2min～5min，退火时间为10min～15min。
优选地，步骤2中，所述的稀硫酸的浓度为0.2～1.0mol/L。
优选地，步骤2中，所述的稀硫酸处理时间为5min～10min。
本发明通过非原位渗透法成功获得了PEDOT：PSS包覆的导电复合纳米纤维膜，并经稀硫酸处理，使纳米纤维膜具有高导电性，导电率达到了3.28ⅹ10-2S cm-1。
附图说明
图1为导电聚丙烯腈复合纳米纤维扫描电镜图。
图2为对比例1中未除去表面多余物质制得的复合纳米纤维扫描电镜图。
图3为实施例1和对比例2制得的复合纳米纤维的循环伏安图。
具体实施方式
下面结合具体实施例，对本发明作进一步详述。
实施例1以聚丙烯腈为原料制作导电聚丙烯腈复合纳米纤维膜
(1)将0.45克的聚丙烯腈溶于3mL的N,N二甲基甲酰胺溶液中，质量分数15％，磁力搅拌至溶液澄清均一，然后1000转下离心1分钟，除去溶液中的气泡。
(2)在搭建好的电纺装置进行电纺，将聚丙烯腈溶液倒入10mL塑料注射器中，金属针内径为0.8mm的不锈钢针头，接收基材为锡箔纸。电纺参数：纺丝电压15kV，接收距离15cm，推进速度为1.0ml/h，纤维膜纺丝溶液体积量为5mL，将得到的聚丙烯腈纳米纤维膜干燥以除去残留溶剂。
(3)取1mL的PEDOT：PSS溶液在3000转下离心3min，取0.3mL的上清液于试剂瓶中，加入1.1mL的去离子水后在超声机中超声10min，配置得到质量分数为0.3％的PEDOT：PSS溶液。
(4)取5×5cm2大小的聚丙烯腈纳米纤维膜，滴加1mL的质量分数为0.3％的PEDOT：PSS溶液，使之均匀的铺展在纳米纤维膜上，静置2min后用滤纸吸干多余的溶液，之后放入烘箱中在120℃下退火15min即得到PEDOT：PSS包覆的聚丙烯腈复合纳米纤维膜。
(5)将聚丙烯腈复合纳米纤维膜用1mol/L的稀硫酸处理10min。导电率由1.29ⅹ10-3S cm-1提升到3.28ⅹ10-2S cm-1。
实施例2以聚乳酸为原料制作导电聚乳酸复合纳米纤维膜
(1)将0.15克的聚乳酸溶于3mL的N,N二甲基甲酰胺溶液中，质量分数5％，磁力搅拌至溶液澄清均一，然后1000转下离心1分钟，除去溶液中的气泡。
(2)在搭建好的电纺装置进行电纺，将聚乳酸溶液倒入10mL塑料注射器中，金属针内径为0.8mm的不锈钢针头，接收基材为锡箔纸。纺丝电压15kV，接收距离15cm，推进速度为1.0ml/h，纤维膜纺丝溶液体积量为5mL，将得到的聚丙烯腈纳米纤维膜干燥以除去残留溶剂。
(3)取1mL的PEDOT：PSS溶液在3000转下离心3min，取0.2mL的上清液于试剂瓶中，加入1.2mL的去离子水后在超声机中超声10min，配置得到质量分数为0.2％的PEDOT：PSS溶液。
(4)取5×5cm2大小的聚乳酸纳米纤维膜，滴加1mL的质量分数为0.2％的PEDOT：PSS溶液，使之均匀的铺展在纳米纤维膜上，静置2min后用滤纸吸干多余的溶液，之后放入烘箱中在120℃下退火15min即得到PEDOT：PSS包覆的聚乳酸复合纳米纤维膜。
(5)将聚乳酸复合纳米纤维膜用1mol/L的稀硫酸处理8min。导电率由3.45ⅹ10- 3Scm-1提升到1.23ⅹ10-2S cm-1。
实施例3以聚己内酯为原料制作导电聚己内酯复合纳米纤维膜
(1)将0.27克的聚己内酯溶于和3mL的N,N二甲基甲酰胺混合溶液中，质量分数为9％，磁力搅拌至溶液澄清均一，然后1000转下离心1分钟，除去溶液中的气泡。
(2)在搭建好的电纺装置进行电纺，将聚己内酯溶液倒入10mL塑料注射器中，金属针内径为0.8mm的不锈钢针头，接收基材为锡箔纸。纺丝电压15kV，接收距离10cm，推进速度为0.8ml/h，纤维膜纺丝溶液体积量为5mL。将得到的聚己内酯纳米纤维膜干燥以除去残留溶剂。
(3)取1mL的PEDOT：PSS溶液在3000转下离心3min,取上清液于试剂瓶中，在超声机中超声10min，得到质量分数为1.4％的PEDOT：PSS溶液。
(4)取5×5cm2大小的聚乳酸纳米纤维膜，滴加1mL的质量分数为1.4％的PEDOT：PSS溶液，使之均匀的铺展在纳米纤维膜上，静置5min后用滤纸吸干多余的溶液，之后放入烘箱中在120℃下退火15min即得到PEDOT：PSS包覆的聚己内酯复合纳米纤维膜。
(5)将聚己内酯复合纳米纤维膜用1mol/L的硫酸处理2min。导电率由4.57ⅹ10- 3Scm-1提升到5.23ⅹ10-2S cm-1。
对比例1
本对比例与实施例1基本相同，唯一不同的是滴加完PEDOT：PSS溶液后，不除去表面多余的溶液。图2为对比例1中未除去表面多余物质制得的复合纳米纤维扫描电镜图。从图2中可看出，PEDOT:PSS在纳米纤维膜表面形成了一层PEDOT：PSS膜。
对比例2
本对比例与实施例1基本相同，唯一不同的是得到导电复合膜后，不用硫酸处理。图2为实施例1和对比例2制得的复合纳米纤维的循环伏安图。从图3循环伏安图中可看出，经硫酸处理后，导电复合膜的电导率得到了一个数量级的提升。

Claims (7)

1.导电复合纳米纤维膜的制备方法，其特征在于，具体步骤如下：
步骤1，采用静电纺丝技术，制备具有能与磺酸基形成氢键的基团的聚合物纳米纤维膜；
步骤2，将聚合物纳米纤维膜平整的置于铜网上，滴加PEDOT：PSS溶液，使之均匀铺展在纳米纤维膜上，静置，除去表面多余的溶液，在100～160℃退火，稀硫酸处理，得到PEDOT：PSS包覆的导电复合纳米纤维。
2.根据权利要求1所述的制备方法，其特征在于，步骤1中，所述的具有能与磺酸基形成氢键的基团的聚合物选自聚丙烯腈、聚己内酯、聚乳酸、聚乳酸-羟基乙酸共聚物或聚乙烯吡咯烷酮。
3.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的PEDOT：PSS溶液的质量分数为0.2wt％～1.4wt％。
4.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的静置时间为2min～5min。
5.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的退火时间为10min～15min。
6.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的稀硫酸的浓度为0.2～1.0mol/L。
7.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的稀硫酸处理时间为5min～10min。
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CN114685811A (zh) * 2020-12-29 2022-07-01 Tcl科技集团股份有限公司 一种pedot材料、量子点发光二极管及制备方法
CN114685811B (zh) * 2020-12-29 2024-03-12 Tcl科技集团股份有限公司 一种pedot材料、量子点发光二极管及制备方法
CN116427052A (zh) * 2023-03-10 2023-07-14 武汉纺织大学 一种防静电聚乳酸面料及其制备方法
CN116427052B (zh) * 2023-03-10 2024-05-03 武汉纺织大学 一种防静电聚乳酸面料及其制备方法

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