CN110993369A - 一种聚乙撑二氧噻吩/二硫化钼复合纤维及其应用 - Google Patents
一种聚乙撑二氧噻吩/二硫化钼复合纤维及其应用 Download PDFInfo
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Abstract
一种聚乙撑二氧噻吩/二硫化钼复合纤维及其应用，属于材料领域和电化学领域。制备方法包括：以四硫代钼酸铵提供钼源和硫源，在聚(3,4‑乙撑二氧噻吩)：聚苯乙烯磺酸钠溶液体系中140‑240℃下反应6.0‑48.0小时，过滤，水洗，干燥后得到一种聚乙撑二氧噻吩/二硫化钼网络多孔复合纤维。将该复合纤维用于超级电容器电极，体积比容量达到436.4F/cm3。本发明合成路线简单，生产周期短，产率较高，易实现工业化生产，产品可应用于生物、催化和储能等领域，具有极大的应用前景。
Description
技术领域
本发明属于材料领域和电化学领域，涉及一种超级电容器复合纤维电极材料，更具体地说涉及一种聚乙撑二氧噻吩/二硫化钼(PEDOT/MoS2)柔性复合纤维的制备方法。
背景技术
过渡金属硫族合物是材料领域中一类重要组成部分。其中，MoS2作为最具代表性的过渡金属硫化物，因其特殊的二维(2D)类石墨烯结构，良好的化学稳定性、热稳定性以及耐腐蚀性，被广泛应用于电化学催化剂、超级电容器、各种离子电池、燃料电池、机械润滑、生物传感以及光电领域等方面。随着人们对2D纳米材料的研究兴趣与日俱增，纳米制备和表征技术不断进步，单层及多层MoS2纳米层在许多领域的应用显示出优异的性能。例如，有报道指出单层MoS2晶体管比石墨烯基器件有更好的光响应，多层MoS2制备的电子传感器对一氧化氮有优异的气敏性，纳米级MoS2制备的超级电容器具有优异的电化学性能。尽管如此，单一MoS2材料所能发挥出来的性能仍然是有限的，且纳米级MoS2粉体无法直接制备成纤维状，较难应用于柔性器件中。众所周知，复合材料能够克服单一材料的缺陷，发挥各组分的优势，具有优越的综合性能。因此，选择适宜种类的基体材料，优化基体材料的掺和比，开发出性能卓越的MoS2复合材料尤为重要。而PEDOT是一种高导电的柔性导电高分子，且原料丰富，价格低廉，容易制备。因此，利用PEDOT为基体，通过控制反应条件与工艺参数，结合硫钼酸盐开发出具有新型功能的柔性复合纤维具有十分重要的意义。
发明内容
针对现有技术存在的不足，为丰富功能化复合材料的种类，本发明提供了一种PEDOT/MoS2复合纤维的制备方法及其应用。
为实现上述目的，本发明所采用的技术方案如下：
一种PEDOT/MoS2复合纤维的制备方法，其包含如下步骤：
(1)复合纤维的制备：将一定量的硫钼酸盐加入到一定浓度的聚(3,4-乙撑二氧噻吩)：聚苯乙烯磺酸钠(PEDOT:PSS)，剧烈摇晃至溶液凝胶化，将凝胶化的混合物注入到聚四氟乙烯毛细管中，一定温度下水热一段时间，冷却至室温，取出PEDOT:PSS/MoS2凝胶纤维，用浓硫酸或极性有机溶剂浸泡一段时间除去大部分PSS，得到PEDOT/MoS2复合纤维。
(2)洗涤：将步骤(1)得到的PEDOT/MoS2复合纤维直接以去离子水洗涤；
(3)干燥：将洗涤过的纤维两端固定，50.0-90.0℃干燥；
优选所述的步骤(1)中硫钼酸盐的添加量为5.0-50.0g/L，PEDOT:PSS的浓度为5.0-20.0g/L，水热反应温度为140.0-240.0℃，反应时间为6.0-48.0小时，浓硫酸或有机溶剂浸泡时间为3.0h-48.0h。
所述的极性有机溶剂指乙二醇或二甲基亚砜中的一种或多种。
所述的硫钼酸盐优选四硫代钼酸铵。
所述的步骤(2)中洗涤是指将得到的PEDOT/MoS2复合纤维置于去离子水中室温下浸泡洗涤。
所述的步骤(3)中干燥是指将洗涤过的复合纤维两端固定，经50.0-90.0℃烘干1.0-12.0小时得到PEDOT/MoS2复合纤维。
本发明的一种PEDOT/MoS2复合纤维，由PEDOT和MoS2构成，通过二者共组装形成网络或多孔复合纤维。
本发明所得PEDOT/MoS2复合纤维，可作为超级电容器电极，比容量达到436.4F/cm3。
本发明的一种PEDOT/MoS2复合纤维，以硫钼酸盐与PEDOT：PSS为原料，通过一步共混水热法得到。与现有技术相比，本发明提供的方法流程操作简单，生产周期短，产率较高，易实现工业化生产，并且所得的一种PEDOT/MoS2复合纤维具有优异的电化学存储性能。
附图说明
为了更详实地表述该发明实施例的技术方案，以下对实施例描述中所使用的附图作简单介绍。显然，以下描述中的附图仅为本发明的一些实施例的附图，对于该领域普通技术人员来讲，在未付诸创造性劳动的前提下，还可依据此类附图获得其它的附图。
图1为本发明实施例1中获得的PEDOT/MoS2复合纤维截面的低倍扫描电子显微镜照片；
图2为本发明实施例1中获得的PEDOT/MoS2复合纤维截面的高倍扫描电子显微镜照片；
图3为本发明实施例2中获得的PEDOT/MoS2复合纤维截面的低倍扫描电子显微镜照片；
图4为本发明实施例2中获得的PEDOT/MoS2复合纤维截面的高倍扫描电子显微镜照片；
图5为本发明实施例1中获得的PEDOT/MoS2复合纤维的X射线衍射图；
图6为本发明实施例1中获得的PEDOT/MoS2复合纤维在不同电流密度下的比容量图；
图7为本发明实施例2中获得的PEDOT/MoS2复合纤维在不同电流密度下的比容量图；
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，使本领域技术人员更好地理解本发明，下面结合附图与实施例对本发明的实施方式作进一步地详细阐述。
实施例1
(1)复合纤维的制备：将26.3mg的四硫代钼酸铵加入到2.0mL浓度为10.5mg/L的PEDOT:PSS溶液中，剧烈摇晃至溶液凝胶化，将凝胶化的混合物注入到聚四氟乙烯毛细管中，180.0℃水热10.0h，冷却至室温，取出PEDOT:PSS/MoS2凝胶纤维，用浓硫酸浸泡12.0h除去大部分PSS，得到PEDOT/MoS2复合纤维。(2)洗涤：将步骤(2)得到的PEDOT/MoS2复合纤维直接以去离子水洗涤；(3)干燥：将洗涤过的纤维两端固定，60.0℃干燥2.0h；
对上述制备得到的一种PEDOT/MoS2复合纤维进行微观形貌、结构以及电化学性能测试，得到如图1所示的低倍扫描电子显微镜照片，如图2所示的高倍扫描电子显微镜照片，如图5所示的X射线衍射图，如图6所示的不同电流密度下的比容量图。
实施例2
(1)复合纤维的制备：将13.15mg的四硫代钼酸铵加入到2mL浓度为7.5mg/L的PEDOT:PSS溶液中，剧烈摇晃至溶液凝胶化，将凝胶化的混合物注入到聚四氟乙烯毛细管中，200.0℃水热8.0h，冷却至室温，取出PEDOT:PSS/MoS2凝胶纤维，用浓硫酸浸泡15.0h除去大部分PSS，得到PEDOT/MoS2复合纤维。(2)洗涤：将步骤(2)得到的PEDOT/MoS2复合纤维直接以去离子水洗涤；(3)干燥：将洗涤过的纤维两端固定，70.0℃干燥1.5h；
对上述制备得到的一种PEDOT/MoS2复合纤维进行微观形貌、结构以及电化学性能测试，得到如图3所示的低倍扫描电子显微镜照片，如图4所示的高倍扫描电子显微镜照片，类似图5所示的X射线衍射图，如图7所示的不同电流密度下的比容量图。
实施例3
(1)复合纤维的制备：将104.0mg的四硫代钼酸铵加入到4.0mL浓度为15.0mg/L的PEDOT:PSS溶液中，剧烈摇晃至溶液凝胶化，将凝胶化的混合物注入到聚四氟乙烯毛细管中，140.0℃水热24.0h，冷却至室温，取出PEDOT:PSS/MoS2凝胶纤维，用乙二醇浸泡30.0h除去大部分PSS，得到PEDOT/MoS2复合纤维。(2)洗涤：将步骤(2)得到的PEDOT/MoS2复合纤维直接以去离子水洗涤；(3)干燥：将洗涤过的纤维两端固定，70.0℃干燥1.5h；
对上述制备得到的一种PEDOT/MoS2复合纤维进行微观形貌、结构以及性能测试，得到类似图3所示的低倍扫描电子显微镜照片，类似图4所示的高倍扫描电子显微镜照片，类似图5所示的X射线衍射图，类似图7所示的不同电流密度下的比容量图。
Claims (9)
1.一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，包含如下步骤：
(1)复合纤维的制备：将一定量的硫钼酸盐加入到一定浓度的聚(3,4-乙撑二氧噻吩)：聚苯乙烯磺酸钠PEDOT:PSS中，剧烈摇晃至溶液凝胶化，将凝胶化的混合物注入到聚四氟乙烯毛细管中，一定温度下水热一段时间，冷却至室温，取出PEDOT:PSS/MoS2凝胶纤维，用浓硫酸或极性有机溶剂浸泡一段时间除去大部分PSS，得到PEDOT/MoS2复合纤维；
(2)洗涤：将步骤(1)得到的PEDOT/MoS2复合纤维直接以去离子水洗涤；
(3)干燥：将洗涤过的纤维两端固定，50.0-90.0℃干燥。
2.按照权利要求1所述的一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，所述的步骤(1)中硫钼酸盐的添加量为5.0-50.0g/L，PEDOT:PSS的浓度为5.0-20.0g/L。
3.按照权利要求1所述的一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，所述的步骤(1)中水热反应温度为140.0-240.0℃，反应时间为6.0-48.0小时。
4.按照权利要求1所述的一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，所述的步骤(1)中浓硫酸或极性有机溶剂浸泡时间为3.0h-48.0h。
5.按照权利要求1所述的一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，所述的步骤(1)中所述的极性有机溶剂指乙二醇或二甲基亚砜中的一种或多种。
6.按照权利要求1所述的一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，所述的步骤(1)中所述的硫钼酸盐优选四硫代钼酸铵。
7.按照权利要求1所述的一种聚乙撑二氧噻吩/二硫化钼复合纤维的制备方法，其特征在于，所述的步骤(2)中洗涤是指将得到的PEDOT/MoS2复合纤维置于去离子水中室温下浸泡洗涤；所述的步骤(3)中干燥是指将洗涤过的复合纤维两端固定，经50.0-90.0℃烘干1.0-12.0小时得到PEDOT/MoS2复合纤维。
8.按照权利要求1-7任一项所述的方法制备得到的一种聚乙撑二氧噻吩/二硫化钼复合纤维。
9.按照权利要求1-7任一项所述的方法制备得到的一种聚乙撑二氧噻吩/二硫化钼复合纤维的应用，用于超级电容器电极。
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| CN110085436A (zh) * | 2019-04-21 | 2019-08-02 | 北京工业大学 | 一种石墨烯/聚乙撑二氧噻吩复合纤维组装体的制备方法 |
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