CN108538619A - 一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法 - Google Patents
一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法 Download PDFInfo
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Abstract
本发明涉及一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，首先将活性炭和石墨烯的混合均匀抽滤成柔性薄膜，活性炭夹杂在石墨烯片层之间，可扩大石墨烯层间距，防止其絮聚，并可作为柔性基体电沉积聚吡咯纳米颗粒，得到柔性、自支撑、无胶黏剂的石墨烯/活性炭/聚吡咯复合电极。通过采用不同电沉积方法和参数设置来合成具有不同微观形貌和优异电化学性能的柔性薄膜电极。本发明利用废弃纤维板制备活性炭粉末，将其应用在柔性电极材料的制备中，具有安全、低价、环保等优点，同时电沉积聚吡咯，提高了赝电容性能，获得的电极材料在柔性储能装置中具有广阔的应用前景。
Description
技术领域
本发明涉及一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，属于电子材料技术领域。
背景技术
随着人们生活水平的不断提高，人们对柔性可穿戴及便携式电子产品(如柔性可折叠显示器、电子书、平板电脑及超薄智能手机等)的需求与日俱增。超级电容器作为一种新型绿色储能器件，具有较大的容量，比能量或能力密度，较宽的工作温度范围和极长的使用寿命，已经成为解决世界所面临的能源、资源和环境等重大问题的最有潜力的电化学储能装置之一。因此，开发具有柔性、轻质、低成本且高性能的超级电容器成为当今储能研究领域的重点及热点。
而作为电容器主要电极材料的活性炭，因其呈粉末状不易被直接加工成柔性电极材料，且活性炭结构复杂，孔利用率低，导电性差，充电慢。并且在传统的超级电容器中，电极材料通常需要胶黏剂粘结在导电集流体上。集流体一般采用导电性良好的金属材料(如泡沫镍，不锈钢网，钛箔等)。但金属材料本身质硬，屈服强度高，易疲劳损伤且质量笨重(密度大)。此外长期浸泡在电解液中很容易被腐蚀，从而影响电极的使用范围和寿命。因此，用它们作为柔性轻质的超级电容器集流体存在着极大的缺点。纵观各种材料，石墨烯因其具有良好的导电性，优异的机械性能和柔韧性，超薄及轻盈的质量(密度小)，成为制备柔性超级电容器电极材料的首选。但石墨烯片层之间由于π-π相互作用和范德华力，极易形成絮聚或堆叠，从而导致电化学性能的下降。因此，石墨烯的组装和调控是影响电化学性能的至关因素。
近年来，大多数研究者们已将重点集中在石墨烯基复合材料上，包括石墨烯与聚合物、无机纳米粒子或其他碳材料(活性炭、碳纳米管等)的复合。石墨烯充当导电剂和粘结剂，将粉末状的活性炭粘结在一起，活性炭颗粒穿插在石墨烯层间，扩大了层间距，阻止石墨烯片层之间的堆积，增大其比表面积，有利于电解液的扩散。石墨烯/活性炭复合薄膜具有优异的机械柔韧性，可作为集流体或自支撑的电极材料。
聚吡咯常被人们制作成为超级电容器的重要电极材料。与传统电极材料比较而言，聚吡咯具有易于制备(氧化电位低)，价格低廉，循环可靠，电化学性能好，结构稳定性好，生物毒性低，对环境友好等优点，因此是超级电容器电极材料的优秀备选材料。并且聚吡咯可以与不同的材料相复合具有更多优秀的物理化学性能，如提高其力学强度，或是在增加大电流充电条件下依然具有良好电容量的性能。通过电沉积法可制备出分散性好且不同形貌的纳米尺寸聚吡咯电活性材料，其电化学储能能力无疑得到大幅度提高，从而达到工业生产的要求。
发明内容
本发明针对现有技术存在的不足，提供一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法。
本发明通过以下技术方案予以实现：
(1)利用废弃的纤维板，在400-600℃下炭化，700-900℃活化后制备活性炭粉末；
(2)按照1:10-5:1的质量比，将活性炭和氧化石墨烯粉末分散在水和N,N-二甲基甲酰胺中，水和N, N-二甲基甲酰胺的体积比为1:9，超声1-3h至均匀；
(3)滴加微量的还原剂于上述混合溶液中，在恒温水浴锅80-95℃下反应2-5h，量取50-100mL在溶剂抽滤器上抽滤成膜；
(4)将上述柔性石墨烯/活性炭薄膜裁剪成规定形状，配制0.05-0.3M的吡咯和0.2-1.5M的硫酸溶液混合溶液，在三电极体系下电沉积聚吡咯，得到石墨烯/活性炭/聚吡咯柔性复合电极。
作为优选方案，步骤(3)所述的还原剂为水合肼，氢碘酸，硼氢化钠，抗坏血酸等中的任意一种或多种，加入量为10-100μL。
作为优选方案，步骤(4)所述的规则形状为长方形，正方形，圆形等任意形状。
作为优选方案，步骤(4)所述的电沉积方法包括恒电流，恒电位，循环伏安，阶跃电势等中的任意一种或多种。
本发明的显著有点在于：(1)将废弃纤维板制备的活性炭穿插在石墨烯层间，制备了柔性、自支撑、无胶黏剂的薄膜，可直接作为集流体。(2)采用不同电沉积方法和参数设置，在柔性石墨烯/活性炭薄膜上沉积获得不同微观形貌的聚吡咯，大大提高了电极材料的电化学性能。
具体实施方式
以下实施例具体说明本发明一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法。本发明提供优选实施例，但不应该被认为局限于在此阐述的实施例。
本发明实施例所提供的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法包括下列步骤：
第一步，利用废弃的纤维板，在500℃下保温1h进行炭化，750℃活化后1h得到活性炭粉末。
第二步，按照1:1的质量比，将活性炭和氧化石墨烯粉末分散在水和N,N-二甲基甲酰胺中，水和N,N- 二甲基甲酰胺的体积比为1:9，超声2h至均匀。
第三步，滴加17μL的水合肼于上述混合溶液中，在恒温水浴锅95℃下反应3h，量取50mL在溶剂抽滤器上抽滤成膜。
第四步，将上述柔性石墨烯/活性炭薄膜裁剪成2cm x 1cm的矩形，配制0.1M的吡咯和0.5M的硫酸溶液混合溶液，在三电极体系下利用恒电流沉积法沉积聚吡咯，沉积电流密度为15mA/cm2，沉积时间为200s，得到石墨烯/活性炭/聚吡咯柔性复合电极。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，对于所属领域的普通技术人员来说，本发明可以在不偏离其主旨与范围内以许多其他的形式实施。因此，所展示的实施例被视为示意性的而非限制性的，在不脱离如所附权利要求所定义的本发明精神及范围的情况下，本发明可能做出其他不同形式的变化或变动。凡是属于本发明技术方案所引申的显而易见的变化或变动，仍处于本发明的保护范围系列。
Claims (8)
1.一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，该制备方法包括以下操作步骤：
(1)利用废弃的纤维板，经过炭化、活化制备活性炭粉末；
(2)按照一定的质量比，将活性炭和氧化石墨烯粉末分散在水和N,N-二甲基甲酰胺中，超声1-3h至均匀；
(3)滴加微量的还原剂于上述混合溶液中，在恒温水浴锅80-95℃下反应2-5h，量取50-100mL在溶剂抽滤器上抽滤成膜；
(4)将上述柔性石墨烯/活性炭薄膜裁剪成规则形状，配制吡咯电解质溶液，在三电极体系下电沉积聚吡咯，得到石墨烯/活性炭/聚吡咯柔性复合电极。
2.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤一所述的活性炭制备过程中的炭化温度为400-600℃，活化温度为700-900℃。
3.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤二所述的活性炭和氧化石墨烯质量比为1:10-5:1。
4.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤二所述的水和N,N-二甲基甲酰胺的体积比为1:9。
5.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤三所述的还原剂为水合肼，氢碘酸，硼氢化钠，抗坏血酸等中的任意一种或多种，加入量为10-100μL。
6.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤四所述的规则形状为长方形，正方形，圆形等任意形状。
7.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤四所述的吡咯电解质溶液为0.05-0.3M的吡咯和0.2-1.5M的硫酸溶液混合均匀而成。
8.根据权利要求1所述的一种制备石墨烯/活性炭/聚吡咯柔性复合电极的方法，其特征在于，步骤四所述的电沉积方法包括恒电流，恒电位，循环伏安，阶跃电势等中的任意一种或多种。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111276335A (zh) * | 2020-02-17 | 2020-06-12 | 南京理工大学 | 芳纶纳米纤维/石墨烯/导电聚合物柔性复合电极及其制备方法 |
| WO2023070856A1 (zh) * | 2021-10-28 | 2023-05-04 | 中国科学院深圳先进技术研究院 | 柔性复合电极及其制备方法、柔性储能器件 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111276335A (zh) * | 2020-02-17 | 2020-06-12 | 南京理工大学 | 芳纶纳米纤维/石墨烯/导电聚合物柔性复合电极及其制备方法 |
| WO2023070856A1 (zh) * | 2021-10-28 | 2023-05-04 | 中国科学院深圳先进技术研究院 | 柔性复合电极及其制备方法、柔性储能器件 |
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