CN106710887A - 一种沥青掺杂的石墨烯基气凝胶电极材料及其制备方法 - Google Patents
一种沥青掺杂的石墨烯基气凝胶电极材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种沥青掺杂的石墨烯基气凝胶电极材料及其制备方法,其特征在于,是由以下原料制成:沥青3‑7,氧化石墨烯12‑22,葡萄糖10‑20,氟化硼0.2‑0.6,ZnCl2溶液20‑30,KMnO4 30‑40,乙醇80‑100,硅烷偶联剂KH560 3‑5,吡咯20‑30,单质硫1‑2,对甲苯磺酸35‑45,过硫酸铵溶液35‑40,蒸馏水500‑1000;用ZnCl2对气凝胶进行活化后,有利于二氧化锰在其表面附着,同时附着二氧化锰能够将双电层电容与法拉第电容结合,既可提高超级电容器的比电容,又可改善二氧化锰的导电性和与电解液的浸渍能力,提高其循环性能;通过添加沥青,增加了电极材料的稳定性,安全性能高。
Description
技术领域
本发明涉及一种超级电容器的电极材料,具体涉及一种沥青掺杂的石墨烯基气凝胶电极材料及其制备方法。
背景技术
MnO2由于储量丰富、价格低廉、环境友好、以及在很宽的工作窗口下表现出良好的电容性质使其成为超级电容器领域中非常理想的电极材料之一。然而,目前 MnO2材料实际所能达到的电容值仅仅只有理论电容值的 30%甚至更低,为了进一步提高 MnO2电极材料的性能,对 MnO2材料的电荷存储机理的研究是非常必要的。三维石墨烯基气凝胶是近年来开发的一种具有微米结构的新型自组装三维多孔碳材料,由于其独特的结构,因而具有特殊性质:1)超高的表面积;2)超高的电导率(空间上石墨烯相互连接)。这两个特性是储能电极材料所追求的关键性质,被认为是超级电容器的理想电极材料之一,然而,目前对石墨烯基气凝胶材料的微观结构的可控合成仍然面临着科学以及技术上的挑战,正如其他的高分子或无机材料那样,石墨烯基材料的性能主要是由石墨烯片层的堆积方式决定的。另外,已有的研究表明,对于 MnO2材料,由于其晶格结构致密,不利于电解液的侵润,造成其实际比电容较低,同时 MnO2材料的电导率也较低,循环性能较差。为了提高 MnO2和石墨烯基材料的电化学性能,石墨烯基气凝胶可以作为非常好的基底材料与 MnO2进行复合。
季辰辰在其硕士学位论文《MnO2与石墨烯基气凝胶的制备、改性与电化学电容性能的研究》中,制备了一种MnO2包覆的石墨烯基气凝胶材料,但是还存在着气凝胶与MnO2结合不够紧密,其活化性不佳等问题。
发明内容
基于以上思考,本发明旨在提供一种石墨烯基气凝胶电极材料,已解决存在的气凝胶与MnO2结合不够紧密,其活化性不佳等问题。
本发明所要解决的技术问题采用以下的技术方案实现:
一种沥青掺杂的石墨烯基气凝胶电极材料,其特征在于,是由以下重量份的原料制成:
沥青3-7,氧化石墨烯12-22,葡萄糖10-20,氟化硼0.2-0.6,ZnCl2溶液20-30,KMnO4 30-40,乙醇80-100,硅烷偶联剂KH560 3-5,吡咯20-30,单质硫1-2,对甲苯磺酸35-45,过硫酸铵溶液35-40,蒸馏水500-1000;
所述ZnCl2溶液浓度为2-5 mol/L,过硫酸铵溶液浓度为3-6 mol/L。
所述的一种沥青掺杂的石墨烯基气凝胶电极材料的制备方法,其特征在于,是由以下步骤制成:
a. 将氧化石墨烯超声分散于100-150份蒸馏水中,得到分散液;将葡萄糖溶于100-150份蒸馏水中,加入到上述分散液中,超声处理5-20min,得到均一悬浮液;然后将上述悬浊液加入到水热釜中,于160-200℃下保温30-40h,冷却至室温后,经冷冻干燥,得到葡萄糖/石墨烯气凝胶;
b. 将步骤a所得气凝胶浸渍于ZnCl2溶液中,在70-120℃烘箱中放置8-15h,之后转移到管式炉中,氩气气氛、700-900℃下活化1-2h,结束后冷却至室温;之后将其超声分散于100-200份蒸馏水中,加入KMnO4,磁力搅拌10-30min后,于60-70℃下,回流磁力搅拌10-30min,过滤、洗涤、干燥,得到MnO2包覆石墨烯基气凝胶材料;
c. 将沥青在90-120℃下融化搅拌,加入氟化硼,反应20-30min后,通过静电纺丝的方法制得沥青短纤维;
d. 将步骤b所得产物、步骤c所得沥青短纤维分散在乙醇中,加入硅烷偶联剂KH560、单质硫、吡咯、对甲苯磺酸,在真空中搅拌40-70min后,逐滴加入过硫酸铵溶液,冰浴搅拌8-15h;过滤、洗涤、干燥后得到复合电极材料。
所述的一种沥青掺杂的石墨烯基气凝胶电极材料的制备方法,其特征在于,步骤b中干燥条件为:在 60-70℃下干燥 10-15h。
本发明的有益效果是:葡萄糖分子链上的官能团和氧化石墨烯表面的含氧基团通过氢键的相互作用,交联在一起,形成了3D网络结构,而水分子则填充至网络结构的间隙,经冷冻干燥,水分子被除去,从而得到多孔结构的气凝胶;用ZnCl2对气凝胶进行活化后,有利于二氧化锰在其表面附着,同时附着二氧化锰能够将双电层电容与法拉第电容结合,既可提高超级电容器的比电容,又可改善 二氧化锰的导电性和与电解液的浸渍能力,提高其循环性能;用聚吡咯对其进行进一步的包裹,不仅可以加强二氧化锰和气凝胶的结合,又可以使材料表现出更好的电学性能;通过添加沥青,增加了电极材料的稳定性,安全性能高。
具体实施方式
下面结合实施例对本发明的具体实施方式作进一步描述。
实施例
一种沥青掺杂的石墨烯基气凝胶电极材料,其特征在于,是由以下重量份的原料制成:
沥青7,氧化石墨烯22,葡萄糖20,氟化硼0.6,ZnCl2溶液30,KMnO4 40,乙醇100,硅烷偶联剂KH560 5,吡咯30,单质硫2,对甲苯磺酸45,过硫酸铵溶液40,蒸馏水1000;
所述ZnCl2溶液浓度为2-5 mol/L,过硫酸铵溶液浓度为3-6 mol/L。
所述的一种沥青掺杂的石墨烯基气凝胶电极材料的制备方法,其特征在于,是由以下步骤制成:
a. 将氧化石墨烯超声分散于100-150份蒸馏水中,得到分散液;将葡萄糖溶于100-150份蒸馏水中,加入到上述分散液中,超声处理5-20min,得到均一悬浮液;然后将上述悬浊液加入到水热釜中,于160-200℃下保温30-40h,冷却至室温后,经冷冻干燥,得到葡萄糖/石墨烯气凝胶;
b. 将步骤a所得气凝胶浸渍于ZnCl2溶液中,在70-120℃烘箱中放置8-15h,之后转移到管式炉中,氩气气氛、700-900℃下活化1-2h,结束后冷却至室温;之后将其超声分散于100-200份蒸馏水中,加入KMnO4,磁力搅拌10-30min后,于60-70℃下,回流磁力搅拌10-30min,过滤、洗涤、干燥,得到MnO2包覆石墨烯基气凝胶材料;
c. 将沥青在90-120℃下融化搅拌,加入氟化硼,反应20-30min后,通过静电纺丝的方法制得沥青短纤维;
d. 将步骤b所得产物、步骤c所得沥青短纤维分散在乙醇中,加入硅烷偶联剂KH560、单质硫、吡咯、对甲苯磺酸,在真空中搅拌40-70min后,逐滴加入过硫酸铵溶液,冰浴搅拌8-15h;过滤、洗涤、干燥后得到复合电极材料。
所述的一种沥青掺杂的石墨烯基气凝胶电极材料的制备方法,其特征在于,步骤b中干燥条件为:在 60-70℃下干燥 10-15h。
本发明的产品性能测试数据为:经过 1000 圈的循环,电极容量仍≥99%的初始容量。
Claims (3)
1.一种沥青掺杂的石墨烯基气凝胶电极材料,其特征在于,是由以下重量份的原料制成:
沥青3-7,氧化石墨烯12-22,葡萄糖10-20,氟化硼0.2-0.6,ZnCl2溶液20-30,KMnO4 30-40,乙醇80-100,硅烷偶联剂KH560 3-5,吡咯20-30,单质硫1-2,对甲苯磺酸35-45,过硫酸铵溶液35-40,蒸馏水500-1000;
所述ZnCl2溶液浓度为2-5 mol/L,过硫酸铵溶液浓度为3-6 mol/L。
2.根据权利要求1所述的一种沥青掺杂的石墨烯基气凝胶电极材料的制备方法,其特征在于,是由以下步骤制成:
a. 将氧化石墨烯超声分散于100-150份蒸馏水中,得到分散液;将葡萄糖溶于100-150份蒸馏水中,加入到上述分散液中,超声处理5-20min,得到均一悬浮液;然后将上述悬浊液加入到水热釜中,于160-200℃下保温30-40h,冷却至室温后,经冷冻干燥,得到葡萄糖/石墨烯气凝胶;
b. 将步骤a所得气凝胶浸渍于ZnCl2溶液中,在70-120℃烘箱中放置8-15h,之后转移到管式炉中,氩气气氛、700-900℃下活化1-2h,结束后冷却至室温;之后将其超声分散于100-200份蒸馏水中,加入KMnO4,磁力搅拌10-30min后,于60-70℃下,回流磁力搅拌10-30min,过滤、洗涤、干燥,得到MnO2包覆石墨烯基气凝胶材料;
c. 将沥青在90-120℃下融化搅拌,加入氟化硼,反应20-30min后,通过静电纺丝的方法制得沥青短纤维;
d. 将步骤b所得产物、步骤c所得沥青短纤维分散在乙醇中,加入硅烷偶联剂KH560、单质硫、吡咯、对甲苯磺酸,在真空中搅拌40-70min后,逐滴加入过硫酸铵溶液,冰浴搅拌8-15h;过滤、洗涤、干燥后得到复合电极材料。
3.根据权利要求书2所述的一种沥青掺杂的石墨烯基气凝胶电极材料的制备方法,其特征在于,步骤b中干燥条件为:在 60-70℃下干燥 10-15h。
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