CN108717904A - 一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法 - Google Patents
一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法。包括以下步骤:聚吡咯的制备、石墨烯量子点/聚吡咯的制备、电化学还原石墨烯量子点/聚吡咯的制备、电化学还原石墨烯量子点/聚吡咯的电化学性能测试。本发明的有益效果是电化学还原石墨烯量子点/聚吡咯制备方法简便,结构规整,具有优异的电化学性能。
Description
技术领域
本发明涉及一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,属于电化学和材料合成领域。
技术背景
为了满足现代社会和生态环境的需求,能量储存设备的发展尤为迫切。锂离子电池和超级电容器是两类主要的电化学储存设备。它们已经受到了全世界科研工作者的关注。相对于锂离子电池来说,超级电容器具有高的功率密度、快速的充放电过程、较长的循环寿命和环境友好性、安全性。超级电容器也叫电化学电容器,按照储电机理可以分为双电层电容器和赝电容器。碳材料是常用的超级电容器材料。金属氧化物/氢氧化物、导电高分子是常用的赝电容电极材料。
导电高分子聚吡咯是一种具有内在导电性的物质。它们具有像金属/半导体等独特的电化学性质并且容易合成、成本低、高的电能储存能力。因此被认为是一种有潜力的超级电容器电极材料。但是导电高分子在充放电过程中结构易形变,导致其倍率性能和循环稳定性能较差。因此,通常将聚吡咯与导电性较好的碳材料复合来制备复合材料来提高其力学性能。但是,由于碳材料尺寸较大,碳材料与导电高分子材料结合程度不均,导致其性能提高程度有限。因此,寻找尺寸恰当的碳材料显得尤为重要。
石墨烯量子点是一种尺寸小于100nm的新型零维碳纳米材料,石墨烯量子点的材料特征主要来源于石墨烯,可以被认为石墨烯非常小的一部分。石墨烯量子点具有良好的发光性能、无毒性、耐光漂白和良好的生物相容性。由于石墨烯量子点表面含有大量含氧官能团,使其导电性不好。近年来,越来越多的方法被用于还原石墨烯量子点来提高其导电性。如水热合成法、化学还原法等。但这些还原方法操作繁琐、耗时较长。电化学还原石墨烯量子点的方法还没有被报道。由于还原石墨烯量子点尺寸较小,导电性较好,因此是理想的与聚吡咯结合均一的碳材料。
本实验通过简单的方法制备出聚吡咯纳米球,控制吡咯单体及氧化剂的含量来控制聚吡咯纳米球的大小,进而探究不同尺寸的聚吡咯纳米球对电容性能的影响。然后通过电化学法还原石墨烯量子点/聚吡咯制备了电化学还原石墨烯量子点/聚吡咯复合材料。实验证明电化学还原石墨烯量子点能够很均匀的分散在聚吡咯微球的表面,并且能够使聚吡咯的导电性能及力学性能增加,从而极大的增大了其比电容,是超级电容器的理想电极材料。
发明内容
本发明的目的是在于提供一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法。本发明提供了一种新型的储能材料的制备方法,将聚吡咯/石墨烯量子点复合材料通过电化学还原的方法制备得到电化学还原石墨烯量子点/聚吡咯复合材料。
本发明所述一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,包括以下步骤:
a、聚吡咯的制备:取0.2mL吡咯单体分散于10mL 0.1mol/L的硫酸溶液中,取0.68g氧化剂溶于5mL去离子水加水稀释至10mL,然后将氧化剂的水溶液滴加到吡咯单体的硫酸溶液中,室温下磁力搅拌5h,最后将得到的产物聚吡咯离心,洗涤,在-54℃下冷冻干燥;
b、石墨烯量子点/聚吡咯的制备:将步骤a中所得聚吡咯超声分散于石墨烯量子点的水溶液中,静置一段时间,然后将分散液离心,洗涤,在-54℃下冷冻干燥;
c、电化学还原石墨烯量子点/聚吡咯修饰电极的制备及电化学性能测试:将步骤b中所得的石墨烯量子点/聚吡咯制成2mg/mL的分散液,用移液枪移取10μL滴涂于玻碳电极的表面并用红外灯烘干,然后通过三电极体系并以石墨烯量子点/聚吡咯修饰玻碳电极为工作电极,饱和甘汞电极为辅助电极,铂片电极为对电极,在pH=7的电解液中通过循环伏安法对石墨烯量子点/聚吡咯进行还原得到电化学还原石墨烯量子点/聚吡咯修饰电极;最后以1mol/L的H2SO4为电解液,以电化学还原石墨烯量子点/聚吡咯修饰电极为工作电极,运用同样的三电极体系对电化学还原石墨烯量子点/聚吡咯进行恒电流充放电测试和循环寿命测试。
进一步,所述步骤a中的氧化剂为过硫酸铵。
进一步,所述步骤b中石墨烯量子点水溶液的浓度为2mg/mL,静置时间为24h。
进一步,所述步骤c中pH=7的电解液为磷酸盐缓冲溶液,循环伏安法扫描的电位区间为-1.4~0V。
本发明的有益效果是:这种电化学还原石墨烯量子点/聚吡咯复合材料制备方法简便,结构规整,具有优异的电化学性能。
附图说明
下面结合附图对本发明进一步说明。
图1为实施例一中制备的电化学还原石墨烯量子点/聚吡咯的透射电镜图;
图2为实施例一中制备的电化学还原石墨烯量子点/聚吡咯、对比例一中制备的电化学还原石墨烯量子点和对比例二中制备的聚吡咯在电流密度为1A/g时的恒电流充放电图;
图3为实施例一中制备的电化学还原石墨烯量子点/聚吡咯、对比例一中制备的电化学还原石墨烯量子点和对比例二中制备的聚吡咯在电流密度10A/g时恒电流充放电循环寿命图。
具体实施方式
现在结合具体实施例对本发明做进一步说明,以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例一:
一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,包括以下步骤:
(1)取0.2mL吡咯单体分散于10mL 0.1mol/L的硫酸溶液中,取0.68g过硫酸铵溶于5mL去离子水加水稀释至10mL,然后将过硫酸铵的水溶液滴加到吡咯单体的硫酸溶液中,室温下磁力搅拌5h,最后将得到的产物聚吡咯离心,洗涤,在-54℃下冷冻干燥。
(2)将步骤(1)中所得聚吡咯超声分散于2mg/mL石墨烯量子点的水溶液中,静置24h,然后将分散液离心,洗涤,在-54℃下冷冻干燥。
(3)将步骤(2)中所得的石墨烯量子点/聚吡咯制成2mg/mL的分散液,用移液枪移取10μL滴涂于玻碳电极的表面并用红外灯烘干,然后通过三电极体系并以石墨烯量子点/聚吡咯修饰玻碳电极为工作电极,饱和甘汞电极为辅助电极,铂片电极为对电极,pH=7的磷酸盐缓冲溶液为电解液,通过循环伏安法在电位区间为-1.4~0V时对石墨烯量子点/聚吡咯进行还原得到电化学还原石墨烯量子点/聚吡咯修饰电极。如图1所示,电化学还原石墨烯量子点/聚吡咯具有规则的形貌。最后以1mol/L的H2SO4为电解液,以电化学还原石墨烯量子点/聚吡咯修饰电极为工作电极,运用同样的三电极体系对电化学还原石墨烯量子点/聚吡咯进行恒电流充放电测试和循环寿命测试。如图2,电化学还原石墨烯量子点/聚吡咯的恒电流充放电测试可以看出,其在电流密度为1A/g时比电容为418F/g。如图3,电化学还原石墨烯量子点/聚吡咯的恒电流充放电测试可以看出,在10A/g的电流密度下,进行1000次循环充放电后,其电容保持率为86.0%,显示了其良好的循环稳定性。
对比例一:
一种可用于电化学储能的电化学还原石墨烯量子点的制备方法,包括以下步骤:
制取2mg/mL的石墨烯量子点的溶液,用移液枪移取10μL滴涂于玻碳电极的表面并用红外灯烘干,然后通过三电极体系并以石墨烯量子点修饰玻碳电极为工作电极,饱和甘汞电极为辅助电极,铂片电极为对电极,pH=7的磷酸盐缓冲溶液为电解液,通过循环伏安法在电位区间为-1.4~0V时对石墨烯量子点进行还原得到电化学还原石墨烯量子点修饰电极。最后以1mol/L的H2SO4为电解液,以电化学还原石墨烯量子点修饰电极为工作电极,运用同样的三电极体系对电化学还原石墨烯量子点进行恒电流充放电测试和循环寿命测试。如图2,电化学还原石墨烯量子点的恒电流充放电测试可以看出,其在电流密度为1A/g时比电容为123F/g。如图3,电化学还原石墨烯量子点的恒电流充放电测试可以看出,在10A/g的电流密度下,进行1000次循环充放电后,其电容保持率为98.8%,显示了其优异的循环稳定性。对比例二:
一种可用于电化学储能的聚吡咯的制备方法,包括以下步骤:
(1)取0.2mL吡咯单体分散于10mL 0.1mol/L的硫酸溶液中,取0.68g过硫酸铵溶于5mL去离子水加水稀释至10mL,然后将过硫酸铵的水溶液滴加到吡咯单体的硫酸溶液中,室温下磁力搅拌5h,最后将得到的产物聚吡咯离心,洗涤,在-54℃下冷冻干燥。
(2)将步骤(1)中所得的聚吡咯制成2mg/mL的分散液,用移液枪移取10μL滴涂于玻碳电极的表面并用红外灯烘干,然后通过三电极体系并以聚吡咯修饰玻碳电极为工作电极,饱和甘汞电极为辅助电极,铂片电极为对电极,1mol/L的H2SO4为电解液,对聚吡咯进行恒电流充放电测试和循环寿命测试。如图2,电化学还原石墨烯量子点/聚吡咯的恒电流充放电测试可以看出,其在电流密度为1A/g时比电容为258F/g。如图3,电化学还原石墨烯量子点/聚吡咯的恒电流充放电测试可以看出,在10A/g的电流密度下,进行1000次循环充放电后,其电容保持率为68.1%。
Claims (4)
1.一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,其特征在于:步骤如下:
a、聚吡咯的制备:取0.2mL吡咯单体分散于10mL 0.1mol/L的硫酸溶液中,取0.68g氧化剂溶于5mL去离子水加水稀释至10mL,然后将氧化剂的水溶液滴加到吡咯单体的硫酸溶液中,室温下磁力搅拌5h,最后将得到的产物聚吡咯离心,洗涤,在-54℃下冷冻干燥;
b、石墨烯量子点/聚吡咯的制备:将步骤a中所得聚吡咯超声分散于石墨烯量子点的水溶液中,静置一段时间,然后将分散液离心,洗涤,在-54℃下冷冻干燥;
c、电化学还原石墨烯量子点/聚吡咯修饰电极的制备及电化学性能测试:将步骤b中所得的石墨烯量子点/聚吡咯制成2mg/mL的分散液,用移液枪移取10μL滴涂于玻碳电极的表面并用红外灯烘干,然后通过三电极体系并以石墨烯量子点/聚吡咯修饰玻碳电极为工作电极,饱和甘汞电极为辅助电极,铂片电极为对电极,在pH=7的电解液中通过循环伏安法对石墨烯量子点/聚吡咯进行还原得到电化学还原石墨烯量子点/聚吡咯修饰电极,最后以1mol/L的H2SO4为电解液,以电化学还原石墨烯量子点/聚吡咯修饰电极为工作电极,运用同样的三电极体系对电化学还原石墨烯量子点/聚吡咯进行恒电流充放电测试和循环寿命测试。
2.根据权利要求1所述一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,其特征是:所述步骤a中的氧化剂为过硫酸铵。
3.根据权利要求1所述一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,其特征是:所述步骤b中石墨烯量子点水溶液的浓度为2mg/mL,静置时间为24h。
4.根据权利要求1所述一种可用于电化学储能的电化学还原石墨烯量子点/聚吡咯复合材料的制备方法,其特征是:所述步骤c中pH=7的电解液为磷酸盐缓冲溶液,循环伏安法扫描的电位区间为-1.4~0V。
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