CN106128790A - 一种石墨烯超级电容器电极材料的制备方法 - Google Patents
一种石墨烯超级电容器电极材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯超级电容器电极材料的制备方法,在纳米多孔金薄膜表面沉积石墨烯材料,所述的沉积方法采用电化学循环伏安法,所述的石墨烯材料的浓度为0.02g/L‑0.5g/L,在采用电化学循环伏安法沉积石墨烯材料的过程中,沉积窗口为0‑2V电压,循环次数50‑600次,扫描速率10‑200mVs‑1。本发明的超级电容器电极材料具有高比电容以及良好的结构稳定性、循环稳定性。比电容高达864 F/g,循环2000次仍保持90%的比电容。适用于高稳定性、高功率密度的电源场合。
Description
技术领域
本发明属于材料学领域,涉及一种超级电容器,具体来说是一种超级电容器电极材料的制备方法。
背景技术
超级电容器是最具应用前景的电化学储能技术之一。目前,超级电容器的研究重点是提高能量密度和功率密度,发展具有高比表面积、高电导率以及结构稳定性的电极材料。相比传统的炭材料,石墨烯具有非常高的导电性、极大的比表面积和大量的层间构造,片层两边均可以富集电荷形成双电层且利于电解液的扩散,是理想的超级电容器电极材料。以石墨烯来制备的石墨烯超级电容器具有大功率、快速充放电和循环稳定性强等特点。石墨烯虽然可以单独作为超级电容器电极材料,但存在以下技术难题:(1)其理论比容量仅有329 F/g,限制了该材料的大规模应用;(2)在石墨烯基电极制备过程中容易发生堆叠现象,影响石墨烯材料在电解质中的分散性和表面可浸润性,导致石墨烯材料比表面积和离子电导率下降。因此,有效减少石墨烯片层聚集和堆叠以获得良好的体积比电容是构建新型石墨烯基超级电容器的关键。
对于超级电容器材料,至关重要的特性是比表面积和导电性。纳米多孔金具有双连续的内部结构、高比表面积和良好的导电性等特点,具有独特的物理、化学性能,是良好的负载材料。通过控制纳米孔径的大小及分布,可进一步提高比表面积。
发明内容
针对现有技术中的上述技术问题,本发明提供了一种石墨烯超级电容器电极材料的制备方法,所述的这种石墨烯超级电容器电极材料的制备方法要解决现有技术中的超级电容器电极材料易于发生堆叠、导电性欠佳的技术问题。
本发明提供了一种超级电容器电极材料的制备方法,在纳米多孔金薄膜表面沉积石墨烯材料,所述的沉积方法采用电化学循环伏安法,所述的石墨烯材料的浓度为0.02g/L-0.5g/L,在采用电化学循环伏安法沉积石墨烯材料的过程中,沉积窗口为0-2V电压,循环次数50-600次,扫描速率10-200mVs-1。
进一步的,所述石墨烯材料选自氧化石墨烯、石墨烯量子点、氮掺杂石墨烯或者氮掺杂石墨烯量子点。
进一步的,石墨烯或者氮掺杂石墨烯为单层或者多层氧化石墨烯;石墨烯量子点或氮掺杂石墨烯量子点颗粒大小为2-10nm。
进一步的,还包括一个对超级电容器电极材料进行热处理的过程,热处理温度为100-500oC,热处理时间20-120分钟。
进一步的,在采用电化学循环伏安法沉积石墨烯材料的过程中,在电解质溶液中加入分散剂,所述的分散剂的质量百分比浓度为0.05%-1%。
进一步的,所述的分散剂为聚乙二醇、维生素C、或者柠檬酸。
本发明的纳米多孔金具有三维多孔结构,弯曲孔壁和孔的毛细现象可以减少石墨烯材料的聚集和堆叠。采用氧化石墨烯及石墨烯量子点为起始材料,利用循环伏安法可实现单层石墨烯或单颗粒石墨烯量子点的沉积。形成单分子分散的复合电极材料。
本发明的纳米多孔金具有良好的导电性,以三维多孔结构为特征,可提高比表面积。石墨烯材料沉积在纳米多孔金表面,仍保留纳米多孔金的三维连续孔隙结构,多孔结构允许电解质离子在复合结构中发生快速扩散和转移,从而在电极材料表面进行可逆的吸附与解吸,进而大幅度提高电极材料的比电容和充放电速率。
本发明通过控制循环次数、循环速率和电压来控制石墨烯材料在NPG薄膜上的沉积量及分布。上述所得的石墨烯/纳米多孔金复合结构超级电容器电极材料,由于具有良好的能量储存能力、高比电容和良好的循环稳定性,因此可作为高效、轻质的复合电极材料。
本发明的超级电容器电极材料,由于负载石墨烯材料,利用微小粒子间相互作用力完成界面扩散和结合,使其具有良好的结构稳定性。同时由于纳米多孔金和石墨烯之间的协同效应使复合材料电极拥有比单纯石墨烯和纳米多孔金更大的比电容。
本发明和已有技术相比,其技术进步是显著的。本发明所制备的超级电容器电极材料具有高比电容以及良好的结构稳定性、循环稳定性。比电容高达864 F/g,循环2000次仍保持90%的比电容。适用于高稳定性、高功率密度的电源场合。本发明是在纳米多孔金表面沉积石墨烯材料,实现了孔隙率高、有效比表面积大和低的离子迁移电阻,解决了石墨烯基电极材料技术难题。而且本发明的方法工艺简单,结构可控、绿色环保。
附图说明
图1是实施例1所制备的石墨烯量子点/纳米多孔金复合材料的TEM图。
图2是实施例1所得石墨烯量子点/纳米多孔金复合电极材料在0.5 M Na2SO4溶液中的循环伏安曲线。
图3是实施例2所制备的氧化石墨烯/纳米多孔金复合材料的TEM图。
图4是实施例2所得氧化石墨烯/纳米多孔金复合电极材料在0.5 M Na2SO4溶液中的循环伏安曲线。
图5是实施例3所得氮掺杂石墨烯量子点/纳米多孔金复合结构材料的TEM图。
图6是实施例3所得氮掺杂石墨烯量子点/纳米多孔金复合结构材料的成分测定EDX图。
具体实施方式
下面通过具体实施例并结合附图对本发明进一步阐述,下面的阐述仅是为了解释本发明的优点和技术方案,并不对本发明进行限定。
实施例1
石墨烯量子点/纳米多孔金复合结构超级电容器电极材料,其通过如下步骤的方法制备而成:
(1)取纳米多孔金薄膜,用去离子水清洗两遍,用铜片取出。
(2)将NPG薄膜置于石墨烯量子点水溶液中,浓度为0.02g/L,加入质量浓度为0.05%PEG。采用三电极***,利用循环伏安法沉积石墨烯量子点,电压窗口为0-1V电压,循环次数50次,扫描速率20mVs-1。即得石墨烯量子点/纳米多孔金复合结构超级电容器电极材料。
采用透射电子显微镜对上述石墨烯量子点/纳米多孔金复合材料进行测试,见附图1。从图1可以看出,石墨烯量子点呈球形单颗粒分布在纳米多孔金孔壁上,颗粒大小为3-8nm。纳米多孔金薄膜多孔分布均匀,负载石墨烯量子点后仍保留有三维连续孔隙结构。
对上述所得的石墨烯量子点/纳米多孔金复合材料进行电容性能测试,以石墨烯量子点/纳米多孔金为工作电极,以饱和甘汞电极为参比电极,以铂片为对电极,以0.5M的Na2SO4溶液为电解液,测电容曲线结果如图2所示。比电容达到823 F/g。功率密度达228 kW/kg。循环3000次后比电容仍保持90%以上。
实施例2
氧化石墨烯/纳米多孔金复合结构超级电容器电极材料,其通过如下步骤的方法制备而成:
(1)取纳米多孔金薄膜,用去离子水清洗两遍,用铜片取出。
(2)将NPG薄膜置于氧化石墨烯水溶液中,浓度为0.5g/L。采用三电极***,利用循环伏安法沉积氧化石墨烯材料,电压窗口为0-2V电压,循环次数500次,扫描速率200mVs-1。即得氧化石墨烯/纳米多孔金复合结构超级电容器电极材料。
(3)所制备的氧化石墨烯/纳米多孔金复合结构超级电容器电极材料在500oC,热处理120分钟。
采用透射电子显微镜对上述氧化石墨烯/纳米多孔金复合材料进行测试,见附图3。从图3可以看出,石墨烯呈片层结构沉淀在纳米多孔金表面。纳米多孔金薄膜多孔分布均匀,负载氧化石墨烯后仍保留有三维连续孔隙结构。
对上述所得的氧化石墨烯/纳米多孔金复合材料进行电容性能测试,以氧化石墨烯/纳米多孔金为工作电极,以饱和甘汞电极为参比电极,以铂片为对电极,以0.5M的Na2SO4溶液为电解液,在该三电极体系下的循环伏安法测电容曲线结果如图4所示。比电容达到423 F/g。功率密度达59 kW/kg。循环4000次后比电容仍保持90%以上。
实施例3
氮掺杂石墨烯量子点/纳米多孔金复合结构超级电容器电极材料,其通过如下步骤的方法制备而成:
(1)取纳米多孔金薄膜,用去离子水清洗两遍,用铜片取出。
(2)将NPG薄膜置于氮掺杂石墨烯量子点水溶液中,浓度为0.1g/L,加入质量浓度为0.05%维生素C。采用三电极***,利用循环伏安法沉积石墨烯量子点,电压窗口为0-1.6V电压,循环次数200圈,扫描速率100mVs-1。即得氮掺杂石墨烯量子点/纳米多孔金复合结构超级电容器电极材料。
采用透射电子显微镜对上述氮掺杂石墨烯量子点/纳米多孔金复合材料进行测试,见附图5。从图5可以看出,氮掺杂石墨烯量子点呈球形单颗粒分布在纳米多孔金孔壁上,颗粒大小为4-9nm。纳米多孔金薄膜多孔分布均匀,负载氮掺杂石墨烯量子点后仍保留有三维连续孔隙结构。氮掺杂石墨烯量子点/纳米多孔金样品表面EDX成分测定结果见附图6。其中,掺杂N含量为2.6%。
对上述所得的氮掺杂石墨烯量子点/纳米多孔金复合材料进行电容性能测试,以氮掺杂石墨烯量子点/纳米多孔金为工作电极,以饱和甘汞电极为参比电极,以铂片为对电极,以0.5M的Na2SO4溶液为电解液,测得的比电容达到864 F/g。功率密度达120 kW/kg。循环2000次后比电容仍保持90%以上。
实施例4
氮掺杂石墨烯/纳米多孔金复合结构超级电容器电极材料,其通过如下步骤的方法制备而成:
(1)取纳米多孔金薄膜,用去离子水清洗两遍,用铜片取出。
(2)将NPG薄膜置于氮掺杂石墨烯水溶液中,浓度为0.3g/L。采用三电极***,利用循环伏安法沉积氮掺杂石墨烯,电压窗口为0-1V电压,循环次数600次,扫描速率50mVs-1。即得氮掺杂石墨烯/纳米多孔金复合结构超级电容器电极材料。
(3)所制备的氮掺杂石墨烯/纳米多孔金复合结构超级电容器电极材料在200oC,热处理30分钟。
对上述所得的氮掺杂石墨烯/纳米多孔金复合材料进行电容性能测试,以氮掺杂石墨烯/纳米多孔金为工作电极,以饱和甘汞电极为参比电极,以铂片为对电极,以0.5M的Na2SO4溶液为电解液,测得的比电容达到514 F/g。功率密度达71 kW/kg。循环2000次后比电容仍保持90%以上。
上述内容仅为本发明构思下的基本说明,而依据本发明的技术方案所作的任何等效变换,均应属于本发明的保护范围。
Claims (6)
1.一种石墨烯超级电容器电极材料的制备方法,其特征在于:在纳米多孔金薄膜表面沉积石墨烯材料,所述的沉积方法采用电化学循环伏安法,所述的石墨烯材料的浓度为0.02g/L-0.5g/L,在采用电化学循环伏安法沉积石墨烯材料的过程中,沉积窗口为0-2V电压,循环次数50-600次,扫描速率10-200mVs-1。
2.如权利要求1所述的一种石墨烯超级电容器电极材料的制备方法,其特征在于:所述石墨烯材料选自氧化石墨烯、石墨烯量子点、氮掺杂石墨烯或者氮掺杂石墨烯量子点。
3.如权利要求2所述的一种石墨烯超级电容器电极材料的制备方法,其特征在于:石墨烯或者氮掺杂石墨烯为单层或者多层氧化石墨烯;石墨烯量子点或氮掺杂石墨烯量子点颗粒大小为2-10nm。
4.如权利要求1所述的一种石墨烯超级电容器电极材料的制备方法,其特征在于:还包括一个对超级电容器电极材料进行热处理的过程,热处理温度为100-500oC,热处理时间20-120分钟。
5.如权利要求1所述的一种石墨烯超级电容器电极材料的制备方法,其特征在于:在采用电化学循环伏安法沉积石墨烯材料的过程中,在电解质溶液中加入分散剂,所述的分散剂的质量百分比浓度为0.05%-1%。
6.如权利要求5所述的一种石墨烯超级电容器电极材料的制备方法,其特征在于:所述的分散剂为聚乙二醇、维生素C、或者柠檬酸。
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CN113643905A (zh) * | 2021-08-23 | 2021-11-12 | 武夷学院 | 石墨烯接枝聚合物电极材料的制备方法及其用途 |
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