CN111430155A - 一种石墨烯/CoOx复合电极的制备方法与应用 - Google Patents
一种石墨烯/CoOx复合电极的制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种石墨烯/CoOx复合电极的制备方法与应用,该复合电极的制备方法,包括以下步骤:(1)将六水合氯化钴与聚酰亚胺溶液混合得到混合物;(2)将混合物涂覆在基底上,烘干后形成复合薄膜;(3)在复合薄膜上设定电极图案;(4)使用激光按照电极图案在复合薄膜上进行雕刻,得到石墨烯/CoOx复合电极;该电极能够应用在超级电容器中。本发明能够直接按照目标电极形状制备出石墨烯/CoOx复合电极,制备方法简单,制备成本低,制备出的石墨烯/CoOx复合电极容量高、导电性好。
Description
技术领域
本发明涉及一种复合电极的制备方法与应用,更具体地,涉及石墨烯/CoOx复合电极的制备方法与应用。
背景技术
氧化钴作为典型的电池型电极材料,有很高的理论容量,优异的氧化还原性,同时相对于Fe、Ni等其他电池型电极材料有很好的稳定性,因此也被认为是非常有前景的超级电容器材料。但由于氧化钴电导率较低,且充放电速率较慢,进而严重阻碍了其在超级电容器的实际应用;石墨烯是由碳原子之间相互连接成六角网络而组成的独特的二维层状结构碳材料,具有较高的导电性和大的比表面积,石墨烯和氧化钴制成的复合材料具有高容量,高电导率,其在电容器领域具有广阔的应用前景。目前石墨烯/氧化钴复合材料的制备方法主要是液相激光辐照/烧蚀法,需要将氧化石墨烯与Co3O4粉末混合,然后再使用激光诱导还原石墨烯,不仅制备成本较高,且在制备成电容器电极时制备方法复杂、难以制备出精确的目标电极形状。
发明内容
发明目的:本发明的目的是提供一种制备方法简单、电极形状精确、制备成本低的石墨烯/CoOx复合电极,本发明的另一目的是提供该复合电极的制备方法,本发明的另一目的是提供该复合电极的应用。
技术方案:本发明所述的石墨烯/CoOx复合电极的制备方法,包括以下步骤:
(1)将六水合氯化钴与聚酰亚胺溶液混合得到混合物;
(2)将混合物涂覆在基底上,烘干后形成复合薄膜;
(3)在复合薄膜上设定电极图案;
(4)使用激光按照电极图案在复合薄膜上进行雕刻,得到石墨烯/CoOx复合电极。
其中,步骤1中六水合氯化钴与聚酰亚胺溶液的质量比为1:20~1:100;步骤2中烘干温度为50~160℃,烘干时间为3~6h,薄膜厚度为50~100μm,基底为柔性基底,柔性基底为柔性聚酰亚胺薄膜。
本发明所述的制备方法制备出的石墨烯/CoOx复合电极在超级电容器中的应用。
有益效果:本发明与现有技术相比,其显著优点是:1、能够直接按照目标电极形状制备出石墨烯/CoOx复合电极,制备方法简单;2、制备成本低;3、制备出的石墨烯/CoOx复合电极容量高、导电性好;4、能够在超级电容器中得到应用。
附图说明
图1是实施例3中石墨烯/CoOx复合电极的扫描电镜图;
图2是实施例3中石墨烯/CoOx复合电极的透射电镜图;
图3是实施例3中石墨烯/CoOx复合电极Co元素的X射线光电子能谱;
图4是实施例3中柔性超级电容器的循环伏安测试图;
图5是实施例3中柔性超级电容器的恒电流充放电测试图;
图6是实施例3中柔性超级电容器在不同弯曲角度下的比电容变化图。
具体实施方式
实施例1
取60g的聚酰亚胺溶液,称取3g的六水合氯化钴,将聚酰亚胺溶液和六水合氯化钴混合均匀得到混合材料,使用涂膜器将混合材料涂覆在柔性聚酰亚胺薄膜上,涂覆的厚度为100μm,将样品在80℃、120℃、160℃下分别烘干0.5h,得到石墨烯/氯化钴复合薄膜,使用绘图软件绘制出插指型电极图样,然后导入Nero Start Smart软件,将激光器功率设置为2.4瓦,波长30微米,利用激光器按照预设的图案对复合薄膜进行雕刻,得到激光诱导石墨烯/CoOx复合电极,在复合电极表面涂覆PVA/H2SO4凝胶电解质,得到柔性超级电容器,在电化学工作站上测试超级电容器的电化学储能特性,计算得到其面积比电容为5.31mF/cm2。
实施例2
取60g的聚酰亚胺溶液,称取1.5g的六水合氯化钴,将聚酰亚胺溶液和六水合氯化钴混合均匀得到混合材料,使用涂膜器将混合材料涂覆在柔性聚酰亚胺薄膜上,涂覆的厚度为100μm,将样品在60℃、100℃、150℃下分别烘干1h,得到石墨烯/CoOx复合薄膜,使用绘图软件绘制出插指型电极图样,然后导入Nero Start Smart软件,将激光器功率设置为2.4瓦,波长30微米,利用激光器按照预设的图案对复合薄膜进行雕刻,得到激光诱导石墨烯/CoOx复合电极,在复合电极表面涂覆PVA/H2SO4凝胶电解质,得到柔性超级电容器,在电化学工作站上测试超级电容器的电化学储能特性,计算得到其面积比电容为7.27mF/cm2。
实施例3
取60g的聚酰亚胺溶液,称取1g的六水合氯化钴,将聚酰亚胺溶液和六水合氯化钴混合均匀得到混合材料,使用涂膜器将混合材料涂覆在柔性聚酰亚胺薄膜上,涂覆的厚度为100μm,将样品在60℃、100℃、150℃下分别烘干1h,得到石墨烯/CoOx复合薄膜,使用绘图软件绘制出插指型电极图样,然后导入Nero Start Smart软件,将激光器功率设置为2.4瓦,波长30微米,利用激光器按照预设的图案对复合薄膜进行雕刻,得到激光诱导石墨烯/CoOx复合电极,从图1可以看出,其表面形态平整,从图2可以看出,CoOx均匀的分布在石墨烯的表面和内部,从图3可以看出,779.7eV和794.9eV的拟合峰对应于Co 2p3+,778.4eV和793.6ev的拟合峰对应Co 2p2+,说明复合电极中存在CoOx,在复合电极表面涂覆PVA/H2SO4凝胶电解质,得到柔性超级电容器,在电化学工作站上测试超级电容器的电化学储能特性,从图4中可以看出,在5mV每秒到80mV每秒的扫描速率下,CV曲线接近矩形,表明该超级电容器具有优异的电容行为和较低接触电阻,在5mV/s的扫描速率下比电容为10.9mF/cm2,从图5可得,恒电流充电和放电曲线的线性轮廓为对称的三角形形状,说明柔性超级电容器接近理想的电容特性,随着扫描速率的增加,充放电时间对应增加。将电容器弯折30~150°,测试其比电容,从图6可以看出,从0-150度,柔性超级电容器的电容一直保持近乎100%,显示出优异的特性,表明其容量不随弯曲角度变化。
实施例4
取60g的聚酰亚胺溶液,称取0.75g的六水合氯化钴,将聚酰亚胺溶液和六水合氯化钴混合均匀得到混合材料,使用涂膜器将混合材料涂覆在柔性聚酰亚胺薄膜上,涂覆的厚度为50μm,将样品在60℃、100℃、150℃下分别烘干1h,得到石墨烯/CoOx复合薄膜,使用绘图软件绘制出插指型电极图样,然后导入Nero Start Smart软件,将激光器功率设置为2.4瓦,波长30微米,利用激光器按照预设的图案对复合薄膜进行雕刻,得到激光诱导石墨烯/CoOx复合电极,在复合电极表面涂覆PVA/H2SO4凝胶电解质,得到柔性超级电容器,在电化学工作站上测试超级电容器的电化学储能特性,计算得到其面积比电容为7.65mF/cm2。
实施例5
取60g的聚酰亚胺溶液,称取0.6g的六水合氯化钴,将聚酰亚胺溶液和六水合氯化钴混合均匀得到混合材料,使用涂膜器将混合材料涂覆在柔性聚酰亚胺薄膜上,涂覆的厚度为100μm,将样品在80℃、120℃、150℃下分别烘干2h,得到石墨烯/CoOx复合薄膜,使用绘图软件绘制出插指型电极图样,然后导入Nero Start Smart软件,将激光器功率设置为2.4瓦,波长30微米,利用激光器按照预设的图案对复合薄膜进行雕刻,得到激光诱导石墨烯/CoOx复合电极,在复合电极表面涂覆PVA/H2SO4凝胶电解质,得到柔性超级电容器,在电化学工作站上测试超级电容器的电化学储能特性,计算得到其面积比电容为5.10mF/cm2。
实施例6
取60g的聚酰亚胺溶液,称取1g的六水合氯化钴,将聚酰亚胺溶液和六水合氯化钴混合均匀得到混合材料,使用涂膜器将混合材料涂覆在柔性聚酰亚胺薄膜上,涂覆的厚度为100μm,将样品在60℃、100℃、150℃下分别烘干2h,得到石墨烯/CoOx复合薄膜,使用绘图软件绘制出插指型电极图样,然后导入Nero Start Smart软件,将激光器功率设置为2.4瓦,波长30微米,利用激光器按照预设的图案对复合薄膜进行雕刻,得到激光诱导石墨烯/CoOx复合电极,在复合电极表面涂覆PVA/H2SO4凝胶电解质,得到柔性超级电容器,在电化学工作站上测试超级电容器的电化学储能特性,计算得到其面积比电容为10.3mF/cm2。
Claims (8)
1.一种石墨烯/CoOx复合电极的制备方法,其特征在于,包括以下步骤:
(1)将六水合氯化钴与聚酰亚胺溶液混合得到混合物;
(2)将混合物涂覆在基底上,烘干后形成复合薄膜;
(3)在复合薄膜上设定电极图案;
(4)使用激光按照电极图案在复合薄膜上进行雕刻,得到石墨烯/CoOx复合电极。
2.根据权利要求1所述的石墨烯/CoOx复合电极的制备方法,其特征在于,所述步骤1中六水合氯化钴与聚酰亚胺溶液的质量比为1:20~1:100。
3.根据权利要求1所述的石墨烯/CoOx复合电极的制备方法,其特征在于,所述步骤2中烘干温度为50~160℃。
4.根据权利要求1所述的石墨烯/CoOx复合电极的制备方法,其特征在于,所述步骤2中烘干时间为1.5~6h。
5.根据权利要求1所述的石墨烯/CoOx复合电极的制备方法,其特征在于,所述步骤2中薄膜厚度为50~100μm。
6.根据权利要求1所述的石墨烯/CoOx复合电极的制备方法,其特征在于,所述步骤2中的基底为柔性基底。
7.根据权利要求6所述的石墨烯/CoOx复合电极的制备方法,其特征在于,所述柔性基底为柔性聚酰亚胺薄膜。
8.一种权利要求1~7所述的制备方法制得的石墨烯/CoOx复合电极在超级电容器中的应用。
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CN114974936A (zh) * | 2022-06-24 | 2022-08-30 | 安徽格兰科新材料技术有限公司 | 高赝电容负载量的石墨烯超级电容器复合电极的制备方法 |
CN114974936B (zh) * | 2022-06-24 | 2023-09-08 | 安徽格兰科新材料技术有限公司 | 高赝电容负载量的石墨烯超级电容器复合电极的制备方法 |
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