CN106898493A - 中空核壳NiCo2O4‑RGO柔性超电材料的制备方法 - Google Patents
中空核壳NiCo2O4‑RGO柔性超电材料的制备方法 Download PDFInfo
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
本发明涉及超级电容器技术领域,特指一种以Ni(NO3)2·6H2O、Co(NO3)2·6H2O,甘油,异丙醇和氧化石墨烯为原料来制备中空核壳NiCo2O4‑RGO柔性超电材料,是一种制备工艺简单,成本低廉的方法。本发明采用中空核壳结构的NiCo2O4和GO材料,通过真空抽滤法首次制备了NiCo2O4‑RGO三明治结构复合材料,一方面中空核壳结构的NiCo2O4具有较大的比表面积,且空心结构更利于电解液体的渗进及转移,另一方面NiCo2O4球形结构也可以支撑开层层石墨烯之间的间距,为电解液体的流通提供了通道并可以加速电解质在材料内部的流动。这种结构的构筑可以有效的提高材料的电化学性能。
Description
技术领域
本发明涉及超级电容器技术领域,特指一种以Ni(NO3)2·6H2O、Co(NO3)2·6H2O,甘油,异丙醇和氧化石墨烯为原料来制备中空核壳NiCo2O4-RGO柔性超电材料,是一种制备工艺简单,成本低廉的方法。
背景技术
随着便携式和柔性电子产品的逐渐推广,开发具有柔韧性、高性能和轻质的二维电极材料有非常重要的现实意义。柔性电子设备也将是未来电子器件的新兴领域,它能够嵌入柔性基体内,承受一定的形变而不引起容量的大幅度衰减。
石墨烯具有良好的机械性能和导电性,是理想的二维柔性自支撑电极材料。将石墨烯抽滤成膜直接用于自支撑柔性导电基体是最常用的方法,这种方法制备条件简单温和,适合大规模生产,但是石墨稀片层中间由于范德华力的存在,片与片之间紧密堆积,这样导致有效利用表面积降低,电解液的传输也会受到一定的限制。因此,通常在石墨稀中同添加一些活性物质。近年来,多元过渡金属氧化物由于自身优异的物理,化学性能,是目前超级电容器电极材料的一个研究热点。尖晶石型NiCo2O4作为多元过渡金属氧化物的一种,具有理论比容高、电化学可逆性好和环境友好等特点,近年来引起了人们的广泛关注。至今为止,不同形貌的NiCo2O4已经被制备出来应用于超级电容器的研究,例如纳米片,微米球,纳米线等等。而在这些结构中,中空核壳球由于其低密度,较大的比表面积以及较好的渗透性可以明显的提高NiCo2O4的电化学性能。
本发明采用真空抽滤法成功制备了中空核壳NiCo2O4-RGO薄膜柔性材料,所制备的NiCo2O4-RGO材料在环境、能源等领域有良好应用前景。
发明内容
本发明目的是提供一种真空抽滤法制备中空核壳NiCo2O4-RGO柔性材料。
本发明通过以下步骤实现:
(1)将Ni(NO3)2·6H2O和Co(NO3)2·6H2O混合于异丙醇中,并加入一定量的甘油,在180℃条件加热一定的时间,之后冷却至室温,用乙醇洗涤6遍后干燥,得到Ni-Co前驱体,随后将Ni-Co前驱体置于马弗炉中400℃煅烧一定的时间,获得NiCo2O4中空核壳球。
所述的Ni(NO3)2·6H2O和Co(NO3)2·6H2O的摩尔比为1:2,异丙醇和甘油的体积比为5:1,每升异丙醇中加入6.25mmol的Co(NO3)2·6H2O,且加热时间为6h;马弗炉煅烧时间为2小时,且升为速率为1℃/min。
(2)氧化石墨烯(GO)通过Hummer方法制备。
(3)将NiCo2O4和GO粉末分别配制成一定浓度的溶液后,分别取一定量进行混合,随后通过真空抽滤装置将其抽滤成NiCo2O4-GO薄膜柔性材料。
所述的NiCo2O4溶液和GO溶液的浓度分别为0.5毫克/毫升和0.2毫克/毫升,取出的NiCo2O4和GO质量比为1:1-3。
(4)将NiCo2O4-GO薄膜柔性材料通过水热法将GO还原为RGO。
所述的水热温度为180℃,时间为8小时。
(5)本发明采用中空核壳结构的NiCo2O4和GO材料,通过真空抽滤法首次制备了NiCo2O4-RGO三明治结构复合材料,一方面中空核壳结构的NiCo2O4具有较大的比表面积,且空心结构更利于电解液体的渗进及转移,另一方面NiCo2O4球形结构也可以支撑开层层石墨烯之间的间距,为电解液体的流通提供了通道并可以加速电解质在材料内部的流动。这种结构的构筑可以有效的提高材料的电化学性能。
(6)利用X-射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、电子透射显微镜(TEM),X光电子能谱仪(XPS)等仪器对产物进行形貌结构分析等仪器对产物进行形貌结构分析,并通过电化学工作站对其进行了测试,以评估其电化学性能。
本发明采用本发明目的是提供一种真空抽滤法制备中空核壳NiCo2O4-RGO柔性材料,所制备NiCo2O4-RGO柔性材料在能源转换领域有良好的应用,这种三明治结构的材料增大了比表面积,加速了电解质在材料内部的流动,进而显示出较优异的电化学性能。
附图说明
图1为所制备的中空核壳NiCo2O4-RGO柔性材料的XRD衍射谱图。
图2为所制备中空核壳NiCo2O4扫描和透射电镜图。
图3为所制备的中空核壳NiCo2O4-RGO柔性材料的场发射扫描电镜图。
图4为所制备中空核壳NiCo2O4-RGO柔性材料的XPS图。
图5为所制备中空核壳NiCo2O4-RGO(1:1,1:2,1:3)柔性材料的循环伏安曲线图。
图6a-b为所制备空心中空核壳NiCo2O4-RGO(1:2)柔性材料的横流充放电曲线图,图6c为能量密度以及功率密度计算值,图6d为循环实验图。
具体实施方式
实施例1中空核壳NiCo2O4-RGO柔性材料的制备
0.25毫摩尔的Co(NO3)2·6H2O和0.125毫摩尔Ni(NO3)2·6H2O的溶解在40毫升的异丙醇中,在8毫升的甘油加入到上述溶液中搅拌30分钟;随后,将得到的混合液转移到100毫升不锈钢高压釜中,在180℃条件下反应6小时。将得到的沉淀物(Ni-Co前驱体)通过离心收集,用无水乙醇洗涤6次,在60℃条件下干燥12小时。最后将获得的Ni-Co前驱体置于马弗炉中400℃煅烧2小时,升温速率为1℃/min,最终获得NiCo2O4中空核壳球材料。氧化石墨烯(GO)通过通过Hummer方法制备。将制备好的NiCo2O4和GO粉末分别配制成浓度为0.5毫克/毫升和0.2毫克/毫升的溶液,分别取一定量(NiCo2O4和GO质量比为1:1,1:2和1:3)进行混合,随后通过真空抽滤装置将其抽滤成NiCo2O4-GO薄膜柔性材料。最终将获得的NiCo2O4-GO材料通过水热法180℃,8小时还原为NiCo2O4-RGO薄膜柔性材料。
实施例2中空核壳NiCo2O4-RGO柔性材料的表征分析
如图1所示,从图中可以看出,NiCo2O4与RGO的特征峰均出现在NiCo2O4-RGO的复合材料中,并且通过RGO量的增加,RGO的特征峰逐渐增强。
图2可以观察到,NiCo2O4展现出300-500nm之间的球状结构,并且球体为中空核壳的结构。
图3a-b展示出NiCo2O4与RGO互相混合并且包覆在一起,图3c-d展示类似于三明治结构,说明中空核壳结构的NiCo2O4球成功的撑开了RGO片状的层层结构。
图4的XPS图中可以看出有Ni,Co,O,C元素的存在。
图5可以观察到,在质量比NiCo2O4:RGO=1:2的情况下,中空核壳NiCo2O4-RGO柔性材料的比容量达到最高,在2mV/s的情况下达到1334.1F g-1。
图6a-b展示除中空核壳NiCo2O4-RGO(1:2)柔性材料在1A g-1的电流密度下,容量达到了1414.7F g-1。并且在进行了10000次的循环实验后,容量仍可以保持原有的90.2%。
实施例3中空核壳NiCo2O4-RGO柔性材料的电化学实验
(1)将制备好的NiCo2O4-RGO薄膜剪成面积为一平方厘米的正方形,夹杂在同样大小的两块泡沫镍中间作为工作电极。
(2)将制备好的工作电极与银/氯化银电极,铂片电极在6摩尔/升的KOH电解质中进行电化学测试。
(3)所制备的中空核壳NiCo2O4-RGO柔性材料在1A g-1的电流密度下的比容量达到了1414.7F g-1。
Claims (5)
1.中空核壳NiCo2O4-RGO柔性超电材料的制备方法,其特征在于,具体步骤如下:
(1)将Ni(NO3)2·6H2O和Co(NO3)2·6H2O混合于异丙醇中,并加入甘油,在180℃条件加热后冷却至室温,洗涤后干燥,得到Ni-Co前驱体,随后将Ni-Co前驱体置于马弗炉中煅烧获得NiCo2O4中空核壳球;
(2)氧化石墨烯GO通过Hummer方法制备;
(3)将NiCo2O4和GO粉末分别配制成溶液后进行混合,随后通过真空抽滤装置将其抽滤成NiCo2O4-GO薄膜柔性材料;
(4)将NiCo2O4-GO薄膜柔性材料通过水热法将GO还原为RGO。
2.如权利要求1所述的中空核壳NiCo2O4-RGO柔性超电材料的制备方法,其特征在于,步骤(1)中,所述的Ni(NO3)2·6H2O和Co(NO3)2·6H2O的摩尔比为1:2,异丙醇和甘油的体积比为5:1,每升异丙醇中加入6.25mmol的Co(NO3)2·6H2O,且加热时间为6h;马弗炉煅烧温度为400℃,时间为2小时,且升为速率为1℃/min。
3.如权利要求1所述的中空核壳NiCo2O4-RGO柔性超电材料的制备方法,其特征在于,步骤(1)中,洗涤指用乙醇洗涤6遍。
4.如权利要求1所述的中空核壳NiCo2O4-RGO柔性超电材料的制备方法,其特征在于,步骤(3)中,所述的NiCo2O4溶液和GO溶液的浓度分别为0.5毫克/毫升和0.2毫克/毫升,NiCo2O4和GO质量比为1:1-3。
5.如权利要求1所述的中空核壳NiCo2O4-RGO柔性超电材料的制备方法,其特征在于,步骤(4)中,所述的水热温度为180℃,时间为8小时。
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