CN107910201B - 一种层状复合材料的制备方法 - Google Patents
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Abstract
本发明提供了一种层状复合材料的制备方法,首先利用水热法制备石墨烯量子点;然后按体积比例称取前驱体溶液:硝酸钴溶液、石墨烯量子点溶液、去离子水,混合均匀,并将所得液转入反应釜中,在160~200℃烘箱中反应12~24 h,抽滤、洗涤、干燥即可得到石墨烯量子点/CoCo2O4层状材料。本发明方法简单,成本低,生产周期短,且获得的层状复合材料具有大的比表面积,高的化学稳定性,良好的电化学性能,最高比电容可达400F/g,循环1000次后,比电容仍然保持原来的93%,在超级电容器、离子电池的电极材料和锂‑空气电池的电催化剂方面具有潜在的应用价值。
Description
技术领域
本发明属于材料学领域,涉及一种层状复合材料,具体来说是一种石墨烯量子点/CoCo2O4层状复合材料的制备方法。
背景技术
随着科学技术的发展,环境和能源问题愈加突出,研究开发清洁和可再生的新型能源材料及其器件已经迫在眉睫。超级电容器作为一种高效、清洁、可持续的能源设备,受到广泛关注。超级电容器主要结构包括电极活性材料、隔膜、电解液和集流体等。其中电极材料是超级电容器的主要组成部分,直接决定超级电容器输出性能的高低。现在常用的电极材料分为碳质材料、金属氧化物、导电聚合物及复合材料四类。
石墨烯量子点( GQDs)是准零维的碳纳米材料,具有小尺寸组装优势、高比表面积、高导电性、高的化学稳定性、丰富的官能团、优良的溶剂分散性。这些优点使之成为优越的高活性物质,用于各种高功率密度、高能量密度和循环寿命长的微型电容器的电极材料具有很好的发展前景。然而,已报道结果表明石墨烯量子点应用于双电层电容器,面容量依然很低且量子点之间易团聚,这将限制石墨烯量子点在高容量超级电容器上的应用。其中在过渡金属氧化物中,钴的氧化物,如CoO、Co3O4、尖晶石型CoCo2O4,因具备成本低廉、资源相对丰富、理论比容量高等优点,近几年成为超级电容器领域电极材料的研究热点。虽然金属氧化物具有良好的电化学性能,但是存在电导率低的缺点。为了克服以上两类单一材料存在的不足,所以研究者将其与碳质材料进行复合,利用各组分之间的协同效应提高超级电容器的综合性能。
目前,在专利CN105632787A中公开了一种四氧化三钴/石墨烯纳米复合超级电容器电极材料的制备方法,所述复合材料电化学性能良好,比电容有所提高,但是制备工艺复杂,需要高温反应,消耗能源,不适合工业化生产。
在专利CN104393283A中公开了一种纳米晶状CoO-石墨烯复合材料的制备方法,所述复合材料,结构稳定,电化学性能较好,但是制备条件苛刻,周期较长,难以应用到实际中。然而,关于石墨烯量子点与层状氧化物CoCo2O4的复合材料还未见报道。
发明内容
针对现有技术中的上述技术问题,本发明提供了一种层状复合材料的制备方法,所述的这种层状复合材料的制备方法要解决现有技术中制备层状复合材料的工艺复杂、生产周期长比电容较低的技术问题。
本发明提供了一种层状复合材料的制备方法,包括如下步骤:
1) 一个制备石墨烯量子点的步骤,先利用Hummers法制备出氧化石墨烯,再将氧化石墨烯超声分散于N,N-二甲基甲酰胺中,氧化石墨烯和N,N-二甲基甲酰胺的物料比为0.2~0.4g:20 mL,形成均匀混合液,然后将所得混合液转入反应釜,180~220℃保持6~10h,最后冷却,再采用0.22μm的微孔滤膜抽滤,得到滤液,在80~100℃下蒸干,即可得到石墨烯量子点;
2)称取前驱体溶液硝酸钴溶液、石墨烯量子点溶液和去离子水,所述的前驱体溶液硝酸钴溶液、石墨烯量子点溶液和去离子水的体积比为10~20mL:4 mL:1 mL,将前驱体溶液硝酸钴溶液、石墨烯量子点溶液和去离子水混合;然后搅拌均匀,转入水热釜中,在160~200 ℃烘箱中反应12~24 h,抽滤、洗涤、干燥即可得到石墨烯量子点/CoCo2O4层状复合材料。
进一步的,所述前驱体溶液硝酸钴溶液浓度为0.02 mol/L,所述的石墨烯量子点溶液浓度为0.1 g/L。
本发明先制备出石墨烯量子点,再利用简单的水热法即可合成石墨烯量子点/CoCo2O4层状复合材料。所述复合材料利用石墨烯量子点高的导电性、CoCo2O4片层状可增加电极的比表面积及电荷的传导速率,以及两者的协同效应三方面有效提高复合电极的比电容。
本发明利用简单的水热法,制备出石墨烯量子点/CoCo2O4层状复合材料。这种复合材料将典型的碳质材料和过渡金属氧化物材料耦合,石墨烯量子点具有大的比表面积,优异的导电性,可大大增加对活性物质的利用率;二维层状材料CoCo2O4具有大范围规整、稳定和顺畅的电荷传导路径,复合材料兼具两者优势,协同发挥电化学性能,从而有效增加电极的比容量和高倍率特性。
本发明可用于超级电容器和离子电池的电极材料,锂-空气电池的电催化剂。此类电极材料具有较好的电化学性能,电流阻抗小,循环稳定性高,最高比电容可达400 F/g,循环1000次后,比电容仍然保持原来的93%。
本发明利用水热法制备一种石墨烯量子点/CoCo2O4层状复合材料,即采用简单的合成技术制备具有优越性能的超级电容器电极材料。克服了两种单一电极材料在超级电容器应用方面上的不足,充分发挥碳材料以及过渡金属氧化物的协同作用,优势相互结合,缺陷相互减弱,极大地提高了材料的电化学性能。
本发明和已有技术相比,其技术进步是显著的。本发明的石墨烯量子点/CoCo2O4复合材料,利用水热法即可完成,操作性强,制备工艺简单可控,设备要求低,制备周期短,原料成本低廉,适合工业化生产。所得复合材料具有良好的循环性能和高比电容量,满足超级电容器电极材料的要求,是一种理想的超级电容器电极材料。在超级电容器、离子电池的电极材料和锂-空气电池的电催化剂方面具有潜在的应用价值。
附图说明
图1是实施例1所得石墨烯量子点/CoCo2O4层状复合材料的XRD图。
具体实施方式
实施例1
1)一个制备石墨烯量子点的步骤,先利用Hummers法制备出氧化石墨烯(GO),再将0.27g GO超声分散于20 mL N,N-二甲基甲酰胺中,形成均匀混合液,然后将所得混合液转入30 mL反应釜,200℃保持8 h,最后冷却、抽滤(0.22μm微孔滤膜),得到滤液,在80℃下蒸干,即可得到石墨烯量子点;
2)一个制备石墨烯量子点/CoCo2O4层状复合材料的步骤,
按照前驱体溶液硝酸钴溶液:石墨烯量子点溶液:去离子水的体积比为(10~20)mL:4 mL:1 mL,称取原料;然后搅拌均匀,转入50 mL水热釜中,在160 ℃烘箱中反应12h,抽滤、洗涤、干燥即可得到石墨烯量子点/CoCo2O4层状材料;所述前驱体溶液硝酸钴溶液浓度为0.02 mol/L,所述的石墨烯量子点溶液浓度为0.1 g/L。
利用CHI660E型号电化学工作站测试样品的电化学性能。以恒电流充电−放电方法在0.5Ag-1电流密度下,测得比电容为400 Fg-1。
实施例2
1)一个制备石墨烯量子点的步骤,先利用Hummers法制备出氧化石墨烯(GO),再将0.27g GO超声分散于20 mL N,N-二甲基甲酰胺中,形成均匀混合液,然后将所得混合液转入30 mL反应釜,200℃保持8 h,最后冷却、抽滤(0.22μm微孔滤膜),得到滤液,在80℃下蒸干,即可得到石墨烯量子点;
2) 一个制备石墨烯量子点/CoCo2O4层状复合材料的步骤,
按照前驱体溶液硝酸钴溶液:石墨烯量子点溶液:去离子水的体积比为(10~20)mL:4 mL:1 mL,称取原料;然后搅拌均匀,转入50 mL水热釜中,在180 ℃烘箱中反应12 h,抽滤、洗涤、干燥即可得到石墨烯量子点/CoCo2O4层状材料;所述前驱体溶液硝酸钴溶液浓度为0.02 mol/L,所述的石墨烯量子点溶液浓度为0.1 g/L。
利用CHI660E型号电化学工作站测试样品的电化学性能。以恒电流充电−放电方法在0.5Ag-1电流密度下,测得比电容为380Fg-1。
实施例3
1) 一个制备石墨烯量子点的步骤,先利用Hummers法制备出氧化石墨烯(GO),再将0.27g GO超声分散于20 mL N,N-二甲基甲酰胺中,形成均匀混合液,然后将所得混合液转入30 mL反应釜,200℃保持8 h,最后冷却、抽滤(0.22μm微孔滤膜),得到滤液,在80℃下蒸干,即可得到石墨烯量子点;
2)一个制备石墨烯量子点/CoCo2O4层状复合材料的步骤,
按照前驱体溶液硝酸钴溶液:石墨烯量子点溶液:去离子水的体积比为(10~20)mL:4 mL:1 mL,称取原料;然后搅拌均匀,转入50 mL水热釜中,在200℃烘箱中反应12 h,抽滤、洗涤、干燥即可得到石墨烯量子点/CoCo2O4层状材料;所述前驱体溶液硝酸钴溶液浓度为0.02 mol/L,所述的石墨烯量子点溶液浓度为0.1 g/L。
利用CHI660E型号电化学工作站测试样品的电化学性能。以恒电流充电−放电方法在0.5Ag-1电流密度下,测得比电容为350Fg-1。
Claims (2)
1.一种层状复合材料的制备方法,其特征在于包括如下步骤:
1)一个制备石墨烯量子点的步骤,先利用Hummers法制备出氧化石墨烯,再将氧化石墨烯超声分散于N,N-二甲基甲酰胺中,氧化石墨烯和N,N-二甲基甲酰胺的物料比为0.2~0.4g:20 mL,形成均匀混合液,然后将所得混合液转入反应釜,180~220℃保持6~10h,最后冷却,再采用0.22μm的微孔滤膜抽滤,得到滤液,在80~100℃下蒸干,即可得到石墨烯量子点;
2)称取前驱体溶液硝酸钴溶液、石墨烯量子点溶液和去离子水,所述的前驱体溶液硝酸钴溶液、石墨烯量子点溶液和去离子水的体积比为10~20mL:4 mL:1 mL,将前驱体溶液硝酸钴溶液、石墨烯量子点溶液和去离子水混合;然后搅拌均匀,转入水热釜中,在160~200℃烘箱中反应12~24 h,抽滤、洗涤、干燥即可得到石墨烯量子点/CoCo2O4层状复合材料。
2.根据权利要求1所述的一种层状复合材料的制备方法,其特征在于:所述前驱体溶液硝酸钴溶液浓度为0.02 mol/L,所述的石墨烯量子点溶液浓度为0.1 g/L。
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