CN105140497A - 一种石墨烯/铜复合电极材料的应用 - Google Patents
一种石墨烯/铜复合电极材料的应用 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000010949 copper Substances 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 57
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 7
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/362—Composites
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/04—Processes of manufacture in general
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
本发明涉及一种石墨烯/铜复合电极材料的应用,属于新能源材料的开发与研究领域。本发明通过一步电沉积法在金属铜表面自组装一层石墨烯活性物质,然后在充满高纯氩气的手套箱内与锂箔组装成扣式模拟锂离子电池,并以恒流充/放电的方法测试其充/放电性能及循环稳定性能。本发明通过自组装方法使金属铜与石墨烯活性物质巧妙而紧密地结合在一起,该电极材料不仅比表面积大,而且与铜集流体结合紧密,有助于减小接触电阻。与传统涂覆式电极制备工艺相比,该工艺操作简单,环境友好,易于放大,且有助于缓解活性物质在长期充/放电过程中的脱落现象,并提高了锂离子电池的充/放电性能与循环稳定性能。
Description
技术领域
本发明涉及一种石墨烯/铜复合电极材料的应用,属于新能源材料的开发与研究领域。
背景技术
锂离子电池是一种高效率、高能量密度的绿色储能装置,已经被广泛应用于可移动电子设备。电极材料是锂离子电池的关键部件之一,与锂离子电池的性能休戚相关,是研究热点之一。
石墨烯是一种新型功能碳材料,独特而完美的二维结构赋予了其超高的机械强度、导热导电性能及比表面积,在太阳能电池、超级电容器、燃料电池等领域具有极其诱人的应用前景。用作锂离子电池负极材料时,不仅具有储锂活性,而且可以降低电荷转移电阻,增加锂离子扩散系数,并最终提高锂离子电池的充/放电性能。
传统锂离子电池的电极制备工艺通常为物理涂抹工艺,即将活性物质与导电剂、粘结剂以一定比例均匀混合成电极浆料并涂覆在集流体表面。基于传统工艺制备的电极在长期循环充/放电过程中,往往因为活性物质与集流体之间结合不够紧密而脱落,并降低电极的循环充/放电寿命,因此有必要开发新型电极制备工艺。与传统电极制备工艺相比,采用原位自组装法制备的电极材料具有如下优点:1)活性物质前驱体在金属集流体表面被电还原、沉积,与金属集流体结合强度高;2)省去了单独合成、处理、加工活性物质等多重工序,工艺简单,成本较低。目前文献中关于锂离子电池石墨烯电极多采用传统工艺制备而成,而利用原位自组装工艺制备电极的报道还比较少。
发明内容
本发明的目的在于提供石墨烯/铜复合电极材料的应用,具体的,将石墨烯/铜复合电极材料用作锂离子电池的工作电极,其中对电极电极、参比电极、隔膜、电解液均为本领域制备锂离子电池过程中的常规选择。
优选的,本发明所述石墨烯/铜复合电极材料在制备锂离子电池时,可以无需添加额外的导电剂和粘结剂。
优选的,本发明采用一步电沉积法在金属铜集流体表面原位自组装石墨烯材料得到石墨烯/铜复合电极材料,具体包括以下步骤:以金属铜为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,以pH值为3~8的氧化石墨烯悬浮液为电解液,采用一步电沉积法在铜表面自组装石墨烯,得到石墨烯/铜复合电极材料。
优选的,电解液中氧化石墨烯悬浮液的浓度为1~5mg/ml。
优选的,一步电沉积的沉积时间为0.5~2.5h。
优选的,一步电沉积的沉积电位为-0.8~-2.5V。
优选的,所述金属铜为铜箔、泡沫铜或铜纳米线。
借助扫描电子显微镜(SEM)、X射线能量色散光谱仪(EDX)、显微拉曼光谱仪以及交流阻抗技术对所制备的石墨烯/Cu复合电极材料进行表征,如图1、图2、图3及图4所示。这些结果清楚地表明了所得到的样品确实石墨烯/铜复合电极材料。
本发明的优点与效果:
本发明中,通过一步电沉积法在金属铜集流体表面原位自组装石墨烯电极活性物质,得到石墨烯/Cu复合电极材料;制备工艺简单,易于批量生产;复合材料中石墨烯的比表面积大,与金属铜集流体结合牢固,无需添加额外的导电剂和粘结剂,直接用作锂离子电池电极材料时,具有高储锂活性,高电导率以及高机械强度等诸多优点,有利于锂离子的可逆脱/嵌过程,提高了复合电极充/放电性能及循环稳定性能;复合电极的首次放电比容量为828mAh/g,并且随着电极的逐步活化,电极的放电比容量将逐渐增大,经过68次循环充放电后,电极的放电比容量为1335mAh/g。
附图说明
图1为实施例1所制备的复合电极材料石墨烯/Cu的SEM图;
图2为实施例2所制备的复合电极材料石墨烯/Cu的EDX图;
图3为实施例3所制备的复合电极材料石墨烯/Cu的拉曼光谱图;
图4为实施例4沉积石墨烯前后复合电极材料的交流阻抗谱图;
图5为实施例5所制备的复合电极材料石墨烯/Cu的充/放电曲线;
图6为实施例5所制备的复合电极材料石墨烯/Cu的循环稳定性曲线。
具体实施方式
下面结合附图和具体实施例对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1
利用稀氢氧化钾溶液将0.5mg/ml的酸性氧化石墨烯电解液的(pH值调节为3),以铜箔为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,恒压(-2.5V)沉积2.5h,冲洗干净并真空干燥后,在铜箔上自组装石墨烯材料,得到石墨烯/Cu复合电极材料,如图1所示,铜箔集流体表面上覆盖了一层薄而透明的绉纱状石墨烯薄膜。
然后直接以所制备的石墨烯/Cu复合材料为工作电极,以锂箔为对电极和参比电极,以Celgard2500膜为隔膜,以含1mol/LLiPF6的碳酸乙烯酯(EC)、碳酸二乙酯(DEC)和碳酸二甲酯(DMC)的混合液为电解液,其中EC、DEC和DMC的体积比为1:1:1,然后在充满高纯氩气的手套箱内与锂箔组装成扣式模拟锂离子电池,并以恒流充/放电的方法测试其充/放电性能及循环稳定性能。
实施例2
利用稀氢氧化钠溶液将1mg/ml的酸性氧化石墨烯电解液(pH=3),以泡沫铜集流体为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,恒压(-1.5V)沉积1h,冲洗干净并真空干燥后,在铜箔上自组装石墨烯材料,得到石墨烯/Cu复合电极材料,如图2所示,样品除了Cu元素之外,还清晰地显示出了与C元素相对应的峰,表明了石墨烯的存在。
然后直接以所制备的石墨烯/Cu复合材料为工作电极,以锂箔为对电极和参比电极,以Celgard2325膜为隔膜,以含1mol/LLiPF6的碳酸乙烯酯(EC)和碳酸二乙酯(DEC)的混合液为电解液,其中EC和DEC的体积比为1:1,然后在充满高纯氩气的手套箱内与锂箔组装成扣式模拟锂离子电池,并以恒流充/放电的方法测试其充/放电性能及循环稳定性能。
实施例3
利用稀氢氧化钾溶液将2.5mg/ml的酸性氧化石墨烯电解液(pH值调节为7),以铜纳米线为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,电极恒压(-1.8V)电化学还原0.5h,冲洗干净并真空干燥后,在铜箔上自组装石墨烯材料,得到石墨烯/Cu复合电极材料。
然后直接以所制备的石墨烯/Cu复合材料为工作电极,以Celgard2400膜为隔膜,以含1mol/LLiPF6的碳酸乙烯酯(EC)、碳酸二乙酯(DEC)和碳酸二甲酯(DMC)的混合液为电解液,其中EC,DEC和DMC的体积之比为1:1:1,然后在充满高纯氩气的手套箱内与锂箔组装成扣式模拟锂离子电池,并以恒流充/放电的方法测试其充/放电性能及循环稳定性能。
实施例4
利用稀氢氧化钠溶液将5mg/ml的酸性氧化石墨烯电解液(pH值调节为8),以铜箔为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,恒压(-0.8V)电沉积0.8h,冲洗干净并真空干燥后,在铜箔上自组装石墨烯材料,得到石墨烯/Cu复合电极材料,如图4所示,由图可知,与纯的铜片电极相比,石墨烯/Cu复合电极的电阻有所降低,表明石墨烯的沉积改善了电极的导电能力。
然后直接以所制备的石墨烯/Cu复合材料为工作电极,以锂箔为对电极和参比电极,以Celgard2500膜为隔膜,以含1mol/LLiPF6的碳酸乙烯酯(EC)、碳酸二乙酯(DEC)的混合液为电解液,其中EC与DEC的体积之比为1:1,然后在充满高纯氩气的手套箱内与锂箔组装成扣式模拟锂离子电池,并以恒流充/放电的方法测试其充/放电性能及循环稳定性能。
实施例5
利用稀氢氧化钠溶液将0.5mg/ml的酸性氧化石墨烯电解液(pH值调节为7),以铜箔为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,恒压(-1.0V)沉积2.3h,冲洗干净并真空干燥后,在铜箔上自组装石墨烯材料,得到石墨烯/Cu复合电极材料。
然后直接以所制备的石墨烯/Cu复合材料为工作电极,以锂箔为对电极和参比电极,以Celgard2400膜为隔膜,以含1mol/LLiPF6的碳酸乙烯酯(EC)和碳酸二乙酯(DEC)的混合液为电解液,其中EC和DEC的体积比为1:1,然后在充满高纯氩气的手套箱内与锂箔组装成扣式模拟锂离子电池,并以恒流充/放电的方法测试其充/放电性能(图5)及循环稳定性能(图6),由图可知,首次放电比容量为828mAh/g,经过68次充/放电后,放电容量升高为1335mAh/g,表现了良好的循环稳定性。
Claims (7)
1.一种石墨烯/铜复合电极材料的应用,其特征在于:石墨烯/铜复合电极材料用作锂离子电池的工作电极。
2.根据权利要求1所述石墨烯/铜复合电极材料的应用,其特征在于:制备锂离子电池过程中无需添加额外的导电剂和粘结剂。
3.根据权利要求1或2所述石墨烯/铜复合电极材料的应用,其特征在于:所述石墨烯/铜复合电极材料的制备方法,具体包括以下步骤:以金属铜为工作电极,以铂片为对电极,以饱和甘汞电极为参比电极,以pH值为3~8的氧化石墨烯悬浮液为电解液,采用一步电沉积法在铜表面自组装石墨烯,得到石墨烯/铜复合电极材料。
4.根据权利要求3所述石墨烯/铜复合电极材料的应用,其特征在于:电解液中氧化石墨烯悬浮液的浓度为0.5~5mg/ml。
5.根据权利要求3所述石墨烯/铜复合电极材料的应用,其特征在于:一步电沉积的沉积时间为0.5~2.5h。
6.根据权利要求3所述石墨烯/铜复合电极材料的应用,其特征在于:一步电沉积的沉积电位为-0.8~-2.5V。
7.根据权利要求3所述石墨烯/铜复合电极材料的应用,其特征在于:所述金属铜为铜箔、泡沫铜或铜纳米线。
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CN108069416A (zh) * | 2016-11-14 | 2018-05-25 | 北京大学 | 超洁净石墨烯及其制备方法 |
CN108110223A (zh) * | 2017-12-18 | 2018-06-01 | 北京鼎能开源电池科技股份有限公司 | 一种石墨烯负极极片及其制备方法 |
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