NiO/AC非对称电容器电极材料的制备及性能研究

doi:10.3724/SP.J.1077.2014.13337

无机材料学报 ›› 2014, Vol. 29 ›› Issue (3): 250-256.DOI: 10.3724/SP.J.1077.2014.13337

NiO/AC非对称电容器电极材料的制备及性能研究

叶晓丹^1,2, 胡建冠^1,3, 杨倩¹, 郑遗凡^1,3, 黄宛真¹

(1．浙江工业大学分析测试中心, 杭州310014; 2. 国家林业局竹子研究开发中心, 杭州 310012; 3. 浙江工业大学化学工程与材料学院, 杭州310014)

收稿日期:2013-06-28 修回日期:2013-08-22 出版日期:2014-03-20 网络出版日期:2014-02-18
作者简介:叶晓丹(1987-), 女, 硕士. E-mail:yxd540723531@126.com
基金资助:
浙江省科技厅公益应用研究项目(2011C21009);浙江省教育厅项目(Y201122763)

Preparation and Properties of NiO/AC Asymmetric Capacitor

YE Xiao-Dan^1,2, HU Jian-Guan^1,3, YANG Qian¹, ZHENG Yi-Fan^1,3, HUANG Wan-Zhen¹

(1. Research Center of Analysis and Measurement, Zhejiang University of Technology, Hangzhou 310014, China; 2. China National Bamboo Research and Development Center, Hangzhou 310012, China; 3. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China)

Received:2013-06-28 Revised:2013-08-22 Published:2014-03-20 Online:2014-02-18
About author:YE Xiao-Dan. E-mail:yxd540723531@126.com
Supported by:
Foundation of Science and Technology Department of Zhejiang Province (2011C21009);Foundation of Education Department of Zhejiang Province (Y201122763)

摘要/Abstract

摘要：

以硫酸镍为原料、氨水为沉淀剂, 采用化学沉积法成功制备出氧化镍纳米颗粒, 分别采用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、热重分析仪(TGA)、物理吸附仪等测试手段对纳米氧化镍的物相、形貌和结构进行分析和表征。结果表明, 所制得的纳米氧化镍为球形多孔颗粒, 直径大约为200 nm。其中在300℃下热处理得到的氧化镍比表面积最大, 为132 m²/g, 平均孔径为7.3 nm。将其作为正极, 活性炭作为负极, 组装成非对称电容器, 结果表明非对称电容器具有良好的电容性能和循环稳定性, 在25 mA/g电流密度下, 比电容达到1039 F/g, 充放电效率高达98%以上。

关键词: 纳米颗粒, 氧化镍, 化学沉积, 非对称电容器, 活性炭

Abstract:

The nickel oxide nanoparticles were prepared by chemical bath deposition method with NiSO₄ as raw materials and NH₃?H₂O as precipitation agent. The crystal phase, microstructure and morphology of the nickel oxide were characterized with X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), thermo gravimetric analyzer (TGA) and physical adsorption instrument. The results show that the product is porous spherical like particles with diameter of about 200 nm. Specific surface area of the nickel oxide heat-treated at 300℃ reaches 132 m²/g, with average diameter of 7.3 nm. The asymmetric capacitor with activated carbon as negative electrode and nickel oxide as positive electrode shows good performance and cycling stability. At the discharge current density of 25 mA/g, the asymmetric capacitor’s specific capacitance can reach 1039 F/g, and its’ charge-discharge efficiency is above 98%.

Key words: nanoparticles, nickel oxide, chemical bath deposition, asymmetric capacitor, activated carbon

中图分类号:

TM53

叶晓丹, 胡建冠, 杨倩, 郑遗凡, 黄宛真. NiO/AC非对称电容器电极材料的制备及性能研究[J]. 无机材料学报, 2014, 29(3): 250-256.

YE Xiao-Dan, HU Jian-Guan, YANG Qian, ZHENG Yi-Fan, HUANG Wan-Zhen. Preparation and Properties of NiO/AC Asymmetric Capacitor[J]. Journal of Inorganic Materials, 2014, 29(3): 250-256.

图/表 13

图1 NiO前驱体的热重分析曲线

Fig. 1 Thermal analysis curves of the NiO precursor

图2 前驱体及不同温度热处理得到的NiO的XRD图谱

Fig. 2 XRD patterns of NiO precursor and NiO after heat-treated at different temperatures

图3 经300℃热处理得到NiO的SEM照片

Fig. 3 Typical SEM images of NiO after heat-treated at 300℃

图4 经300℃热处理得到NiO的TEM、HRTEM照片(a, b)及SAED图样(c)

Fig. 4 TEM (a) and HRTEM (b) images and SAED pattern(c) of NiO after heat-treated at 300℃

表1 不同温度热处理得到氧化镍的比表面积和孔结构参数

Table 1 Parameters of specific surface area and pore structure of NiO after heat-treated at different temperatures

Sample	S_BET /(m²?g^-1)	V_{tot /}(cm³?g^-1)	D /nm
AC NiO-250℃	1833 80	2.11 0.11	5.4 8.9
NiO-300℃	132	0.15	7.3
NiO-350℃	112	0.15	6.5
NiO-450℃	71	0.13	8.5

图5 不同温度热处理得到的NiO孔径分布图

Fig. 5 Pore size distribution of NiO after heat-treated at different temperatures

图6 (a)AC和(b) 300℃热处理得到的NiO循环伏安曲线

Fig. 6 Voltammetry characteristics of (a) AC and (b) NiO-300℃

图7 电流密度为25 mA/g时, 不同温度热处理NiO/AC电容器的放电曲线

Fig. 7 Discharge curves of NiO/AC asymmetric capacitor at current density of 25 mA/g

图8 不同温度热处理的NiO/AC电容器比电容

Fig. 8 Specific capacitance of NiO/AC asymmetric capacitor with NiO after heat-treated at different temperatures

图9 NiO(300℃)/AC电容器在不同电流密度下的充放电曲线

Fig. 9 Charge-discharge curves of NiO(300℃)/AC asymmetric capacitor at different current densities

表2 NiO(300℃)/AC在不同电流密度下比电容及电容保持率

Table 2 Specific capacitance and capacity retention of NiO(300℃)/AC asymmetric capacitor at different current densities

Current density/(mA?g^-1)	Specific capacitance/(F?g^-1)	Capacity retention/%
25 50	1039 833	100.0 80.1
100	700	61.5
300	588	51.6
600	579	50.8

图10 NiO(300℃)/AC非对称电容器在不同电流密度下的比电容和循环稳定性关系

Fig. 10 Specific capacitance and cycling performances of NiO(300℃)/AC asymmetric capacitor

图11 NiO(300℃)/AC非对称电容器充放电效率及比电容

Fig. 11 Change of efficiency and specific capacitance with cycle for NiO(300℃)/AC asymmetric capacitor

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NiO/AC非对称电容器电极材料的制备及性能研究

Preparation and Properties of NiO/AC Asymmetric Capacitor

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