NiCo2O4@C纳米复合材料的水热合成及电化学储锂性能

doi:10.7503/cjcu20170173

摘要/Abstract

摘要：

采用一步水热法合成了棒状NiCo₂O₄前驱体, 并通过调节水热反应过程中碳源(葡萄糖)的加入量以及后续热处理条件(气氛、温度)得到了一系列不同的NiCo₂O₄及NiCo₂O₄@C产物, 并对这些产物的结构、形貌及电化学储锂性能进行了测试. 结果表明, 适当的葡萄糖加入量(0.5 g)配合合理的煅烧条件(400 ℃, 氮气气氛)可以获得倍率性能和循环稳定性兼具的NiCo₂O₄@C纳米复合材料. 在100 mA/g的电流密度下, 该材料的首次充/放电比容量为634.1/767.2 mA·h/g, 对应的库仑效率为82.7%, 5周后的放电比容量为650.1 mA·h/g, 容量保持率为84.74%, 且在300 mA/g的高电流密度下可逆比容量仍可保持在225.9 mA·h/g.

关键词: 锂离子电池, 水热合成, NiCo₂O₄@C, 棒状形貌, 原位碳包覆, 电化学性能

Abstract:

Rodlike NiCo₂O₄ precursor was prepored via one-step hydrothermal method and then a series of NiCo₂O₄ and NiCo₂O₄@C products was prepared by regulating the amount of glucose as well as the calcination conditions such as calcination temperature and atmosphere. The products were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy and charge/discharge testing, cyclic voltammetry and electrochemical impedance spectroscopy. The results show that proper amount of glucose(0.5 g) in conjunction with appropriate post-calcination conditions can produce NiCo₂O₄@C nanocomposite with good rate capability and cycling stability. At a current density of 100 mA/g, the material demonstrated the charge/discharge capacities of 634.1/767.2 mA·h/g, corresponding to a Coulombic efficiency of 82.7%, and maintained the discharge capacity of 650.1 mA·h/g after five cycles with a retention rate of 84.74%. Furthermore, at a higher current density of 300 mA/g, the material could still afford a high reversible capacity of 225.9 mA·h/g.

Key words: Lithium ion battery, Hydrothermal synthesis, NiCo₂O₄@C, Rodlike morphology, In-situ carbon coating, Electrochemical performance

中图分类号:

O614.8
O646

TrendMD:

李方方, 王洪宾, 王润伟, 裘式纶, 张宗弢. NiCo₂O₄@C纳米复合材料的水热合成及电化学储锂性能. 高等学校化学学报, 2017, 38(11): 1913.

LI Fangfang, WANG Hongbin, WANG Runwei, QIU Shilun, ZHANG Zongtao. Hydrothermal Synthesis and Electrochemical Li-storage Performances of NiCo₂O₄@C Nanocomposite^†. Chem. J. Chinese Universities, 2017, 38(11): 1913.

图/表 9

Fig.1 XRD patterns of NiCo2O4 materials calcined in air at different temperatures for 5 hTemperature/℃: a. 400; b. 450; c. 500; d. 550.

Fig.2 XPS spectra of NiCo2O4 material calcined in air at 400 ℃ and NiCo2O4/C material calcined in N2 at 400 ℃ (A) Full scan; (B) Ni2p; (C) Co2p; (D) C1s; (E) O1s.

Fig.3 SEM images of the precursor(A), NiCo2O4(B, C) and NiCo2O4@C(D—F) and TEM(G),HRTEM(H) images of NiCo2O4@C-0.5(B) Calcined in air; (C) calcined in N2 atmosphere; (D) NiCo2O4@C-0.25; (E) NiCo2O4@C-0.5; (F) NiCo2O4@C-1.0.

Table 1 CHN testing results(mass fraction) for different samples

Sample	N(%)	C(%)	H(%)
NiCo₂O₄	0.02	0.68	0.123
NiCo₂O₄@C-0.25	1.97	11.63	0.785
NiCo₂O₄@C-0.5	3.59	23.44	1.179
NiCo₂O₄@C-1.0	4.15	28.36	1.476

Fig.4 Charge/discharge curves of NiCo2O4 calcined in air(A) and in N2 atmosphere(B) Current density was 100 mA/g.

Fig.5 Charge-discharge curves of NiCo2O4@C-0.25(A), NiCo2O4@C-0.5(B), NiCo2O4@C-1.0(C) and NiCo2O4@C-M(D)Current density was 100 mA/g.

Fig.6 CV curves of NiCo2O4@C-0.25(A), NiCo2O4@C-0.5(B) and NiCo2O4@C-1.0(C) corresponding to the first five turns(voltage window was 0.01—3.0 V, scan rate was 0.05 mV/s)

Fig.7 Rate performances of NiCo2O4@C-0.25(A), NiCo2O4@C-0.5(B), NiCo2O4@C-1.0(C) electrodes

Fig.8 EIS spectra of NiCo2O4@C-0.25(a), NiCo2O4 @C-0.5(b) and NiCo2O4@C-1.0(c) after five cycles of charge/discharge at current density of 100 mA/gInset: equivalent circuit diagram.

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NiCo₂O₄@C纳米复合材料的水热合成及电化学储锂性能

Hydrothermal Synthesis and Electrochemical Li-storage Performances of NiCo₂O₄@C Nanocomposite^†

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