多孔花状异质结构NiCo2O4/Co3S4-M: 制备及其非对称超级电容器性能

doi:10.15541/jim20250387

无机材料学报 ›› 2026, Vol. 41 ›› Issue (8): 1078-1086.DOI: 10.15541/jim20250387

多孔花状异质结构NiCo₂O₄/Co₃S₄-M: 制备及其非对称超级电容器性能

石璞¹(), 鲁芊芊¹, 刘鑫¹, 张亚琴¹, 李福枝²()

¹ 包装工程学院, 湖南工业大学株洲 412007
² 材料科学与工程学院, 湖南工业大学株洲 412007

收稿日期:2025-10-04 修回日期:2025-12-19 出版日期:2026-08-20 网络出版日期:2026-01-21
通讯作者: 李福枝, 副教授. E-mail: lifuzhi@hut.edu.cn
作者简介:石璞(1976-), 男, 副教授. E-mail: shipu@hut.edu.cn
基金资助:
湖南省教育厅项目(23A0416)

Porous Flowerball-like NiCo₂O₄/Co₃S₄-M Heterostructure: Preparation and Its Performance of Asymmetric Supercapacitor

SHI Pu¹(), LU Qianqian¹, LIU Xin¹, ZHANG Yaqin¹, LI Fuzhi²()

¹ School of Packaging Engineering, Hunan University of Technology, Zhuzhou 412007, China
² School of Materials Science and Engineering, Hunan University of Technology, Zhuzhou 412007, China

Received:2025-10-04 Revised:2025-12-19 Published:2026-08-20 Online:2026-01-21
Contact: LI Fuzhi, associate professor. E-mail: lifuzhi@hut.edu.cn
About author:SHI Pu (1976-), male, associate professor. E-mail: shipu@hut.edu.cn
Supported by:
Education Department of Hunan Province(23A0416)

摘要/Abstract

摘要：

超级电容器具有高功率密度、快速充放电能力和长循环寿命, 在储能领域展现巨大的应用潜力。然而, 其能量密度较低, 限制了进一步发展。本研究通过水热法、模板辅助法及硫化处理构筑了多孔花球状NiCo₂O₄/ Co₃S₄-M异质结构的电极材料, 并系统研究了其电化学性能。三电极体系中, NiCo₂O₄/Co₃S₄-M在1 A·g⁻¹下比容量达2362 F·g⁻¹。其多孔花球结构提供了丰富活性位点, 异质界面优化了电子与离子传输, 两者协同作用显著增强了材料的导电性及稳定性。进一步组装了以多孔花球状NiCo₂O₄/Co₃S₄-M为正极、多孔碳(PC)为负极的非对称超级电容器(NiCo₂O₄/Co₃S₄-M//PC), 当功率密度为375 W·kg⁻¹时, 其能量密度高达98.40 Wh·kg⁻¹; 当功率密度增至7500 W·kg⁻¹时, 能量密度依然保持在45.42 Wh·kg⁻¹。此外, NiCo₂O₄/Co₃S₄-M//PC循环稳定性优异, 在5 A·g⁻¹的电流密度下循环10000次后容量保持率为99.7%, 库仑效率为97.56%。本研究通过异质结构设计与微观形貌调控的策略, 有效实现了高比电容与优异的循环稳定性, 为开发高性能超级电容器电极材料提供了新的研究思路。

关键词: 多孔花球状, 异质结构, 高比电容, 循环稳定性, 超级电容器

Abstract:

Supercapacitors demonstrate significant application potential in the energy storage field due to their high power density, rapid charge-discharge capability, and long cycle life. However, their relatively low energy density restricts further development. In this study, porous flowerball-like NiCo₂O₄/Co₃S₄-M heterostructured electrode materials were constructed via hydrothermal method, template-assisted growth, and sulfuration treatments, and their electrochemical performance was systematically investigated. In a three-electrode system, NiCo₂O₄/Co₃S₄-M exhibits a specific capacitance of 2362 F·g⁻¹ at 1 A·g⁻¹. The porous flowerball structure affords abundant active sites, and the heterointerface facilitates electron/ion transport, synergistically boosting both conductivity and stability. Furthermore, an asymmetric supercapacitor (NiCo₂O₄/Co₃S₄-M//PC) was assembled using porous flowerball-like NiCo₂O₄/Co₃S₄-M as the cathode and porous carbon (PC) as the anode, achieving a high energy density of 98.40 Wh·kg⁻¹ at a power density of 375 W·kg⁻¹, which maintained 45.42 Wh·kg⁻¹ even at a power density of 7500 W·kg⁻¹, along with outstanding cycling stability. After 10000 cycles at a current density of 5 A·g⁻¹, the capacitance retention rate reached 99.7% with a Coulombic efficiency of 97.56%. This study indicates that the strategy of heterostructure design and microstructure modulation can effectively achieve high specific capacity and superior cycling stability, providing new research insights for the development of high-performance supercapacitor electrode materials.

Key words: porous flowerball, heterostructure, high specific capacitance, cycling stability, supercapacitor

中图分类号:

TQ152

石璞, 鲁芊芊, 刘鑫, 张亚琴, 李福枝. 多孔花状异质结构NiCo₂O₄/Co₃S₄-M: 制备及其非对称超级电容器性能[J]. 无机材料学报, 2026, 41(8): 1078-1086.

SHI Pu, LU Qianqian, LIU Xin, ZHANG Yaqin, LI Fuzhi. Porous Flowerball-like NiCo₂O₄/Co₃S₄-M Heterostructure: Preparation and Its Performance of Asymmetric Supercapacitor[J]. Journal of Inorganic Materials, 2026, 41(8): 1078-1086.

图/表 10

图1 (a) NiCo-gly和NiCo-gly@Co-MIM, (b) NiCo2O4-M和NiCo2O4, (c) NiCo2O4/Co3S4-M和NiCo2O4/Co3S4的XRD图谱

Fig. 1 XRD patterns of (a) NiCo-gly and NiCo-gly@Co-MIM, (b) NiCo2O4-M and NiCo2O4, (c) NiCo2O4/Co3S4-M and NiCo2O4/Co3S4 In Fig. (c), star indicating Co3S4 (PDF#47-1738), and diamond indicating NiCo2O4 (PDF#20-0781)

图2 (a~c) NiCo2O4/Co3S4和(d~f) NiCo2O4/Co3S4-M的SEM照片; (g) NiCo2O4/Co3S4-M的EDS元素分布图

Fig. 2 SEM images of (a-c) NiCo2O4/Co3S4 and (d-f) NiCo2O4/Co3S4-M; (g) EDS elemental mappings of NiCo2O4/Co3S4-M

图3 NiCo2O4/Co3S4-M的(a, b) TEM照片、(c) HRTEM照片、(d, f, h) FFT图像、(e, g, i) IFFT图像以及(j~l)晶格间距计算

Fig. 3 (a, b) TEM images, (c) HRTEM image, (d, f, h) FFT images, (e, g, i) IFFT images and (j-l) lattice spacing of NiCo2O4/Co3S4-M

图4 NiCo2O4/Co3S4-M//PC超级电容器的电化学性能

Fig. 4 Electrochemical performance of NiCo2O4/Co3S4-M//PC supercapacitor (a) CV curves of anode PC and cathode NiCo2O4/Co3S4-M at 10 mV·s−1; (b) CV curves at different scan rates; (c) GCD curves at different current densities; (d) EIS spectrum; (e) Ragon plots[10,43,45 -50]; (f) Cyclic stability and Coulombic efficiencies

表1 NiCo2O4/Co3S4-M//PC与同类器件的性能对比

Table 1 Performance of NiCo2O4/Co3S4-M//PC compared with reported systems

Device	Energy density/(Wh·kg⁻¹)	Power density/(W·kg⁻¹)	Capacity retention	Ref.
NiMoO₄@MoS₂//RPHPC	47.5	440	80.2%, 10000 cycles	[43]
CuCo₂O₄@CoS-Cu/Co-MOF//CNTs	73.19	849.94	95.77%, 10000 cycles	[10]
NiCo₂S₄@NiCoS₂//AC	46.3	799.8	80%, 10000 cycles	[45]
MnCo₂O₄@CoS//AC	55.1	477.3	91%, 6000 cycles	[46]
CuCo₂S₄@NiMn-LDH//AC	45.8	1499	87.6%, 10000 cycles	[47]
NiCo-LDH@NiCo-HOS-5//AC	63.6	800	67%, 10000 cycles	[48]
rGO@NiCo-OH/Ni₃S₂//AC	53.5	760	95.5%, 20000 cycles	[49]
CoMoS₄@Ni-Co-S-8//AC	49.1	800	90.3%, 10000 cycle	[50]
NiCo₂O₄/Co₃S₄-M//PC	98.40	375	99.7%, 10000 cycles	This work

图S1 (a~c) NiCo-gly, (d~f) NiCo2O4, (g~i) CoNi-gly@Co-MIM和(j~l) NiCo2O4-M的SEM照片

Fig. S1 SEM images of (a-c) NiCo-gly, (d-f) NiCo2O4, (g-i) CoNi-gly@Co-MIM and (j-l) NiCo2O4-M

图S2 NiCo2O4/Co3S4-M的(a) XPS谱图, 以及(b) Ni2p、(c) Co2p、(d) O1s、(e) S2p的高分辨XPS谱图

Fig. S2 (a) Survey, (b) Ni2p, (c) Co2p, (d) O1s and (e) S2p XPS spectra of NiCo2O4/Co3S4-M

图S3 NiCo2O4/Co3S4-M、NiCo2O4/Co3S4、NiCo2O4-M和NiCo2O4样品的(a) N2吸附-脱附曲线和(b)孔径分布图

Fig. S3 (a) Nitrogen adsorption-desorption isotherms and (b) pore size distributions of NiCo2O4/Co3S4-M, NiCo2O4/Co3S4, NiCo2O4-M and NiCo2O4 samples

图S4 三电极体系的电化学性能

Fig. S4 Electrochemical performance of three-electrode systems (a) CV curves at 10 mV·s−1 and (b) GCD curves at 1 A·g−1 of NiCo2O4/Co3S4-M, NiCo2O4/Co3S4, NiCo2O4-M and NiCo2O4; (c) GCD curves of the NiCo2O4/Co3S4-M electrode at different current densities; (d) Rate capability of NiCo2O4/Co3S4-M; (e) Nyquist plots of NiCo2O4/Co3S4-M, NiCo2O4/Co3S4, NiCo2O4-M and NiCo2O4 with inset showing magnified view of the high-frequency region; (f) CV curves of NiCo2O4/Co3S4-M at 5-80 mV·s−1; (g) Linear relationship between anodic/cathodic peak currents and scan rates for NiCo2O4/Co3S4-M; (h) Proportion of capacitive-controlled and diffusion-controlled contributions in NiCo2O4/Co3S4-M at 20 mV·s−1; (i) Contribution of diffusion-controlled and surface capacitive-controlled processes in NiCo2O4/Co3S4-M within 5-50 mV·s−1

表S1 电极材料的溶液阻抗(Rs)和电荷转移阻抗(Rct)

Table S1 Solution resistance (Rs) and charge transfer resistance (Rct) of electrodes

Parameter	NiCo₂O₄/Co₃S₄-M	NiCo₂O₄/Co₃S₄	NiCo₂O₄-M	NiCo₂O₄
R_s/Ω	0.51	0.55	0.60	0.68
R_ct/Ω	0.34	0.39	0.46	0.54

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多孔花状异质结构NiCo₂O₄/Co₃S₄-M: 制备及其非对称超级电容器性能

Porous Flowerball-like NiCo₂O₄/Co₃S₄-M Heterostructure: Preparation and Its Performance of Asymmetric Supercapacitor

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