NiCo2S4/N,S-rGO纳米复合材料的制备和电化学储钠性能

doi:10.11949/0438-1157.20200525

摘要/Abstract

摘要：

NiCo₂S₄是一种极具发展前景的钠离子电池(SIBs)负极材料。采用简单的一步法(混合和热处理)原位合成了锚定在N、S共掺杂还原氧化石墨烯上的纳米颗粒自组装的NiCo₂S₄亚微米球(NiCo₂S₄/N,S-rGO)。XPS表明了NiCo₂S₄与N,S-rGO之间存在电子转移，证实了NiCo₂S₄与N,S-rGO之间强的协同作用。纳米粒子自组装的NiCo₂S₄亚微米球有效地促进了离子的扩散，N,S-rGO优异的电学和力学性能不仅提高了电极的导电性，而且有效地缓冲了充/放电过程中NiCo₂S₄/N,S-rGO的体积变化。NiCo₂S₄/N,S-rGO作为SIBs的负极材料呈现出高可逆容量，优越的倍率性能和长期稳定性(在电流密度为0.5 A/g时循环130次后仍保持了396.7 mA·h/g的高比容量。即使在电流密度为2 A/g时，经过1000次循环后比容量仍保持在283.3 mA·h/g)。研究结果为高效负极材料的设计和合成提供了新的思路。

关键词: NiCo₂S₄亚微米球, N、S共掺杂还原氧化石墨烯, 纳米材料, 复合材料, 负极材料, 钠离子电池, 电化学

Abstract:

NiCo₂S₄ is a promising anode material for sodium ion batteries (SIBs). In this paper, a simple one-step method (mixing and heat treatment) was used to synthesize in-situ synthesized NiCo₂S₄ submicron spheres (NiCo₂S₄/N,S-rGO) anchored on N, S co-doped reduced graphene oxide. XPS characterization demonstrated electron transfer between NiCo₂S₄ and N,S-rGO, which confirmed the strong synergistic effect between NiCo₂S₄ and N,S-rGO. The nanoparticles self-assembled NiCo₂S₄ spheres effectively promoted ion diffusion, and the excellent electrical and mechanical properties of N,S-rGO not only improved the conductivity of the electrode, but also effectively buffeted the large volume changes of NiCo₂S₄/N,S-rGO during the charge/discharge process. Benefiting from the unique nano-architecture and strong synergistic effect, NiCo₂S₄/N,S-rGO applied as anode materials for SIBs presented a high reversible capacity, impressive rate capability and superior long-term stability (396.7 mA·h/g at 0.5 A/g after 130 cycles, 283.3 mA·h/g at 2 A/g after 1000 cycles). Those results open an interesting strategy for rational design and preparation of efficient anode materials for SIBs.

Key words: homogeneous NiCo₂S₄ spheres, N,S co-doping rGO, nanomaterials, composites, anode material, sodium ion batteries, electrochemistry

中图分类号:

O 646

冯雪廷, 矫庆泽, 李群, 冯彩虹, 赵芸, 黎汉生, 李海军, 蔡惠群. NiCo₂S₄/N,S-rGO纳米复合材料的制备和电化学储钠性能[J]. 化工学报, 2020, 71(9): 4314-4324.

Xueting FENG, Qingze JIAO, Qun LI, Caihong FENG, Yun ZHAO, Hansheng LI, Haijun LI, Huiqun CAI. Preparation and sodium storage performance of NiCo₂S₄/N,S-rGO nanocomposites[J]. CIESC Journal, 2020, 71(9): 4314-4324.

图/表 7

图1 N,S-rGO的SEM (a)和TEM (b)图；NiCo2S4/N,S-rGO的SEM (c)和TEM (d)图；NiCo2S4/N,S-rGO的HRTEM图(e)；NiCo2S4的SEM图(f)

Fig.1 SEM (a) and TEM (b) images of the N,S-rGO； SEM (c) and TEM (d) images of the NiCo2S4/N,S-rGO； HRTEM image of the NiCo2S4/N,S-rGO (e)； SEM image of the NiCo2S4 (f)

图2 NiCo2S4/N,S-rGO, NiCo2S4和N,S-rGO的XRD谱图(a); NiCo2S4/N,S-rGO的EDS谱图(b); NiCo2S4/N,S-rGO(c) 和NiCo2S4(d) 的N2吸-脱附曲线图和孔径分布图

Fig.2 XRD patterns of NiCo2S4/N,S-rGO, NiCo2S4 and N,S-rGO (a); EDS spectrum of NiCo2S4/N,S-rGO (b); N2 adsorption-desorption isotherms and corresponding pore size distribution curves of NiCo2S4/N,S-rGO (c) and NiCo2S4 (d)

图3 NiCo2S4/N,S-rGO和N,S-rGO的N 1s XPS谱图(a); NiCo2S4/N,S-rGO，NiCo2S4和N,S-rGO的S 2p XPS谱图(b); NiCo2S4/N,S-rGO和NiCo2S4的Ni 2p (c)和Co 2p (d) XPS谱图

Fig.3 N 1s XPS spectra of NiCo2S4/N,S-rGO and N,S-rGO (a); S 2p XPS spectra of NiCo2S4/N,S-rGO, NiCo2S4 and N,S-rGO (b); Ni 2p (c) and Co 2p (d) XPS spectra of NiCo2S4/N,S-rGO and NiCo2S4

图4 0.2 mV/s的扫速下NiCo2S4/N,S-rGO的循环伏安曲线(a); 电流密度为0.5 A/g的前3圈的充放电曲线(b); NiCo2S4/N,S-rGO和NiCo2S4的倍率性能(c); NiCo2S4/N,S-rGO在电流密度为0.5 A/g下的循环性能图(d); NiCo2S4/N,S-rGO和NiCo2S4在电流密度为2 A/g下的长期循环性能图 (图中库仑效率为NiCo2S4/N,S-rGO的数值) (e)

Fig.4 CV curves of NiCo2S4/N,S-rGO at a sweep rate of 0.2 mV/s (a); Galvanostatic discharge/charge curves of NiCo2S4/N,S-rGO at 0.5 A/g at initial 3 cycles (b); Rate capability of NiCo2S4/N,S-rGO and NiCo2S4 (c); Cycling stability of NiCo2S4/N,S-rGO at 0.5 A/g (d); Long-term cycling stability of NiCo2S4/N,S-rGO and NiCo2S4 at 2 A/g (the coulombic efficiency is the value of NiCo2S4/N,S-rGO) (e)

图5 NiCo2S4/N,S-rGO和NiCo2S4的交流阻抗图(a); NiCo2S4/N,S-rGO和NiCo2S4在低频区Z′和ω-1/2的线性关系图(b)

Fig.5 Nyquist plots of NiCo2S4/N,S-rGO and NiCo2S4 (a); Relation between Z′ and ω-1/2 at low frequency region of NiCo2S4/N,S-rGO and NiCo2S4 (b)

图6 不同扫速下NiCo2S4/N,S-rGO的循环伏安曲线(a); lgν和lgi线性关系图(b); 1 mV/s扫速下的赝电容贡献(c); 不同扫速下的赝电容贡献(d)

Fig.6 CV curves of NiCo2S4/N,S-rGO at different scan rate (a); Linear relationship between lgν and lgi (b); Contribution ratio of pseudocapacitance at 1 mV/s (c); Contribution ratio of pseudocapacitance at different scan rate (d)

图7 NiCo2S4/N,S-rGO与其他基于过渡金属硫化物的电极材料的性能比较：循环容量(图中数字为循环圈数) (a); 倍率性能(b)this work; RGO-NiCo2S4 hollow prisms[12]; NiCo2S4 nanoparticles@rGO[25]; NiCo2S4 nanosheets[13]; Co3S4@N-Carbon[44]; NiCo2S4@MoS2[45]; CuCo2S4/rGO[46]; Co3S4/CoMo2S4@rGO[47]; multi-layered sandwich-like CuCo2S4/rGO[48]; Ni-Fe-S-CNT[49]; Co9S8@B,N-carbon[50]

Fig.7 Cyclic capacity (the numbers indicate the number of cycles) (a) and rate performance comparison (b) of NiCo2S4/N,S-rGO with other transition metal sulfide-based anodes for sodium ions battery

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NiCo₂S₄/N,S-rGO纳米复合材料的制备和电化学储钠性能

Preparation and sodium storage performance of NiCo₂S₄/N,S-rGO nanocomposites

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