一步水热法制备电解水析氧反应Ni3S2@Mo2S3高效催化剂

doi:10.11949/0438-1157.20211147

摘要/Abstract

摘要：

采用一步水热法，由泡沫钼镍合金同时提供钼源和镍源在泡沫钼镍合金表面原位制备了Ni₃S₂@Mo₂S₃，并将其直接作为自支撑电极用于催化碱性介质中的电解水析氧反应（OER）。利用多种表征测试技术研究了样品的形貌、组成、OER电催化性能，结果显示：Ni₃S₂@Mo₂S₃呈纳米板形貌，由六方Ni₃S₂和单斜Mo₂S₃按5∶1的比例复合而成；在1 mol·L^-1KOH 溶液中，Ni₃S₂@Mo₂S₃催化剂仅需要170 mV过电位就可达到10 mA·cm^-2电流密度（欧姆补偿后），且在50 h的稳定性测试期间性能基本无衰减，优于贵金属催化剂IrO₂以及文献报道的Ni-Mo基复合催化剂。Ni₃S₂@Mo₂S₃具有优异电催化性能的原因可归于不同过渡金属化合物的协同作用、原位生长自支撑、电化学活性面积大以及液下疏气性等因素。

关键词: 水热, 电化学, 催化, 析氧反应

Abstract:

The Ni₃S₂@Mo₂S₃ self-supported catalyst for oxygen evolution reaction in water electrolysis was in situ synthesized on MoNi foam (MNF) by one-step hydrothermal method with MNF as the sources of Ni and Mo. The morphology, composition and OER electrocatalytic performance of the as-prepared catalyst were characterized by the corresponding characterization techniques and electrochemical methods. The catalyst was consisted of irregular nano-slabs with the composition of hexagonal Ni₃S₂ and monoclinic Mo₂S₃ in a ratio of 5∶1. The as-prepared Ni₃S₂@Mo₂S₃ only needed an overpotential of 170 mV (after IR compensation) to drive a current density of 10 mA·cm^-2 in 1 mol·L^-1KOH with negligible degradation during the 50 h stability test, which was superior to the commercial catalyst IrO₂ and other Ni-Mo based catalysts reported. The excellent electrocatalytic performance of Ni₃S₂@Mo₂S₃ can be attributed to the synergistic effect of different transition metal compounds, self-supporting in situ growth, large electrochemically active area, and aerophobicity under liquid.

Key words: hydrothermal, electrochemistry, catalysis, oxygen evolution reaction

中图分类号:

TQ 151.1

赵娟, 吴梦成, 雷惊雷, 李凌杰. 一步水热法制备电解水析氧反应Ni₃S₂@Mo₂S₃高效催化剂[J]. 化工学报, 2022, 73(4): 1575-1584.

Juan ZHAO, Mengcheng WU, Jinglei LEI, Lingjie LI. One-step hydrothermal method toward preparation of Ni₃S₂@Mo₂S₃high-efficient catalyst for oxygen evolution reaction in water electrolysis[J]. CIESC Journal, 2022, 73(4): 1575-1584.

图/表 7

图1 水热样品在不同放大倍数下的FE-SEM图像

Fig.1 FE-SEM images at different resolutions of the hydrothermal sample

图2 水热产物的XRD与XPS表征结果

Fig.2 XRD patterns and XPS spectra of the hydrothermal products

图3 电催化性能测试结果

Fig.3 Electrocatalytic performance

表1 Ni-Mo基复合催化剂催化性能比较

Table 1 Comparison of the OER electrocatalytic performance of Ni-Mo based catalysts

催化剂	η₁₀/mV	Stability/h	文献
Ni₃S₂@Mo₂S₃/NMF	170	50	this work
MoS₂/NiS/NF	216	10000 cycles	[48]
MoS₂/NiS₂	278	24	[49]
MoS₂/Ni₃S₂	218	10	[50]
Ni₃S₂@MoS₂/FeOOH	234	50	[51]
MoS₂-Ni₃S₂ HNRs/NF	249	48	[52]
light Fe-doped (NiS₂/MoS₂)/CNT	234	—	[53]
NiMoS	260	15	[54]
MoS₂/NiS yolk-shell	350	24	[55]

图4 CV曲线和Cdl拟合结果

Fig.4 CV curves and fitting results of Cdl

图5 气体接触角测试结果

Fig.5 Gas contact angles of different sample surfaces

图6 理论模型（蓝色代表Ni原子；绿色代表Mo原子；黄色代表S原子）

Fig.6 Theoretical models（atom colors: Ni, blue; Mo, green; and S, yellow）

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一步水热法制备电解水析氧反应Ni₃S₂@Mo₂S₃高效催化剂

One-step hydrothermal method toward preparation of Ni₃S₂@Mo₂S₃high-efficient catalyst for oxygen evolution reaction in water electrolysis

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