Ni-Co-B-RE(Sm、Dy、Tb)复合电极: 化学沉积法制备及电催化析氢性能研究

doi:10.15541/jim20230491

无机材料学报 ›› 2024, Vol. 39 ›› Issue (5): 467-476.DOI: 10.15541/jim20230491 CSTR: 32189.14.10.15541/jim20230491

所属专题：【能源环境】氢能材料(202409)

Ni-Co-B-RE(Sm、Dy、Tb)复合电极: 化学沉积法制备及电催化析氢性能研究

景欣欣(), 陈必清(), 翟佳鑫, 袁美玲

青海师范大学化学化工学院, 西宁 810000

收稿日期:2023-10-23 修回日期:2024-01-03 出版日期:2024-05-20 网络出版日期:2024-01-31
通讯作者: 陈必清, 教授. E-mail: chenbq2332@163.com
作者简介:景欣欣(1998-), 女, 硕士研究生. E-mail: 470375822@qq.com
基金资助:
国家自然科学基金(22062020)

Ni-Co-B-RE (Sm, Dy, Tb) Composite Electrodes: Preparation by Chemical Deposition Method and Electrocatalytic Hydrogen Evolution Performance

JING Xinxin(), CHEN Biqing(), ZHAI Jiaxin, YUAN Meiling

College of Chemistry and Chemical Engineering, Qinghai Normal University, Xining 810000, China

Received:2023-10-23 Revised:2024-01-03 Published:2024-05-20 Online:2024-01-31
Contact: CHEN Biqing, professor. E-mail: chenbq2332@163.com
About author:JING Xinxin (1998-), female, Master candidate. E-mail: 470375822@qq.com
Supported by:
National Natural Science Foundation of China(22062020)

摘要/Abstract

摘要：

开发低成本、高活性的非贵金属电催化剂对电解水的实际应用具有重要意义, 稀土(Rare Earth, RE)元素因其独特的电子结构成为金属催化剂改性的研究热点, 但在泡沫镍(Nickel Foam, NF)基体上制备稀土复合催化剂的方法存在成本高、工艺复杂和耗时长等问题。本研究采用一步化学沉积法, 在NF基体上制备了三种稀土复合电极Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF, 对催化电极的结构和形貌进行了表征, 并研究其在1 mol·L^-1 KOH溶液中的析氢性能。结果表明, 添加Sm、Dy和Tb可使电极的电子结构发生改变, 改善催化剂材料的本征性质, 进而提高析氢反应(Hydrogen Evolution Reaction, HER)的催化性能。其中, Ni-Co-B-Tb/NF表现出最佳的析氢性能, 达到10 mA·cm^-2的电流密度仅需58 mV的过电位, Tafel斜率为65 mV·dec^-1, 析氢反应由Volmer-Heyrovsky步骤控制。进一步研究发现稀土浓度对电催化性能影响较大, 当Tb浓度为3 g·L^-1时, Ni-Co-B-Tb/NF表面颗粒尺寸较小且分布均匀, 暴露出更多的活性位点, 有利于HER的电荷转移, 析氢性能最佳。此外, 经过100 h长期稳定性测试和2000次循环伏安(Cyclic Voltammetry, CV)测试后, 该催化剂表现出良好的电化学稳定性。

关键词: 稀土, 化学沉积, 析氢反应, 泡沫镍

Abstract:

Developing low-cost, high-activity non-precious metal electrocatalysts is of great significance for the practical application of water electrolysis. Rare earth (RE) elements have become a research hotspot for the modification of metal catalysts due to their unique electronic structures. However, the methods for preparing rare earth composite catalysts on nickel foam (NF) substrates are demanding, presenting issues such as high cost, complex processes, and long production time. This research employed a straightforward chemical deposition technique to fabricate rare earth composite electrodes on NF substrates. The structure and morphology of the catalytic electrodes were characterized, and their hydrogen evolution performances in 1 mol·L^-1 KOH solution were investigated. The results revealed that adding Sm, Dy, and Tb could alter the electronic structure of the electrodes, improve the intrinsic properties of the catalyst materials, and enhance the catalytic performance for hydrogen evolution reaction (HER). Ni-Co-B-Tb/NF displayed superior hydrogen evolution performance with an overpotential of only 58 mV at a current density of 10 mA·cm^-2 and a Tafel slope of 65 mV·dec^-1. HER was controlled by the Volmer-Heyrovsky step. It was found that the variation of rare earth concentration had great effect on the electrocatalytic performance. When the Tb concentration was 3 g·L^-1, smaller size and uniformer distribution of particles on the surface of Ni-Co-B-Tb/NF exposed more active sites, which was favorable for HER charge transfer, and the best performance of hydrogen evolution was achieved. Furthermore this catalyst exhibited remarkable electrochemical stability following an extensive 100 h stability test and 2000 cyclic voltammetry (CV) testing.

Key words: rare earth, chemical deposition, hydrogen evolution reaction, nickel foam

中图分类号:

TQ151

景欣欣, 陈必清, 翟佳鑫, 袁美玲. Ni-Co-B-RE(Sm、Dy、Tb)复合电极: 化学沉积法制备及电催化析氢性能研究[J]. 无机材料学报, 2024, 39(5): 467-476.

JING Xinxin, CHEN Biqing, ZHAI Jiaxin, YUAN Meiling. Ni-Co-B-RE (Sm, Dy, Tb) Composite Electrodes: Preparation by Chemical Deposition Method and Electrocatalytic Hydrogen Evolution Performance[J]. Journal of Inorganic Materials, 2024, 39(5): 467-476.

图/表 23

图1 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF的(a~d)低倍率和(e~h)高倍率SEM照片

Fig. 1 (a-d) Low-magnification and (e-h) high-magnification SEM images of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF, and Ni-Co-B-Dy/NF

图2 (a) Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF样品粉末的XRD谱图; (b) Ni-Co-B-Tb/NF的EDS谱图

Fig. 2 (a) XRD patterns of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF and Ni-Co-B-Dy/NF powders, and (b) EDS mappings of Ni-Co-B-Tb/NF

图3 Ni-Co-B-Tb/NF的XPS谱图

Fig. 3 XPS spectra of Ni-Co-B-Tb/NF (a) Total survey; (b) Ni2p; (c) Co2p; (d) B1s; (e) Tb3d

图4 Ni-Co-B-Tb/NF的(a)TEM和(b)HRTEM照片

Fig. 4 (a) TEM and (b) HRTEM images of Ni-Co-B-Tb/NF

图5 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF电极的(a)LSV曲线, (b) Tafel曲线, (c) Tafel曲线外推得到的交换电流密度(j0)和(d)EIS图谱(插图为等效电路图)

Fig. 5 (a) LSV curves, (b) Tafel curves, (c) exchange current densities (j0) extrapolated from Tafel plots and (d) EIS spectra with inset showing equivalent circuit of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF, and Ni-Co-B-Dy/NF electrodes Colorful figures are available on website

图6 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF(a~d)在不同温度下的LSV曲线(插图为相应的Tafel曲线)和(e)阿伦尼乌斯曲线

Fig. 6 (a-d) LSV curves at different temperatures with insets showing corresponding Tafel curves and (e) Arrhenius plots of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF and Ni-Co-B-Dy/NF Colorful figures are available on website

图7 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF电极(a~d)在不同扫描速率下的CV曲线, (e)充电双电层库仑曲线和(f) ECSA归一化后的LSV曲线

Fig. 7 (a-d) CV curves at different scan rates, (e) charge double-layer voltammetry, and (f) ECSA-normalized LSV curves of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF, and Ni-Co-B-Dy/NF electrodes Colorful figures are available on website

图8 x-TNCB/NF(x=1, 2, 3, 4, 5)电极的(a)LSV曲线, (b) Tafel曲线, (c) Tafel曲线外推得到的交换电流密度(j0)和(d)EIS图谱(插图为等效电路图)

Fig. 8 (a) LSV curves, (b) Tafel curves, (c) exchange current densities (j0) extrapolated from Tafel plots, and (d) EIS spectra with inset showing equivalent circuit of x-TNCB/NF (x=1, 2, 3, 4, 5) electrodes Colorful figures are available on website

图9 3-TNCB/NF电极(a)在2000圈CV扫描前后的LSV曲线和(b)在100 mV电位下电解100 h的电流-时间曲线

Fig. 9 (a) LSV curves before and after 2000 CV sweeps, and (b) I-t curve under 100 mV static overpotential for 100 h electrolysis of 3-TNCB/NF electrode

表S1 化学沉积镀液配方

Table S1 Chemical deposition plating solution formula

Composition of plating solution	Concentration/(g·L^-1)
Anhydrous nickel chloride (NiCl₂)	10.0
Anhydrous cobalt chloride (CoCl₂)	5.0
Borane dimethylamine	1.0
Samarium nitrate [Sm(NO₃)₃]	3.0
Terbium nitrate [Tb(NO₃)₃]	1.0-5.0
Dysprosium nitrate [Dy(NO₃)₃]	3.0
Succinic acid	1.5
Citric acid	1.5
Malic acid	1.5

图S1 (a) Ni-Co-B-Sm/NF的EDS元素分布图; (b) Ni-Co-B-Dy/NF的EDS元素分布图

Fig. S1 (a) EDS mappings of Ni-Co-B-Sm/NF; (b) EDS mappings of Ni-Co-B-Dy/NF

表S2 Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF电极的ICP-MS数据

Table S2 ICP-MS data of Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF and Ni-Co-B-Dy/NF electrodes

Catalyst	Element	Content/%(in mass)
Ni-Co-B-Tb/NF	Ni	49.08
	Co	22.20
	B	2.71
	Tb	1.57
Ni-Co-B-Sm/NF	Ni	39.48
	Co	9.41
	B	2.16
	Sm	1.35
Ni-Co-B-Dy/NF	Ni	53.89
	Co	21.66
	B	2.49
	Dy	1.94

图S2 x-TNCB/NF (x=1, 2, 3, 4, 5)样品的SEM照片

Fig. S2 SEM images of x-TNCB/NF (x=1, 2, 3, 4, 5)

表S3 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF电极的EIS参数

Table S3 EIS parameters of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF and Ni-Co-B-Dy/NF electrodes

Catalyst	R_s/(Ω·cm^-2)	R_ct/(Ω·cm^-2)
Ni-Co-B/NF	0.379	0.171
Ni-Co-B-Tb/NF	0.376	0.144
Ni-Co-B-Sm/NF	0.390	0.251
Ni-Co-B-Dy/NF	0.393	0.357

表S4 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF的动力学参数

Table S4 Kinetic parameters of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF and Ni-Co-B-Dy/NF

Catalyst	T/K	Tafel slope/(mV·dec^-1)	j₀/(mA·cm^-2)	E_a/(kJ·mol^-1)
Ni-Co-B/NF	298	115	1.86	32.2
	313	88	4.36
	323	104	8.12
	333	99	18.6
Ni-Co-B-Tb/NF	298	123	2.69	11.5
	313	125	3.71
	323	125	4.89
	333	114	6.02
Ni-Co-B-Sm/NF	298	152	1.65	19.8
	313	140	2.57
	323	150	3.46
	333	219	6.30
Ni-Co-B-Dy/NF	298	164	1.99	17.2
	313	168	3.01
	323	165	4.36
	333	187	6.30

表S5 Ni-Co-B/NF、Ni-Co-B-Tb/NF、Ni-Co-B-Sm/NF和Ni-Co-B-Dy/NF催化剂的ECSA数据

Table S5 ECSA of Ni-Co-B/NF, Ni-Co-B-Tb/NF, Ni-Co-B-Sm/NF and Ni-Co-B-Dy/NF catalysts

Catalyst	ECSA/(cm²·g^-1)
Ni-Co-B/NF	677.5
Ni-Co-B-Tb/NF	1517.5
Ni-Co-B-Sm/NF	980
Ni-Co-B-Dy/NF	1262.5

图S3 x-TNCB/NF(x=1, 2, 3, 4, 5)电极在不同扫描速率下的CV曲线

Fig. S3 CV curves at different scan rates for x-TNCB/NF (x=1, 2, 3, 4, 5)

图S4 x-TNCB/NF (x=1, 2, 3, 4, 5)电极的(a)充电双电层库仑曲线和(b)ECSA归一化后LSV曲线

Fig. S4 (a) Charge double-layer voltammetry and (b) LSV curves with normalized ECSA of x-TNCB/NF (x=1, 2, 3, 4, 5) electrodes

表S6 x-TNCB/NF (x=1, 2, 3, 4, 5)催化剂的ECSA数据

Table S6 ECSA of x-TNCB/NF (x=1, 2, 3, 4, 5) catalysts

Catalyst	ECSA/(cm²·g^-1)
1-TNCB/NF	802.5
2-TNCB/NF	1140.0
3-TNCB/NF	1505.0
4-TNCB/NF	1322.5
5-TNCB/NF	862.5

表S7 x-TNCB/NF (x=1, 2, 3, 4, 5)电极的EIS参数

Table S7 EIS parameters of x-TNCB/NF (x=1, 2, 3, 4, 5) electrodes

Catalyst	R_s/(Ω·cm^-2)	R_ct/(Ω·cm^-2)
1-TNCB/NF	0.307	0.376
2-TNCB/NF	0.299	0.275
3-TNCB/NF	0.320	0.222
4-TNCB/NF	0.306	0.258
5-TNCB/NF	0.315	0.353

图S5 x-TNCB/NF(x=1, 2, 3, 4, 5)电极(a~e)在不同温度下LSV曲线(插图为不同温度下Tafel曲线)和(f)阿伦尼乌斯曲线

Fig. S5 (a-e) LSV curves at different temperatures and (f) Arrhenius plots with inset showing corresponding Tafel curves of x-TNCB/NF (x=1, 2, 3, 4, 5)

表S8 x-TNCB/NF (x=1, 2, 3, 4, 5)的动力学参数

Table S8 Kinetic parameters of x-TNCB/NF (x=1, 2, 3, 4, 5)

Catalyst	T/K	Tafel slope/(mV·dec^-1)	j₀/(mA·cm^-2)	E_a/(kJ·mol^-1)
1-TNCB/NF	298	138	1.94	24.8
	313	152	3.23
	323	141	6.02
	333	130	10.71
2-TNCB/NF	298	177	1.73	19.7
	313	154	2.75
	323	137	4.46
	333	130	7.24
3-TNCB/NF	298	141	3.01	11.5
	313	130	3.98
	323	163	5.24
	333	162	6.76
4-TNCB/NF	298	148	2.13	16.2
	313	128	3.31
	323	161	4.89
	333	195	6.60
5-TNCB/NF	298	169	1.69	19.8
	313	167	2.57
	323	163	4.57
	333	205	6.91

图S6 3-TNCB/NF的法拉第效率

Fig. S6 Faradaic efficiency for 3-TNCB/NF

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Ni-Co-B-RE(Sm、Dy、Tb)复合电极: 化学沉积法制备及电催化析氢性能研究

Ni-Co-B-RE (Sm, Dy, Tb) Composite Electrodes: Preparation by Chemical Deposition Method and Electrocatalytic Hydrogen Evolution Performance

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