3D核壳结构NiMoO4@CoFe-LDH纳米棒的高效析氧及全解水性能研究

doi:10.15541/jim20240098

无机材料学报 ›› 2024, Vol. 39 ›› Issue (11): 1254-1264.DOI: 10.15541/jim20240098 CSTR: 32189.14.10.15541/jim20240098

所属专题：【能源环境】氢能材料(202409)

3D核壳结构NiMoO₄@CoFe-LDH纳米棒的高效析氧及全解水性能研究

岳全鑫¹^,²^,³(), 郭瑞华¹^,²^,³(), 王瑞芬¹^,²^,³, 安胜利¹^,²^,³, 张国芳¹, 关丽丽¹^,²

1.材料科学与工程学院内蒙古科技大学, 包头 014010
2.内蒙古自治区先进陶瓷材料与器件重点实验室内蒙古科技大学, 包头 014010
3.轻稀土资源绿色提取与高效利用教育部重点实验室, 包头 014010

收稿日期:2024-03-04 修回日期:2024-05-15 出版日期:2024-11-20 网络出版日期:2024-05-31
通讯作者: 郭瑞华, 教授. E-mail: grh7810@163.com
作者简介:岳全鑫(1998-), 男, 硕士研究生. E-mail: 2438079303@qq.com
基金资助:
国家自然科学基金(51864040);国家自然科学基金(51962028);国家自然科学基金(52162010);内蒙古自治区科技计划(2021GG0042);内蒙古自治区高等学校青年科技英才(NJYT22064);内蒙古自治区自然科学基金(2022MS05018);内蒙古自治区自然科学基金(2022LHMS05021)

3D Core-shell Structured NiMoO₄@CoFe-LDH Nanorods: Performance of Efficient Oxygen Evolution Reaction and Overall Water Splitting

YUE Quanxin¹^,²^,³(), GUO Ruihua¹^,²^,³(), WANG Ruifen¹^,²^,³, AN Shengli¹^,²^,³, ZHANG Guofang¹, GUAN Lili¹^,²

1. School of Materials Science and Engineering, Inner Mongolia University of Science & Technology, Baotou 014010, China
2. Inner Mongolia Key Laboratory of Advanced Ceramic Materials and Devices, Inner Mongolia University of Science & Technology, Baotou 014010, China
3. Key Laboratory of Green Extraction & Efficient Utilization of Light Rare-Earth Resources, Ministry of Education, Inner Mongolia University of Science & Technology, Baotou 014010, China

Received:2024-03-04 Revised:2024-05-15 Published:2024-11-20 Online:2024-05-31
Contact: GUO Ruihua, professor. E-mail: grh7810@163.com
About author:YUE Quanxin (1998-), male, Master candidate. E-mail: 2438079303@qq.com
Supported by:
National Natural Science Foundation of China(51864040);National Natural Science Foundation of China(51962028);National Natural Science Foundation of China(52162010);Inner Mongolia Autonomous Region Science and Technology Program(2021GG0042);Inner Mongolia Autonomous Region Youth Science and Technology Excellence in Higher Education(NJYT22064);Inner Mongolia Autonomous Region Natural Science Foundation Program(2022MS05018);Inner Mongolia Autonomous Region Natural Science Foundation Program(2022LHMS05021)

摘要/Abstract

摘要：

电解水制氢因具有绿色环保、制氢纯度高等优点而得到了科学界的广泛关注。然而, 电催化水分解过程中缓慢的阳极析氧反应(OER)极大地阻碍了电解水制氢的发展进程, 使其在实际应用中面临着许多挑战。本研究采用水热和电沉积相结合的策略, 成功在导电泡沫镍(NF)基底上制得了一种以晶体NiMoO₄纳米棒为“核”、非晶态CoFe-LDH纳米片为“壳”的新型三维(3D)核壳异质结构催化剂。这种特殊的3D核壳结构充分激发了NiMoO₄和CoFe-LDH的电催化潜力, 极大地提升了电化学水分解反应的效率。通过NiMoO₄和非晶态CoFe-LDH的协同作用, NiMoO₄@CoFe-LDH/NF纳米催化剂产生了更多的活性位点, 表现出了高效的电子转移能力和优异的OER电催化活性。电化学测试表明, 当电沉积时间为60 s时, NiMoO₄@CoFe-LDH/NF具有最优异的电化学性能, 在10和100 mA·cm⁻²下的过电位η₁₀和η₁₀₀只有168和216 mV, 且具有极小的Tafel斜率和出色的长期稳定性。同时, NiMoO₄@CoFe-LDH||NiMoO₄全解水系统也表现出了较低的驱动电压, 在1.57 V电压下即可产生10 mA·cm⁻² 的电流密度。这项工作为设计开发高效的电解水催化材料提供了新的思路。

关键词: 析氧反应, 水热和电沉积法, 3D核壳结构, 全解水

Abstract:

Hydrogen generation from electrolyzed water has received extensive attention in the scientific community due to its green and environmentally friendly properties, as well as the high purity of hydrogen produced. However, the slow oxygen evolution reaction (OER) during electrocatalytic water splitting has significantly hampered the development of hydrogen production, posing numerous challenges in its practical application. In this study, a novel three-dimensional (3D) core-shell heterostructure catalyst with crystalline NiMoO₄ nanorods as “core” and amorphous CoFe-LDH nanosheets as “shell” was successfully fabricated on a conductive nickel foam (NF) substrate by using a combination of hydrothermal and electrodeposition strategy. This special 3D core-shell structure fully stimulates the electrocatalytic potential of NiMoO₄and CoFe-LDH, which greatly enhances the efficiency of the overall water-splitting. Through the synergistic interaction of NiMoO₄ and amorphous CoFe-LDH, the NiMoO₄@CoFe-LDH/NF nanocatalysts generates more active sites and exhibits highly efficient electron transfer ability and excellent OER electrocatalytic activity. Electrochemical tests show that NiMoO₄@CoFe-LDH/NF exhibits the most excellent electrochemical performance when the electrodeposition time is 60 s. The overpotentials η₁₀ and η₁₀₀ at 10 and 100 mA·cm⁻²are only 168 and 216 mV, respectively, which shows a very small Tafel slope and excellent long-term stability. Meanwhile, the overall water-splitting system of NiMoO₄@CoFe-LDH||NiMoO₄ exhibits a low driving voltage, which can produce a current density of 10 mA·cm⁻² at 1.57 V. In conclusion, this work provides new ideas for design and development of efficient catalytic materials for electrolyzed water.

Key words: oxygen evolution reaction, hydrothermal and electrodeposition, 3D core-shell structure, overall water splitting

中图分类号:

TQ116

岳全鑫, 郭瑞华, 王瑞芬, 安胜利, 张国芳, 关丽丽. 3D核壳结构NiMoO₄@CoFe-LDH纳米棒的高效析氧及全解水性能研究[J]. 无机材料学报, 2024, 39(11): 1254-1264.

YUE Quanxin, GUO Ruihua, WANG Ruifen, AN Shengli, ZHANG Guofang, GUAN Lili. 3D Core-shell Structured NiMoO₄@CoFe-LDH Nanorods: Performance of Efficient Oxygen Evolution Reaction and Overall Water Splitting[J]. Journal of Inorganic Materials, 2024, 39(11): 1254-1264.

图/表 13

图1 NiMoO4@CoFe-LDH/NF的合成过程示意图

Fig. 1 Synthesis process of NiMoO4@CoFe-LDH/NF

图2 (a) NiMoO4@CoFe-LDH/NF、CoFe-LDH/NF的XRD图谱和(b) CoFe-LDH的拉曼光谱图

Fig. 2 (a) XRD patterns of NiMoO4@CoFe-LDH/NF and CoFe-LDH/NF, and (b) Raman spectrum of CoFe-LDH

图3 催化剂样品的SEM照片

Fig. 3 SEM images of catalyst samples (a) NF; (b, c) CoFe-LDH/NF; (d) NiMoO4/NF; (e, f) NiMoO4@CoFe-LDH-30s/NF; (g, h) NiMoO4@CoFe-LDH-60s/NF; (i, j) NiMoO4@CoFe-LDH-90s/NF; (k, l) NiMoO4@CoFe-LDH-120s/NF

图4 NiMoO4@CoFe-LDH/NF的TEM、HRTEM和EDS面扫照片

Fig. 4 TEM, HRTEM and EDS mapping images of NiMoO4@CoFe-LDH/NF (a) TEM; (b-d) HRTEM images; (e) EDS elemental mappings

图5 NiMoO4@CoFe-LDH和NiMoO4的XPS谱图

Fig. 5 XPS spectra of NiMoO4@CoFe-LDH and NiMoO4 (a) Total, (b) Ni2p, (c) Mo3d, (d) O1s XPS spectra of NiMoO4@CoFe-LDH and NiMoO4; (e) Co2p and (f) Fe2p XPS spectra of NiMoO4@CoFe-LDH

图6 不同催化剂样品的电化学性能

Fig. 6 Electrochemical performance of different catalytic samples (a) OER-LSV curves; (b) OER overpotentials at 10 and 100 mA·cm−2; (c) Tafel plots; (d) Comparison of overpotentials and Tafel slopes at 10 mA·cm-2 for currently reported OER electrocatalysts[56,59⇓⇓⇓⇓ -64]; (e) Nyquist plots; (f) Double-layer capacitance plots. Colorful figures are available on website

图7 NiMoO4@CoFe-LDH/NF的稳定性

Fig. 7 Stability of NiMoO4@CoFe-LDH/NF (a) Chrono-potential testing; (b) LSV polarization curves before and after 12 h of chrono-potential testing; (c, d) SEM images of NiMoO4@CoFe-LDH/NF after chrono-potential testing

图8 OER稳定性测试后NiMoO4@CoFe-LDH的XPS谱图

Fig. 8 XPS spectra of NiMoO4@CoFe-LDH after OER stability test (a) Ni2p; (b) Mo3d; (c) O1s; (d) Co2p; (e) Fe2p

图9 NiMoO4@CoFe-LDH/NF||NiMoO4/NF双电极系统的全解水性能

Fig. 9 Overall water splitting performance of NiMoO4@CoFe-LDH/NF||NiMoO4/NF double electrode system (a) LSV curve; (b) Chrono-potential testing; (c) LSV curves before and after chrono-potential testing; (d) Photograph of the experimental setup; (e) Comparison of overall water splitting potential at 10 mA·cm−2 for currently reported electrocatalysts[39,46,56,71⇓⇓ -74]

图S1 不同沉积时间下制备的催化剂的OER-LSV曲线

Fig. S1 OER-LSV curves of different catalysts prepared for various deposition time

表S1 本实验制备的催化剂与其他文献报道的CoFe-LDH、NiMoO4相关电催化剂在1.0 mol·L-1 KOH中的过电位和Tafel斜率

Table S1 Overpotentials and Tafel slopes of this work, other reported CoFe-LDH, and NiMoO4 related electrocatalysts in 1.0 mol·L-1 KOH

Catalyst	Overpotential/mV (at 10 mA·cm^-2)	Tafel slope/(mV·dec^-1)	Ref.
NiMoO₄@CoFe-LDH/NF	168	29	This work
CoFe-LDH@NiFe	190	45	[56]
NiSe@CoFe LDH/NF	203	90	[59]
NiMoO₄/NiFe	188	39	[60]
Ni₉S₈/MoS₂@NiMoO₄	360	49	[61]
NiMoO₄/Ni-MOF/NF	218	67	[62]
Co₃S₄@NiMoO₄	320	102	[63]
CeNiS@NiMoO₄/NF	187	35	[64]

图S2 不同样品在不同扫描速率(40~120 mV·s-1)下的CV曲线

Fig. S2 CV plots for different samples at different sweep speeds (40-120 mV·s-1) (a) NiMoO4@CoFe-LDH/NF; (b) CoFe-LDH/NF; (c) NiMoO4/NF

图S3 NiMoO4/NF的HER-LSV曲线

Fig. S3 HER-LSV curve of NiMoO4/NF

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3D核壳结构NiMoO₄@CoFe-LDH纳米棒的高效析氧及全解水性能研究

3D Core-shell Structured NiMoO₄@CoFe-LDH Nanorods: Performance of Efficient Oxygen Evolution Reaction and Overall Water Splitting

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