铁掺杂多孔非晶镍磷酸盐材料制备及阴离子交换膜电解水制氢

doi:10.15541/jim20250463

无机材料学报 ›› 2026, Vol. 41 ›› Issue (9): 1255-1264.DOI: 10.15541/jim20250463

铁掺杂多孔非晶镍磷酸盐材料制备及阴离子交换膜电解水制氢

高卯¹(), 唐春¹^,²(), 陈明³^,⁴, 钟勇斌³^,⁴, 王鑫³^,⁴, 丁毅⁵, 文俊元¹, 周莹¹^,²()

¹ 西南石油大学新能源与材料学院, 成都 610500
² 氢能绿色制储与高效利用川渝共建重点实验室, 成都 610500
³ 东方电气集团东方锅炉股份有限公司, 成都 611731
⁴ 科技有限公司, 成都 610000
⁵ 西南化工研究设计院有限公司多孔材料与分离转化全国重点实验室, 国家碳一化学工程技术研究中心, 成都 610225

收稿日期:2025-11-21 修回日期:2026-02-13 出版日期:2026-09-20 网络出版日期:2026-03-18
通讯作者: 唐春, 副研究员. E-mail: tangchun@swpu.edu.cn;
周莹, 教授. E-mail: yzhou@swpu.edu.cn
作者简介:高卯(2000-), 男, 硕士研究生. E-mail: gm18254378418@163.com
基金资助:
中国博士后科学基金(2024M750704);四川省重大科技专项(2024ZDZX0034);四川省博士后科研项目特别资助(TB2024006)

Synthesis of Iron-doped Porous Amorphous Nickel Phosphate and Its Application in Hydrogen Production via Anion Exchange Membrane Water Electrolysis

GAO Mao¹(), TANG Chun¹^,²(), CHEN Ming³^,⁴, ZHONG Yongbin³^,⁴, WANG Xin³^,⁴, DING Yi⁵, WEN Junyuan¹, ZHOU Ying¹^,²()

¹ School of New Energy and Materials, Southwest Petroleum University, Chengdu 610500, China
² Sichuan-Chongqing Joint Key Laboratory of Green Hydrogen Production and Storage and Efficient Utilization, Chengdu 610500, China
³ Dongfang Electric Group Dongfang Boiler Co., Ltd., Chengdu 611731, China
⁴ Dongfang Electric (Hydrogen Energy) Technology Co., Ltd., Chengdu 610000, China
⁵ National Engineering Research Center for C1 Chemistry, State Key Laboratory of Porous Materials for Separation and Conversion, Southwest Institute of Chemical Co., Ltd., Chengdu 610225, China

Received:2025-11-21 Revised:2026-02-13 Published:2026-09-20 Online:2026-03-18
Contact: TANG Chun, associate professor. E-mail:tangchun@swpu.edu.cn;ZHOU Ying, professor. E-mail:yzhou@swpu.edu.cn
About author:GAO Mao (2000-), male, Master candidate. E-mail: gm18254378418@163.com
Supported by:
China Postdoctoral Science Foundation(2024M750704);Sichuan Province Major Science and Technology Special Project(2024ZDZX0034);Sichuan Province Postdoctoral Scientific Research Project Special Grant(TB2024006)

摘要/Abstract

摘要：

高效稳定的双功能非贵金属电催化材料对于降低电解水制氢成本至关重要。本研究通过电沉积结合化学刻蚀策略, 在镍泡沫(Nickel Foam, NF)上构筑了铁掺杂的多孔镍磷酸盐非晶催化材料(Fe-NiOP/NF)。该策略通过电沉积法在导电基底NF上可控制备纳米薄膜, 并利用化学刻蚀原位诱导薄膜产生多孔结构。多孔结构有利于电解液传质和气体析出, 铁掺杂诱导电荷从Ni转移到Fe, 有效优化了活性位点Ni的电子结构, 基于电化学活性面积(ECSA)归一化的本征活性比较, Fe-NiOP/NF的双电层电容是未掺杂Fe样品的2.95倍。此外, Fe-NiOP/NF催化材料在析氢和析氧反应中均表现出优异的双功能催化活性, 在-500 mA·cm^-2电流密度下, 其析氢和析氧过电位分别为246和291 mV。Fe-NiOP/NF作为双功能催化材料应用于阴离子交换膜电解水(AEMWE)器件, 在70 ℃实现了1.92 V@1 A·cm^-2和2.13 V@2 A·cm^-2的催化性能, 并能够在1 A·cm^-2大电流密度下稳定运行200 h以上。本研究开发的Fe-NiOP/NF电催化材料的合成方法简便, 并且兼具高性能与高稳定性的优点, 为开发适用于工业级绿氢生产的电极材料提供了新方法。

关键词: 氢能, 多孔结构, 非晶材料, 大电流密度, 阴离子交换膜电解水

Abstract:

Efficient and stable bifunctional non-noble metal electrocatalytic materials are essential to reduce the cost of hydrogen production by electrolysis. This study constructed iron-doped hierarchical porous amorphous nickel phosphate catalytic materials (Fe-NiOP/NF) on nickel foam (NF) using electrodeposition combined with chemical etching. This strategy allows the controllable preparation of nanosheets on the conductive substrate nickel foam by electrodeposition and in-situ induction of the nanosheets to a porous structure by chemical etching. The porous structure facilitates mass transfer of electrolyte and gas evolution. Iron doping effectively optimizes the electronic structure of active site Ni by triggering charge redistribution from Ni to Fe. The intrinsic activity normalized by electrochemical active surface area (ECSA) increases by approximately 2.95 times compared to the undoped sample. The Fe-NiOP/NF catalytic material exhibits excellent bifunctional catalytic activity in both the hydrogen evolution reaction and the oxygen evolution reaction, with a hydrogen evolution overpotential of 246 mV and an oxygen evolution overpotential of 291 mV at a current density of -500 mA·cm^-2. When used as a bifunctional catalytic material in anion exchange membrane water electrolysis (AEMWE) devices, Fe-NiOP/NF achieves catalytic performances of 1.92 V@1 A·cm^-2 and 2.13 V@2 A·cm^-2 at 70 ℃, and operates steadily for longer than 200 h at a current density of 1 A·cm^-2. The electrocatalytic material Fe-NiOP/NF developed in this study possesses the advantages of a simple synthesis method, high performance, and high stability, providing a new method for development of the electrode for industrial-level green hydrogen production.

Key words: hydrogen energy, porous structure, amorphous material, large current density, anion exchange membrane water electrolysis

中图分类号:

TQ116

高卯, 唐春, 陈明, 钟勇斌, 王鑫, 丁毅, 文俊元, 周莹. 铁掺杂多孔非晶镍磷酸盐材料制备及阴离子交换膜电解水制氢[J]. 无机材料学报, 2026, 41(9): 1255-1264.

GAO Mao, TANG Chun, CHEN Ming, ZHONG Yongbin, WANG Xin, DING Yi, WEN Junyuan, ZHOU Ying. Synthesis of Iron-doped Porous Amorphous Nickel Phosphate and Its Application in Hydrogen Production via Anion Exchange Membrane Water Electrolysis[J]. Journal of Inorganic Materials, 2026, 41(9): 1255-1264.

图/表 21

图1 Fe-NiOP/NF的微观形貌

Fig. 1 Microstructure of Fe-NiOP/NF (a-c) SEM images; (d, e) TEM images; (f) High-resolution TEM image; (g) STEM image and EDS line-scanning profiles

图2 NiOP/NF和Fe-NiOP/NF的XRD图谱和XPS谱图

Fig. 2 XRD patterns and XPS spectra of NiOP/NF and Fe-NiOP/NF (a) XRD patterns of NF, NiOP/NF and Fe-NiOP/NF; (b) Survey, high-resolution (c) Ni2p, (d) Fe2p, (e) O1s, and (f) P2p XPS spectra of NiOP/NF and Fe-NiOP/NF

图3 催化剂材料的Ni K边和Fe K边XANES谱和FT-EXAFS曲线

Fig. 3 Ni, Fe K-edge XANES spectra and FT-EXAFS curves of catalysts materials (a) Ni K-edge XANES spectra; (b) Ni R-space FT-EXAFS curves; (c) Fe K-edge XANES spectra;(d) Fe R-space FT-EXAFS curves. Colorful figures are available on website

图4 Fe-NiOP/NF的(a~c) HER电化学性能以及(d)与文献报道的其他催化材料性能对比[32-41]

Fig. 4 (a-c) Electrochemical HER performance of Fe-NiOP/NF and (d) comparison with reported catalysts[32-41] (a) LSV curves; (b) Tafel plots; (c) Nyquist plots

图5 Fe-NiOP/NF的(a~c) OER电化学性能以及(d)与文献报道的其他催化材料的性能对比[34,36-37,41-47]

Fig. 5 (a-c) Electrochemical OER performance of Fe-NiOP/NF and (d) comparison with reported catalysts[34,36-37,41-47] (a) LSV curves; (b) Tafel plots; (c) Nyquist plots

图6 Fe-NiOP/NF AEMWE器件的性能

Fig. 6 Electrochemical analysis of Fe-NiOP/NF AEMWE electrolyzer (a) Schematic of anion exchange membrane (AEM) electrolyzer; (b) Polarization curves of AEM-electrolyzers equipped with Fe-NiOP/NF and NiOP/NF catalysts; Overvoltage subdivision of AEMWE catalyzed by (c) Fe-NiOP/NF and (d) NiOP/NF; (e) Overpotential (η) subdivisions of AEMWE by Ohmic loss (ηohm), activation loss (ηact) and mass transport loss (ηmass); (f) Durability test results for the AEM electrolyzer at 1 A·cm-2 for 200 h. Colorful figures are available on website

图S1 Fe-NiOP电极电化学测试及不同刻蚀时间的对比

Fig. S1 Electrochemical testing of Fe-NiOP electrode and comparison of different etching durations: (a) Hydrogen evolution polarization curves; (c) Oxygen evolution polarization curves; Overpotential required to reach the benchmark current density for (b) hydrogen and (d) oxygen evolution

图S2 NiOP/NF的微观形貌

Fig. S2 Microstructure of NiOP/NF (a-d) SEM images; (e, f) TEM images

图S3 Fe-NiOP/NF的SAED图谱

Fig. S3 SAED pattern of Fe-NiOP/NF

图S4 Fe-NiOP/NF的元素分布图

Fig. S4 Elemental distribution mappings of Fe-NiOP/NF

图S5 (a, b) Ni k-2与(c, d) Fe k-2加权EXAFS信号的小波变换图谱

Fig. S5 Wavelet transform spectra of weighted EXAFS signals for Ni k-2 and Fe k-2 (a) NiOP/NF; (b) Fe-NiOP/NF; (c) Fe-Foil; (d) Fe-NiOP/NF

图S6 析氢电位测试下(a) NiOP/NF和(b) Fe-NiOP/NF的Bode谱图

Fig. S6 Bode spectra of NiOP/NF and (b) Fe-NiOP/NF under hydrogen evolution potential.

图S7 NiO/NF、NiOP/NF和Fe-NiOP/NF的(a~c)循环伏安曲线和(d)双电层电容

Fig. S7 (a-c) CV curves and (d) double-layer capacitances of NiO/NF, NiOP/NF and Fe-NiOP/NF (a) NiO/NF; (b) NiOP/NF; (c) FeNiOP/NF

图S8 (a) NiOP/NF和(b) Fe-NiOP/NF的稳定性对比

Fig. S8 Comparison of the stability of (a) NiOP/NF and (b) Fe-NiOP/NF I-t curves at -0.87 V (vs. RHE) without iR correction

图S9 析氧电位测试下(a) NiOP/NF和(b) Fe-NiOP/NF的Bode谱图

Fig. S9 Bode spectra of (a) NiOP/NF and (b) Fe-NiOP/NF under oxygen evolution potential

图S10 NiOP/NF和Fe-NiOP/NF的Nyquist谱图

Fig. S10 Nyquist plots of NiOP/NF and Fe-NiOP/N

图S11 NiOP/NF和Fe-NiOP/NF AEMWE的极化曲线和HFR-free电压曲线

Fig. S11 Polarization curves and HFR-free voltage curves of AEMWE catalyzed by Fe-NiOP/NF and NiOP/NF

图S12 (a) Fe-NiOP/NF和(b) NiOP/NF的接触角测试

Fig. S12 Contact angle tests of (a) Fe-NiOP/NF and (b) NiOP/NF

图S13 Fe-NiOP/NF工作200 h后的SEM照片

Fig. S13 SEM images of Fe-NiOP/NF after operation for 200 h

图S14 Fe-NiOP/NF 200 h稳定性测试后的高分辨(a) Fe2p、(b) Ni2p、(c) P2p和(d) O1s XPS谱图

Fig. S14 High-resolution (a) Fe2p, (b) Ni2p, (c) P2p and (d) O1s XPS spectra of Fe-NiOP/NF after 200 h durability test

表S1 在1 mol·L-1 KOH电解液中AEMWE的性能比较

Table S1 Performance comparison of AEMWE with 1 mol·L-1 KOH as electrolyte

Cathode	Anode	AEM	Temperature/℃	Performance	Ref.
FeNiOP	FeNiOP	Alkymer® W-75	70	1 A/cm² at 1.92 V_cell	This work
CoFe@HNCS20	NiFe-LDH	Sustainion® X37-50 Grade T	55	0.5 A/cm² at 1.808 V_cell	[S1]
Pt/C	NiMn₂O₄	FAA3-50	80	0.53 A/cm² at 2 V_cell	[S2]
Ni@Ni(OH)₂/Ti	IrO₂/CP	Sustainion®37	50	1 A/cm² at 2 V_cell	[S3]
Pt	NiFeO_x	Sustainion^TMX37-50	50	0.65 A/cm² at 2 V_cell	[S4]
NiFeCo	NiFe	Sustainion^TMX37-50	60	1 A/cm² at 1.9 V_cell	[S5]
NiFeCo	NiFe₂O₄	Sustanion	60	2 A/cm² at 2.13 V_cell	[S6]
NiFeCo	NiFe₂O₄	Sustainion®37	60	1 A/cm² at 1.9 V_cell	[S7]
Ni-MoO₂	Ni_0.6Co_0.2Fe_0.2	Fumasep-3-PE-30	50	1.15 A/cm² at 2 V_cell	[S8]
NiMo/TP-4	NiFe/TP-4	Sustainion®X37-50	50	10 A/cm² at 2.7 V_cell	[S9]
MnP/Gr	NiFeOOH	Sustainion® X37-50 Grade T	50	0.8 A/cm² at 2 V_cell	[S10]
MD-Co/NiS₂	IrO₂	Sustainion X37-50	70	1 A/cm² at 1.97 V_cell	[S11]
HNA-CA-H	HNA-CA-O	Sustainion®X37-50Grade RT	25	1 A/cm² at 1.89 V_cell	[S12]
PdH@Ru	RuO₂	Sustainion® X37-50 Grade T	60	1 A/cm² at 1.8 V_cell	[S13]
NiMo-AS1	NiFe/Ni	Branion	80	3 A/cm² at 2.03 V_cell	[S14]
Pt/C	V-NiFe₂O₄/NF	Sustainion® X37-50 Grade T	50	1 A/cm² at 1.71 V_cell	[S15]
NiFe LDH	r-Ru-Ni/NiO	Fumasep FAA-3-50	25	1 A/cm² at 2.03 V_cell	[S16]
Ni₃N@W₅N₄	NFP	FAA-3-50	60	1 A/cm² at 2.12 V_cell	[S17]
Pt@Co NPC-800	NiCo₂O₄	LDPE-VBC-TMA	60	1.32 A/cm² at 2.34 V_cell	[S18]
Pt/C	B-MOF-Zn-Co	Fumatech FAA-3-PK-130	60	0.55 A/cm² at 2 V_cell	[S19]
Pt/C	NiS_x/Ni(OH)₂ /NiOOH	AF1-HNN8-50	60	1.8 A/cm² at 2 V_cell	[S20]
Pt/C	MOF@POM	Sustainion X37-50 Grade T	80	3 A/cm² at 1.78 V_cell	[S21]

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铁掺杂多孔非晶镍磷酸盐材料制备及阴离子交换膜电解水制氢

Synthesis of Iron-doped Porous Amorphous Nickel Phosphate and Its Application in Hydrogen Production via Anion Exchange Membrane Water Electrolysis

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