高熵工程促进层状双氢氧化物活性位点构筑用于海水析氧反应

doi:10.1016/S1872-2067(26)65180-7

催化学报 ›› 2026, Vol. 89: 246-257.DOI: 10.1016/S1872-2067(26)65180-7

高熵工程促进层状双氢氧化物活性位点构筑用于海水析氧反应

陈沛然^,¹, 成洛^,¹, 郭从宝, 何语, 刘洋洋, 王毅^*(), 宋树芹^*()

中山大学材料科学与工程学院、化学工程与技术学院,广东省低碳化学与节能重点实验室, PCFM Laboratory,广东广州 510275

收稿日期:2026-04-01 接受日期:2026-05-07 出版日期:2026-10-18 发布日期:2026-09-01
通讯作者: *电子信箱: wangyi76@mail.sysu.edu.cn (王毅),
stsssq@mail.sysu.edu.cn (宋树芹).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(22478450);国家自然科学基金(22478451);国家自然科学基金(22408408);国家催化国家重点实验室(2024SKL-A-013);榆林清洁能源创新研究院能源革命科技专项(E511030817);广东省基础与应用基础研究基金(2021A1515010167);广东省基础与应用基础研究基金(2022A1515011196);广州关键研发计划/项目发布旗舰项目(20220602JBGS02);广州基础与应用基础研究项目(202201011449);中山大学百人研究基金(76110-12230029)

High entropy engineering promoted active sites in layered double hydroxide for seawater oxygen evolution reaction

Peiran Chen^,¹, Luo Cheng^,¹, Congbao Guo, Yu He, Yangyang Liu, Yi Wang^*(), Shuqin Song^*()

The Key Laboratory of Low-carbon Chemistry & Energy Conservation of Guangdong Province, PCFM Laboratory, School of Materials Science and Engineering, School of Chemical Engineering and Technology, Sun Yat-sen University, Guangzhou 510275, Guangdong, China

Received:2026-04-01 Accepted:2026-05-07 Online:2026-10-18 Published:2026-09-01
Contact: *E-mail:wangyi76@mail.sysu.edu.cn(Y. Wang),stsssq@mail.sysu.edu.cn(S. Song).
About author:
¹ Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22478450);National Natural Science Foundation of China(22478451);National Natural Science Foundation of China(22408408);National State Key Laboratory of Catalysis(2024SKL-A-013);Energy Revolution S&T Program of Yulin Innovation Institute of Clean Energy(E511030817);Guangdong Basic and Applied Basic Research Foundation(2021A1515010167);Guangdong Basic and Applied Basic Research Foundation(2022A1515011196);Guangzhou Key R&D Program/Plan Unveiled Flagship Project(20220602JBGS02);Guangzhou Basic and Applied Basic Research Project(202201011449);100 Talent Research Foundation of Sun Yat-sen University(76110-12230029)

摘要/Abstract

摘要：

绿色氢能是实现可再生能源储存和低碳能源转型的重要载体, 电催化水分解为其规模化制备提供了可持续路径. 与依赖高纯水的传统电解体系相比, 海水资源储量丰富、获取便利, 并可与海上风电等可再生能源场景耦合, 因而直接电解海水制氢具有重要应用潜力. 然而, 海水中高浓度氯离子及多种无机离子会引发析氯副反应、活性位点阻塞和电极腐蚀等问题; 同时, 阳极析氧反应(OER)涉及四电子转移, 动力学缓慢, 成为限制碱性海水电解效率和寿命的关键步骤. 因此, 开发兼具高活性、高选择性、耐氯腐蚀和高电流密度稳定性的非贵金属OER电极, 对推动海水电解制氢走向实际应用具有重要意义.

针对传统NiFe基层状双氢氧化物(LDH)在高电流密度下易发生相分离、导电性不足和稳定性衰减等问题, 本文提出高熵组分调控与自支撑电极构筑相结合的设计思路, 通过一步水热法在预处理泡沫Ni (NF)上原位生长由Fe, Ni, Co, Zn和Cr五种非贵金属元素组成的CoNiFeZnCr LDH@NF, 无需黏结剂和后退火处理. Ni, Fe和Co提供可变价态及有利于OER中间体吸附的3d轨道, 而Zn和Cr则有助于稳定晶体结构; 五种金属离子半径差异为14.1%, 满足形成均匀多金属位点的要求. X-射线衍射结果表明, 所得样品保持LDH晶相, 扫描电镜/透射电镜显示其为由超薄纳米片组装而成的纳米花结构, 单片宽度约300 nm; 选区电子衍射、球差电镜及元素映射证明多金属组分均匀分布且未出现明显元素偏析; 诱导耦合等离子体-原子发射光谱计算得到CoNiFeZnCr LDH@NF的构型熵为1.61R, 高于高熵材料判据, 证实其为高熵材料. X-射线光电子能谱分析显示, 该高熵电极表面Ni³⁺比例达到63.93%, Co³⁺比例达到69.18%, 说明多金属耦合作用调节了Ni, Co和Fe的电子结构, 有利于生成OER活性相并优化反应中间体吸附. 在1.0 mol L^-1 KOH中, 对于OER, CoNiFeZnCr LDH@NF在10, 100和500 mA cm^-2下分别仅需174, 234和271 mV过电位, Tafel斜率为42.38 mV dec^-1, 电荷转移电阻低至0.321 Ω, ECSA达到61.75 cm², 均优于CoNiFeZn LDH@NF, CoNiFe LDH@NF, NiFe LDH@NF和IrO₂@NF. 在1.0 mol L^-1 KOH+0.5 mol L^-1 NaCl模拟海水中, 其在10, 100和500 mA cm^-2下的OER过电位分别为179, 245和280 mV, 说明Cl^-的存在仅造成轻微性能衰减. 在更接近实际应用的1.0 mol L^-1 KOH+真实海水中, 该电极在100和500 mA cm^-2下分别仅需250和299 mV的OER过电位, 且从碱性基准电解液切换至真实碱性海水时η₁₀₀仅增加15 mV, 明显低于IrO₂@NF的57 mV, 表明其具有优异海水耐受性. 以排水法在1.0 mol L^-1 KOH+0.5 mol L^-1 NaCl中于500 mA cm^-2定量检测O₂, OER法拉第效率高达99.6%, 证明在该测试条件下OER占主导. 稳定性方面, CoNiFeZnCr LDH@NF在1.0 mol L^-1 KOH+真实海水中以100 mA cm^-2连续运行200 h后电位仅升高41 mV, 而NiFe LDH@NF在70 h内快速失活. 进一步构建CoNiFeZnCr LDH@NF||Pt/C@NF双电极碱性模拟海水电解器, 在500和1000 mA cm^-2下分别仅需1.847和2.017 V, 并可在500 mA cm^-2稳定运行72 h, 电压仅增加86 mV. 密度泛函理论计算表明, 各催化剂OER速控步均为*O向*OOH转化, 而CoNiFeZnCr LDH的ΔG₃最低, 仅为1.37 eV; 同时其d带中心为-2.689 eV, 更接近费米能级, 高熵工程能够使金属d带中心上移、增强电荷转移、优化*O中间体吸附并降低速控步能垒, 从而协同提升碱性海水OER活性、选择性和长期稳定性.

综上, 本文证明高熵工程可有效突破传统LDH在海水OER中的活性与稳定性瓶颈, 并提供了一种简便、可扩展的自支撑非贵金属电极构筑策略. 未来若进一步结合原位表征、真实海水长期测试和器件放大优化, 该类高熵LDH电极有望推动高电流密度海水电解制氢的发展.

关键词: 层状双氢氧化物, 高熵工程, 海水析氧反应, 碱性海水电解, 非贵金属催化剂

Abstract:

Efficient oxygen-evolving electrodes that can operate under high-current-density alkaline water/seawater electrolysis are essential for practical hydrogen production, yet the simultaneous achievement of high activity, chloride tolerance, and long-term durability remains difficult for non-precious-metal catalysts. In this work, a binder-free high-entropy layered double hydroxide electrode has been successfully constructed by directly growing multimetal LDH nanosheets on nickel foam through a facile one-step hydrothermal process. The optimized quinary LDH, composed of five non-noble transition metals, namely Fe, Ni, Co, Zn, and Cr, is denoted as CoNiFeZnCr LDH@NF. Benefiting from the high-entropy multimetal coordination environment, this electrode exhibits superior OER performance compared with the corresponding binary, ternary, and quaternary LDH counterparts. In alkaline seawater, CoNiFeZnCr LDH@NF requires a low OER overpotential of 250 mV to reach 100 mA cm^-2 and shows a Tafel slope of 66.93 mV dec^-1. The electrode also maintains stable operation for 200 h at 100 mA cm^-2, indicating strong resistance to seawater-induced degradation. Density functional theory calculations further reveal that the quinary high-entropy configuration optimizes the adsorption behavior of *O intermediates and lowers the energy barrier of the rate-determining OER step. The improved activity and durability are therefore attributed to the synergistic electronic and structural effects arising from the incorporation of Fe, Ni, Co, Zn, and Cr into the LDH framework. This study demonstrates a practical high-entropy engineering strategy for developing robust non-precious-metal OER electrodes toward seawater-relevant hydrogen production.

Key words: Layered double hydroxide, High entropy engineering, Seawater oxygen evolution reaction, Alkaline seawater electrolysis, Non-precious-metal catalyst

陈沛然, 成洛, 郭从宝, 何语, 刘洋洋, 王毅, 宋树芹. 高熵工程促进层状双氢氧化物活性位点构筑用于海水析氧反应[J]. 催化学报, 2026, 89: 246-257.

Peiran Chen, Luo Cheng, Congbao Guo, Yu He, Yangyang Liu, Yi Wang, Shuqin Song. High entropy engineering promoted active sites in layered double hydroxide for seawater oxygen evolution reaction[J]. Chinese Journal of Catalysis, 2026, 89: 246-257.

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Fig. 1. (a) Schematic illustration for the preparation of CoNiFeZnCr LDH@NF. (b) XRD patterns of LDHs. SEM image (c), TEM image with SAED patterns and HRTEM image (d) (inset: the corresponding lattice fringe pattern) of the CoNiFeZnCr LDH@NF. (e-k) HAADF-STEM image of CoNiFeZnCr LDH@NF and element mappings of CoNiFeZnCr LDH for Ni (green), Fe (yellow), Co (orange), Zn (purple), Cr (indigo), and O (red).

Fig. 2. High-resolution XPS spectra of LDH electrodes. Spectra were collected for CoNiFeZnCr LDH@NF, CoNiFeZn LDH@NF, CoNiFe LDH@NF, and NiFe LDH@NF unless otherwise specified. (a) Ni 2p; (b) Fe 2p; (c) Co 2p (Co-containing samples); (d) Zn 2p (CoNiFeZnCr LDH@NF and CoNiFeZn LDH@NF); (e) Cr 2p (CoNiFeZnCr LDH@NF); (f) O 1s.

Fig. 3. Electrocatalytic performances of the different catalysts in 1.0 mol L-1 KOH solution. (a) LSV curves. (b) Comparison of overpotential and the corresponding current density with the reported data, which detailed information can be found in Table S4. (c) Tafel plots. (d) EIS at a potential of 1.456 V (vs. RHE). (e) ECSA. (f) LSV curves normalized by ECSA.

Fig. 4. LSV curves (a) and EIS (b) of the different catalysts in 1.0 mol L-1 KOH + seawater solution. (c) LSV curves of CoNiFeZnCr LDH@NF in different electrolytes. (d) Overpotentials at 100 and 500 mA cm-2 from polarization curves presented in (c). (e) Measured (dots), theoretical (solid lines) gaseous products, and Faradaic efficiency of CoNiFeZnCr LDH@NF at 500 mA cm-2 in alkaline simulated seawater (1.0 mol L-1 KOH + 0.5 mol L-1 NaCl). (f) LSV curves of CoNiFeZnCr LDH@NF before and after 200 h chronopotentiometry stability test in 1.0 mol L-1 KOH + seawater electrolyte. (g) Stability test with chronopotentiometry on CoNiFeZnCr LDH@NF and NiFe LDH@NF at 100 mA cm-2.

Fig. 5. Overall alkaline simulated seawater electrolysis. (a) Schematic diagram of AWE. (b) LSV curves for the CoNiFeZnCr LDH@NF||Pt/C@NF, CoNiFeZn LDH@NF||Pt/C@NF, and CoNiFe LDH@NF||Pt/C@NF, and NiFe LDH@NF||Pt/C@NF. (c) EIS of CoNiFeZnCr LDH@NF||Pt/C@NF, CoNiFeZn LDH@NF||Pt/C@NF, and CoNiFe LDH@NF||Pt/C@NF, and NiFe LDH@NF||Pt/C@NF. (d) Stability test with chronopotentiometry on CoNiFeZnCr LDH@NF||Pt/C@NF and NiFe LDH@NF||Pt/C@NF at 500 mA cm-2.

Fig. 6. (a) Schematic illustration of the four-step OER process on the surface of the CoNiFeZnCr LDH catalyst. (b) Gibbs free-energy diagram of O-containing intermediates. (c) Calculated DOS for Co, Ni, Fe, Zn, and Cr in CoNiFeZnCr LDH, with the Fermi level indicated by the black dashed line. (d) d-band centers of CoNiFeZnCr LDH, CoNiFeZn LDH, CoNiFe LDH, and NiFe LDH.

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高熵工程促进层状双氢氧化物活性位点构筑用于海水析氧反应

High entropy engineering promoted active sites in layered double hydroxide for seawater oxygen evolution reaction

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