构筑非晶/晶体NiFe-MOF@NiS异质结构催化剂增强大电流密度下水/海水氧化

doi:10.1016/S1872-2067(24)60030-6

催化学报 ›› 2024, Vol. 61: 192-204.DOI: 10.1016/S1872-2067(24)60030-6

构筑非晶/晶体NiFe-MOF@NiS异质结构催化剂增强大电流密度下水/海水氧化

侯现飚^,¹, 于辰^,¹, 倪腾嘉, 张树聪, 周健, 代水星, 初蕾^*(), 黄明华^*()

中国海洋大学材料科学与工程学院, 山东青岛 266100

收稿日期:2024-01-21 接受日期:2024-03-26 出版日期:2024-06-18 发布日期:2024-06-20
通讯作者: * 电子信箱: chulei@ouc.edu.cn (初蕾),huangminghua@ouc.edu.cn (黄明华).
作者简介:
¹共同第一作者.
基金资助:
国家自然科学基金(52261145700);国家自然科学基金(22279124);山东省自然科学基金(ZR2022ZD30);青岛新能源山东实验室开放项目(QNESL OP202307);中央高校基本科研业务费(202262010)

Constructing amorphous/crystalline NiFe-MOF@NiS heterojunction catalysts for enhanced water/seawater oxidation at large current density

Xianbiao Hou^,¹, Chen Yu^,¹, Tengjia Ni, Shucong Zhang, Jian Zhou, Shuixing Dai, Lei Chu^*(), Minghua Huang^*()

School of Materials Science and Engineering, Ocean University of China, Qingdao 266100, Shandong, China

Received:2024-01-21 Accepted:2024-03-26 Online:2024-06-18 Published:2024-06-20
Contact: * E-mail: chulei@ouc.edu.cn (L. Chu), huangminghua@ouc.edu.cn (M. Huang).
About author:
¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(52261145700);National Natural Science Foundation of China(22279124);Natural Science Foundation of Shandong Province(ZR2022ZD30);Qingdao New Energy Shandong Laboratory Open Project(QNESL OP202307);Fundamental Research Funds for the Central Universities(202262010)

摘要/Abstract

摘要：

电化学水分解作为一种生产高纯度氢气的绿色技术, 虽然前景广阔, 但阳极析氧反应(OER)动力学缓慢, 严重制约了其能量转换效率. 目前, 电化学水分解系统主要以淡水作为原料. 然而, 大规模使用淡水进行分解无疑会给淡水资源带来沉重负担. 相比之下, 占水资源总量96%以上的海水, 因其丰富的储量, 成为替代淡水的理想选择. 然而, 由于海水中含有大量的氯离子, 会引发与OER的竞争性氯析出反应(ClER)形成次氯酸盐(ClO^-), 导致活性位点失活, 严重降低催化剂的活性和稳定性. 因此, 如何在利用海水进行电化学水分解的同时, 有效抑制ClER的发生, 是当前亟待解决的科学问题.
在最新催化剂研究中, 金属有机框架(MOF)凭借其高孔隙率、大比表面积和分散的活性位点, 在电化学水分解中展现出良好的性能. 然而, MOF的电子导电性和OER反应能垒受限于氧原子p轨道与金属原子d轨道间的电子云重叠. 因此, 设计MOF活性位点的电子结构, 促进自发电子转移, 对于提升导电性和OER效率至关重要. 界面工程能优化MOF活性位点的电子结构, 增强局部电荷再分配, 从而提高OER活性. 为满足工业高电流密度需求, 构建富含缺陷的异质结构是关键, 其能暴露更多OER活性位点, 优化质量传递, 缩短电子迁移路径. 结合高导电、可调电子结构的NiS晶体相, 构建MOF非晶/NiS晶体异质界面, 可调控电子结构并加速电荷转移. 目前, 关于MOF基非晶/晶异质界面催化剂用于海水氧化的报道尚少, 这一方向具有巨大潜力.
本文通过两步法耦合策略, 成功在泡沫镍基底上制备了NiFe-MOF@NiS异质结构催化剂. 首先, 利用硫温和改性腐蚀方法在泡沫镍基体生长晶相NiS纳米片; 随后, 通过电沉积处理在NiS表面生长非晶相NiFe-MOF纳米颗粒. 理论计算结果表明, NiFe-MOF和NiS之间的电子相互作用可以加速电荷转移, 有效调节金属位点的d带中心, 从而优化含氧中间体的吸附能力. 与NiFe-MOF和NiS相比, NiFe-MOF@NiS/NF催化剂对OOH*中间体的吸附能力更为突出, 这大大降低了速率决定步骤(O*→OOH*)的反应能垒, 为高效催化OER提供了理论支撑. 实验结果表明, 在1 mol L^‒1 KOH和碱性海水电解液中, NiFe-MOF@NiS/NF催化剂仅需要346和355 mV的低过电位, 即可驱动500 mA cm^-2的大电流密度. Tafel斜率和电化学阻抗谱的结果表明, 该催化剂具有较好的OER动力学特征. 此外, 质量活性和转换频率结果表明, NiFe-MOF@NiS/NF催化剂展现出良好的本征催化活性. 多步恒电流阶梯曲线以及在100和500 mA cm^‒2电流密度下的计时电位曲线结果表明, NiFe-MOF@NiS/NF催化剂具有出色的长期稳定性. 通过对在碱性海水电解液OER反应后的NiFe-MOF@NiS/NF催化剂进行表征发现, 在OER过程中, NiS物种会在阳极电压下自重构形成硫酸盐膜, 可以显著抑制Cl^-离子在催化剂表面的吸附, 使NiFe-MOF@NiS/NF催化剂在海水电解质中具有强大的耐腐蚀性. 这一特性使得NiFe-MOF@NiS/NF催化剂在碱性KOH和碱性海水中均能保持较好的OER活性和稳定性, 性能超过了商业RuO₂以及大多数报道的其他MOF基的催化剂.
综上所述, 本文通过简便易行的合成策略, 制备了高性能的NiFe-MOF@NiS异质结催化剂, 其表现出高效电解海水性能和稳定性. 本工作为合理设计高活性、稳定性、选择性的MOF基抗氯腐蚀催化剂以提高碱性海水的OER性能提供了新视角.

关键词: 金属有机框架, 非晶/晶异质界面, 电催化, 海水氧化, 大电流密度

Abstract:

Developing metal-organic frameworks (MOF) based catalysts with high activity and chlorine corrosion resistance is of paramount importance for seawater oxidation at large current density. Herein, we report a heterogeneous structure coupling NiFe-MOF nanoparticles with NiS nanosheets onto Ni foam (denoted as the NiFe-MOF@NiS/NF) via the mild strategy involving sulfur-modified corrosion and electrodeposition treatment. The constructed amorphous/crystalline interfaces could not only facilitate the adequate infiltration of electrolyte and release of O₂ bubbles at large current densities, but also significantly improve the charge transfer from NiFe-MOF to NiS and the adsorption/desorption capacity of oxygen intermediates. Intriguingly, during oxygen evolution reaction process, the sulfate film formed by the self-reconstruction could remarkably inhibit the adsorption of Cl^- ions on the catalyst surface in the seawater electrolytes. Benefiting from the robust corrosion resistance, unique amorphous/crystalline interfaces, and the charge redistribution, the well-designed NiFe-MOF@NiS/NF exhibits the low overpotential of 346 and 355 mV under a high current density of 500 mA cm^-2 in alkaline water and seawater electrolytes, respectively. More importantly, the as-fabricated NiFe-MOF@NiS/NF demonstrates prolonged stability and durability, lasting over 600 h at a current density of 100 mA cm^-2 in both electrolytes. This study enriches the understanding of electronic structure modulation and chlorine corrosion resistance in seawater, providing broad prospects for designing advanced MOF-based catalysts.

Key words: Metal-organic framework, Amorphous/crystalline heterointerface, Electrocatalyst, Water/seawater oxidation, Large current density

侯现飚, 于辰, 倪腾嘉, 张树聪, 周健, 代水星, 初蕾, 黄明华. 构筑非晶/晶体NiFe-MOF@NiS异质结构催化剂增强大电流密度下水/海水氧化[J]. 催化学报, 2024, 61: 192-204.

Xianbiao Hou, Chen Yu, Tengjia Ni, Shucong Zhang, Jian Zhou, Shuixing Dai, Lei Chu, Minghua Huang. Constructing amorphous/crystalline NiFe-MOF@NiS heterojunction catalysts for enhanced water/seawater oxidation at large current density[J]. Chinese Journal of Catalysis, 2024, 61: 192-204.

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https://www.cjcatal.com/CN/Y2024/V61/I6/192

图/表 6

Fig. 1. (a) Schematic illustration for the fabrication of the NiFe-MOF@NiS/NF. SEM image (b) and TEM image (c) of NiS/NF. SEM image (d) and TEM image (e) of NiFe-MOF/NF. SEM image (f), TEM image (g), HR-TEM image (h), the enlarged HR-TEM image (i) (The inset is the SAED pattern), HAADF-STEM image and corresponding elemental mapping images (j) of NiFe-MOF@NiS/NF.

Fig. 2. Powder XRD patterns (a) and Raman spectra (b) of NiS/NF, NiFe-MOF/NF and NiFe-MOF@NiS/NF. The high resolution XPS spectra of Ni 2p (c), Fe 2p (d), O 1s (e), S 2p (f) for NiS/NF, NiFe-MOF/NF and NiFe-MOF@NiS/NF. The droplet contact angle and the bubble contact angle images of NiS/NF (g), NiFe-MOF/NF (h), and NiFe-MOF@NiS/NF (i).

Fig. 3. The calculated OER free-energy diagram of NiS, NiFe-MOF, and NiFe-MOF@NiS at U = 0 V (a) and U = 1.23 V (b). Charge density difference (c) and energy band diagram (d) of NiFe-MOF@NiS. The DOS of NiS (e), NiFe-MOF (f) and NiFe-MOF@NiS (g). The d-band centers of NiS (h), NiFe-MOF (i) and NiFe-MOF@NiS (j). (k) Proposed OER pathway for the NiFe-MOF@NiS.

Fig. 4. The electrochemical measurements in 1 mol L-1 KOH. LSV curves (a), corresponding Tafel slopes (b), and the EIS (c) of NiS/NF, NiFe-MOF/NF, and NiFe-MOF@NiS/NF. (d) Comparison of the overpotential needed at 100 mA cm-2 among the NiFe-MOF@NiS/NF and previously reported catalysts in 1 mol L-1 KOH. the Cdl values (e), the mass activity (f), and specific activities (g) of NiS/NF, NiFe-MOF/NF, and NiFe-MOF@NiS/NF. (h) The LSV curves before and after 10000 cycles and (i) the time-dependent potential curve at 100 mA cm-2 for NiFe-MOF@NiS/NF.

Fig. 5. TEM (a) and HR-TEM (b) images of NiFe-MOF@NiS/NF after OER test. The high resolution XPS spectra of Ni 2p (c), Fe 2p (d), O 1s (e), and S 2p (f) for NiFe-MOF@NiS/NF before and after OER test. (g) In situ ATR-FTIR spectra of NiFe-MOF@NiS/NF. (h) Schematic graphs of performance interpretation of the NiFe-MOF@NiS/NF.

Fig. 6. The electrochemical measurements in alkaline seawater electrolytes. The LSV curves (a) and corresponding Tafel slopes (b) for NiS/NF, NiFe-MOF/NF, NiFe-MOF@NiS/NF, and RuO2. (c) The EIS of NiS/NF, NiFe-MOF/NF, and NiFe-MOF@NiS/NF. (d) Comparison of the overpotential needed at 100 mA cm-2 among the NiFe-MOF@NiS/NF and previously reported catalysts in alkaline seawater. The Cdl values (e), the TOF (f) (the inset is the TOF value at the overpotential of 370 mV), the mass activity (g) of NiS/NF, NiFe-MOF/NF, and NiFe-MOF@NiS/NF. LSV curves before and after 10000 cycles (h), the multi-potential steps curves (i), and the time-dependent potential curve (j) at 100 mA cm-2 for NiFe-MOF@NiS/NF.

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构筑非晶/晶体NiFe-MOF@NiS异质结构催化剂增强大电流密度下水/海水氧化

Constructing amorphous/crystalline NiFe-MOF@NiS heterojunction catalysts for enhanced water/seawater oxidation at large current density

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