金属-氧共价性增强的缺陷态高熵岩盐型氧化物用于电催化析氧

doi:10.1016/S1872-2067(21)63794-4

催化学报 ›› 2022, Vol. 43 ›› Issue (1): 122-129.DOI: 10.1016/S1872-2067(21)63794-4

金属-氧共价性增强的缺陷态高熵岩盐型氧化物用于电催化析氧

刘芳名, 于勐, 陈祥, 李金翰, 刘欢欢, 程方益^*()

南开大学化学学院, 先进能源材料化学教育部重点实验室, 新能源转化与存储交叉科学中心, 天津300071

收稿日期:2021-02-04 接受日期:2021-02-19 出版日期:2022-01-18 发布日期:2021-05-06
通讯作者: 程方益
基金资助:
国家重点研发计划纳米科技专项(2017YFA0206700);国家自然科学基金(21925503);国家自然科学基金(21871149);国家自然科学基金(51571125);国家自然科学基金(51622102);111引智计划(B12015)(B12015);中央高校基本科研业务费专项资金

Defective high-entropy rocksalt oxide with enhanced metal-oxygen covalency for electrocatalytic oxygen evolution

Fangming Liu, Meng Yu, Xiang Chen, Jinhan Li, Huanhuan Liu, Fangyi Cheng^*()

Key Laboratory of Advanced Energy Materials Chemistry (Ministry of Education), Renewable Energy Conversion and Storage Center, College of Chemistry, Nankai University, Tianjin 300071, China

Received:2021-02-04 Accepted:2021-02-19 Online:2022-01-18 Published:2021-05-06
Contact: Fangyi Cheng
About author:* Tel: +86-22-23497716; E-mail: fycheng@nankai.edu.cn
Supported by:
Ministry of Science and Technology of the People's Republic of China(2017YFA0206700);National Natural Science Foundation of China(21925503);National Natural Science Foundation of China(21871149);National Natural Science Foundation of China(51571125);National Natural Science Foundation of China(51622102);Ministry of Education of the People's Republic of China(B12015);Fundamental Research Funds for the Central Universities

摘要/Abstract

摘要：

高熵材料可以在单一晶相中引入五种或五种以上元素以优化电子结构和配位环境, 可作为一类新兴的电催化剂. 本文制备了一种岩盐型高熵氧化物Mg_0.2Co_0.2Ni_0.2Cu_0.2Zn_0.2O (HEO)用于催化氧析出反应(OER). 由于相邻的不同金属离子晶格失配, 所制备的HEO具有丰富的缺陷. 此外, 电负性更小的Mg和Zn元素的存在使Co/Ni-O共价性增强. 得益于此, HEO在碱性条件下展现出优异的OER本征催化活性, 其转换频率(TOF)在1.65 V时分别达到CoO和NiO的15和84倍. 本文探究了HEO电催化性能提升机制, 论证了通过合理添加低成本和低电负性元素的高熵策略在发展高效氧电催化剂方面的潜能.
采用静电纺丝和热处理的方法制备了含有五种金属元素的HEO, X射线衍射(XRD)结果表明其为岩盐型晶体结构. X射线能量色散谱(EDS)和电感耦合等离子体发射光谱(ICP-OES)分析表明五种元素接近等摩尔比, 且均匀分布. 通过高分辨透射电子显微镜(HRTEM)发现HEO晶格中含有大量缺陷; 同步辐射扩展X射线吸收精细结构(EXAFS)谱拟合数据显示HEO中Co和Ni的配位数相比CoO和NiO均有所降低, 证实了缺陷的存在. 此外, O 1s的X射线光电子能谱(XPS)和电子顺磁共振谱(EPR)进一步证明HEO含有大量氧缺陷. 缺陷结构有利于配位不饱和的活性位点充分暴露, 促进反应中间体的吸附, 从而提升电催化活性. 通过X射线吸收近边结构(XANES)谱分析了HEO中Co和Ni的电子结构信息. 结果表明, 相比CoO和NiO, HEO中Co和Ni的氧化态更低, 因为HEO中电负性更低的Mg和Zn可以向O转移更多电子, 使相邻的Co和Ni贡献更少电子. 更高的电荷密度说明Co/Ni-O键的共价性增强, 与傅里叶变换的EXAFS谱中Co/Ni-O键的键长变短相吻合. 此外, Co和Ni 2p的XPS结果表明, HEO表面Co(Ⅱ)和Ni(Ⅱ)成分占比较CoO和NiO更高, 也证明HEO中Co/Ni-O键具有更高的共价性.
在1 M KOH中, HEO展现出优越的OER电催化性能, 其达到10 mA cm^-2电流密度时过电位为360 mV, 明显小于CoO和NiO, 且与大多数文献报道的高熵电催化剂相当. 此外, 其Tafel斜率、质量比活性、单位面积活性和TOF均显著优于CoO和NiO, 而采用相同方法制备的Co_0.5Ni_0.5O则性能较差. 据此可以推测HEO电催化性能提升的主要原因在于: 高熵策略可以调控活性金属的电子结构, 通过引入低电负性元素增强Co/Ni-O键的共价性, 提升其本征催化活性; 高熵体系中不同金属元素的尺寸差异导致大量缺陷产生, 调控了活性位点的配位环境, 从而促进活性位点暴露, 提升催化性能.

关键词: 高熵材料, 岩盐型氧化物, 氧析出反应, 电催化剂, 缺陷, 金属-氧共价性

Abstract:

High-entropy materials are emerging electrocatalysts by integrating five or more elements into one single crystallographic phase to optimize the electronic structures and geometric environments. Here, a rocksalt-type high-entropy oxide Mg_0.2Co_0.2Ni_0.2Cu_0.2Zn_0.2O (HEO) is developed as an electrocatalyst towards the oxygen evolution reaction (OER). The obtained HEO features abundant cation and oxygen vacancies originating from the lattice mismatch of neighboring metal ions, together with enlarged Co/Ni-O covalency due to the introduction of less electronegative Mg and Zn. As a result, the HEO exhibits superior intrinsic OER activities, delivering a turnover frequency (TOF) 15 and 84 folds that of CoO and NiO at 1.65 V, respectively. This study provides a mechanistic understanding of the enhanced OER on HEO and demonstrates the potential of high-entropy strategy in developing efficient oxygen electrocatalysts by elaborately incorporating low-cost elements with lower electronegativity.

Key words: High-entropy material, Rocksalt oxide, Oxygen evolution reaction, Electrocatalyst, Defect, Metal-oxygen covalency

刘芳名, 于勐, 陈祥, 李金翰, 刘欢欢, 程方益. 金属-氧共价性增强的缺陷态高熵岩盐型氧化物用于电催化析氧[J]. 催化学报, 2022, 43(1): 122-129.

Fangming Liu, Meng Yu, Xiang Chen, Jinhan Li, Huanhuan Liu, Fangyi Cheng. Defective high-entropy rocksalt oxide with enhanced metal-oxygen covalency for electrocatalytic oxygen evolution[J]. Chinese Journal of Catalysis, 2022, 43(1): 122-129.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(21)63794-4

https://www.cjcatal.com/CN/Y2022/V43/I1/122

图/表 5

Fig. 1. Schematic of the synthetic process and the morphological evolution of the HEO.

Fig. 2. HRTEM image (a) and SAED pattern (b) of the HEO; (c) Magnified HRTEM image of the M zone indicated by the carmine rectangle in panel b, with inset showing the profile plot of the atoms array indicated by the cyan rectangle; (d) HAADF STEM image and the corresponding elemental mapping images of the HEO.

Fig. 3. Co K-edge (a) and Ni K-edge (b) XANES spectra of the materials; Fourier transforms (FT) of Co K-edge (c) and Ni K-edge (d) EXAFS spectra of the materials; Contour plots of Morlet WT of Co K-edge (e) and Ni K-edge (f) EXAFS spectra of the materials.

Fig. 4. Co 2p (a), Ni 2p (b), O 1s (c) XPS spectra and EPR (d) spectra of CoO, NiO and HEO.

Fig. 5. The LSV curves (a) and corresponding Tafel plots (b) of the catalysts in 1 M KOH saturated with O2; (c) Nyquist plots recorded at 1.6 V with the equivalent circuit in the inset; (d) Potential-dependent TOF curves of the catalysts; (e) Nightingale rose diagram showing multi-angle comparisons of the catalysts, with the TOF, mass activities and specific activities evaluated at 1.65 V; (f) Chronopotentiometry profile of HEO at a current density of 10 mA cm-2.

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金属-氧共价性增强的缺陷态高熵岩盐型氧化物用于电催化析氧

Defective high-entropy rocksalt oxide with enhanced metal-oxygen covalency for electrocatalytic oxygen evolution

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