多配位水分子的焦磷酸锰用于电催化水氧化研究

doi:10.1016/S1872-2067(24)60052-5

催化学报 ›› 2024, Vol. 62: 166-177.DOI: 10.1016/S1872-2067(24)60052-5

多配位水分子的焦磷酸锰用于电催化水氧化研究

杨树姣^a, 江鹏飞^b, 岳楷航^c, 郭凯^a, 杨璐娜^a, 韩金秀^a, 彭欣阳^a, 张学鹏^a, 郑浩铨^a, 杨韬^b, 曹睿^a, 严雅^c^,^*(), 张伟^a^,^*()

^a陕西师范大学化学化工学院, 应用表面与胶体化学教育部重点实验室, 陕西西安 710119
^b重庆大学化学化工学院, 重庆 401331
^c中国科学院上海硅酸盐研究所, 上海 200050

收稿日期:2024-02-22 接受日期:2024-05-14 出版日期:2024-07-18 发布日期:2024-07-10
通讯作者: *电子信箱: zw@snnu.edu.cn (张伟), yanya@mail.sic.ac.cn (严雅).
基金资助:
陕西师范大学启动研究基金;国家自然科学基金(22379088);陕西师范大学优秀研究生培养计划(LHRCYB23005)

Manganese pyrophosphate with multiple coordinated water molecules for electrocatalytic water oxidation

Shujiao Yang^a, Pengfei Jiang^b, Kaihang Yue^c, Kai Guo^a, Luna Yang^a, Jinxiu Han^a, Xinyang Peng^a, Xuepeng Zhang^a, Haoquan Zheng^a, Tao Yang^b, Rui Cao^a, Ya Yan^c^,^*(), Wei Zhang^a^,^*()

^aKey Laboratory of Applied Surface and Colloid Chemistry, Ministry of Education; School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi'an 710119, Shaanxi, China
^bCollege of Chemistry and Chemical Engineering, Chongqing University, Chongqing 401331, China
^cShanghai Institute of Ceramics, Chinese Academy of Sciences (SICCAS), Shanghai 200050, China

Received:2024-02-22 Accepted:2024-05-14 Online:2024-07-18 Published:2024-07-10
Contact: *E-mail: zw@snnu.edu.cn (W. Zhang), yanya@mail.sic.ac.cn (Y. Yan).
Supported by:
Starting Research Funds of Shaanxi Normal University;National Natural Science Foundation of China(22379088);Excellent Graduate Training Program of Shaanxi Normal University(LHRCYB23005)

摘要/Abstract

摘要：

自然界水氧化中心Mn₄CaO₅团簇中的配位水被认为在促进水氧化方面起着重要作用. 许多报道模拟了Mn₄CaO₅结构并研究了其析氧反应(OER)过程, 但配位水结构难以模拟, 在OER过程中的具体功能尚不明确. 目前, 揭示配位水在OER中的具体作用存在以下挑战. 首先, 大多数锰基材料的配位结构, 特别是表面结构是模糊的, 导致结构-性能相关性难以确定. 其次, 在Mn位点上引入配位水时, 往往不可避免地会改变Mn中心的核心结构, 甚至改变Mn的化合价, 这些干扰因素可能严重混淆配位水对OER的影响, 不利于探究OER过程中配位水分子的作用. 因此, 构建一个理想的催化剂平台用于研究配位水分子在水氧化过程中的作用具有重要意义.

本文提出了一种研究OER过程中配位水分子作用的有效方法, 并阐明了OER过程中源于锰中心配位水分子结构-活性关系. 采用水热法合成了一种结晶型焦磷酸锰(crystalline MnPi). 在相同起始物料比、不同反应条件下, 采用共沉淀法制备了分子式相同的非晶型焦磷酸锰(amorphous MnPi). 通过X射线衍射、红外光谱、拉曼光谱、热重分析和理论模拟, 确定了MnPi催化剂的晶体结构(Mn₂P₂O₇·3H₂O). 在0.05 mol L^‒1 pH = 7.0的磷酸盐缓冲溶液中, crystalline MnPi催化剂比amorphous MnPi催化剂表现出更好的OER活性. 晶体结构研究结果表明, crystalline MnPi催化剂暴露的Mn位点上含有四个配位水分子, 并且相邻Mn位点通过氢键相互连接形成连续的氢键网络结构. 连续的氢键网络使氧原子的电荷中和水平更高, 使得crystalline MnPi催化剂中Mn^II/III转换更容易, 进一步揭示了配位水在水氧化机理中扮演的重要角色. 详细的电化学动力学研究、原位/非原位表面表征和理论计算结果表明, crystalline MnPi催化剂的Mn^II/III氧化过程在动力学和热力学上都比amorphous MnPi催化剂容易发生. 同时, crystalline MnPi催化剂中配位水分子有效参与了Mn(II)到Mn(III)的质子耦合电子转移过程, 此过程是锰基体系中水氧化反应中的起始关键步骤. pH动力学实验结果表明, amorphous MnPi催化剂的Mn^II/III氧化步骤为常见的2H⁺/1e单位点过程. 然而, 由于crystalline MnPi催化剂表面暴露的Mn位点上存在多个配位水分子, 导致crystalline MnPi催化剂的Mn^II/III氧化步骤为3H⁺/2e双位点过程. 双位点上的三个配位水分子失去三个质子生成三个OH基团, OH基团通过彼此之间以及与周围配位水分子之间的氢键来有效稳定中间体电荷, 进而促进水氧化的发生.

综上所述, 以精心设计的催化剂平台进行对比研究, 直观地观察和理解了配位水分子对电催化水氧化的重要作用, 为阐明锰基催化体系中配位水分子在水氧化过程中的重要作用提供了有价值的见解.

关键词: 水氧化, 结构, 电催化, 配位水, 磷酸锰

Abstract:

The coordinated water in the Mn₄CaO₅ clusters in natural water oxidation center is believed to play an important role in promoting water oxidation. However, its specific role is unclear. In this work, based on a new manganese phosphate (Mn₂P₂O₇·3H₂O) with well-defined crystal surfaces (crystalline MnPi) and its amorphous counterpart (amorphous MnPi), the effects of coordinated water molecules on water oxidation have been systematically investigated. There are four coordinated water molecules on one Mn site, which is very rare and valuable to study relevant effects from water coordination. Unusually, the crystalline MnPi outperformed the amorphous MnPi in electrocatalysis. The exposed well-defined surface of the crystalline MnPi contains continuous Mn sites with multiple coordinated water molecules. The kinetics and thermodynamics of surface oxidation have been quantitatively studied based on the appealing catalyst platform. The interaction between adjacent Mn sites leads to a 3H⁺/2e dual site oxidation in crystalline MnPi, while this process is 2H⁺/1e single site conversion in amorphous MnPi. The higher level of charge neutralization of oxygen atoms from continuous H-bond network in crystalline MnPi is helpful for the Mn^II/III oxidation, which subsequently promotes water oxidation. This study provides valuable insight into the role of coordinated water molecules in initiating water oxidation in Mn-based catalytic systems.

Key words: Water oxidation, Structure, Electrocatalysis, Coordinated water molecules, Manganese phosphate

杨树姣, 江鹏飞, 岳楷航, 郭凯, 杨璐娜, 韩金秀, 彭欣阳, 张学鹏, 郑浩铨, 杨韬, 曹睿, 严雅, 张伟. 多配位水分子的焦磷酸锰用于电催化水氧化研究[J]. 催化学报, 2024, 62: 166-177.

Shujiao Yang, Pengfei Jiang, Kaihang Yue, Kai Guo, Luna Yang, Jinxiu Han, Xinyang Peng, Xuepeng Zhang, Haoquan Zheng, Tao Yang, Rui Cao, Ya Yan, Wei Zhang. Manganese pyrophosphate with multiple coordinated water molecules for electrocatalytic water oxidation[J]. Chinese Journal of Catalysis, 2024, 62: 166-177.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60052-5

https://www.cjcatal.com/CN/Y2024/V62/I7/166

图/表 5

Fig. 1. The SEM (a,b), TEM (c,d) and HR-TEM (e,f) images of the crystalline MnPi (a,c,e) and amorphous MnPi (b,d,f) samples. (g) The XRD patterns of the MnPi samples, and calculated XRD patterns of MnPi from resolved crystal structure. (h,i) The SEM images and corresponding EDX elemental mapping images of the crystalline MnPi (h) and amorphous MnPi (i) samples.

Fig. 2. (a,b) The XRD patterns of the crystalline MnPi and amorphous MnPi samples treated at different calcination temperatures. The XPS survey scan spectrum (c), the Mn 2p (d) and Mn 3s (e) XPS spectra of the two MnPi samples. The IR spectra (f) and the TGA (g,h) studies of the two MnPi samples. (i) The crystal structures of Mn2P2O7·3H2O (top) and surface atomic configuration of MnPi sample in the (100) crystal plane (bottom).

Fig. 3. LSV (a) and DPV (b) curves of the MnPi samples in 0.05 mol L-1 pH = 7.0 PBS solution. (c) The anodic charging current at 0.84 V plotted against the scan rates, the slope of which is the capacitance of the two samples that is proportional to ECSA. (d,e) The precatalytic oxidation events from DPV of the MnPi samples in electrolytes with different pH values. (f,g) The potential responses of the samples to the pH values of the electrolyte at Epa(MnII/III) (f) and Epa(MnIII/IV) (g).

Fig. 4. (a) The current responses of the electrocatalysts to the KNO3 concentrations in electrolyte under different potentials. (b) DPV curves of the MnPi samples in 0.05 mol L?1 pH = 7.0 PBS solution with 3 mmol L?1 KNO3 concentrations. (c) The potential responses of the electrocatalysts to the KNO3 concentrations of the electrolyte at Epa(MnII/III). (d) Schematic illustration of in-situ EQCM-D experiment. (e) Mass change of the MnPi samples monitored by in-situ EQCM-D experiment in 0.05 mol L?1 pH = 7.0 PBS solution. (f) Bode plots of the MnPi samples at 1.20 V. (g) CA curves obtained from MnPi samples from surface titration by FcDM at 1.20 V substrate potentials. Inset: schematic diagram of the SECM experimental setup. (h) The relative titration charge density from the surface Mn(III) sites. (i) A time-dependent profile for the formation of Mn(III) of the MnPi samples at 1.20 V substrate potentials.

Fig. 5. (a,b) XAS for Mn K-edge of the MnPi samples and standard MnO. (c,d) Mn K-edge EXAFS spectra for the MnPi samples. The insets show details of the denoted boxe areas. (e,f) Proposed Mn(II) to Mn(III) processes of the crystalline MnPi (e) and amorphous MnPi (f) samples. (g) The energy changes for the Mn(II) to Mn(III) of the two samples based on DFT calculations.

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多配位水分子的焦磷酸锰用于电催化水氧化研究

Manganese pyrophosphate with multiple coordinated water molecules for electrocatalytic water oxidation

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