Manipulating the spin configuration by topochemical transformation for optimized intermediates adsorption ability in oxygen evolution reaction

doi:10.1016/S1872-2067(24)60140-3

Chinese Journal of Catalysis ›› 2024, Vol. 66: 195-211.DOI: 10.1016/S1872-2067(24)60140-3

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Manipulating the spin configuration by topochemical transformation for optimized intermediates adsorption ability in oxygen evolution reaction

Jinchang Xu^a^,^b^,¹, Yongqi Jian^a^,¹, Guang-Qiang Yu^a, Wanli Liang^a, Junmin Zhu^a, Muzi Yang^c, Jian Chen^c, Fangyan Xie^c, Yanshuo Jin^a, Nan Wang^a^,^*(), Xi-Bo Li^a^,^*(), Hui Meng^a^,^*()

^aSiyuan laboratory, Guangzhou Key Laboratory of Vacuum Coating Technologies and New Energy Materials, Guangdong Provincial Engineering Technology Research Center of Vacuum Coating Technologies and New Energy Materials, Guangdong Provincial Key Laboratory of Nanophotonic Manipulation, Department of Physics, Jinan University, Guangzhou 510632, Guangdong, China
^bGuangdong Provincial Key Laboratory of Terahertz Quantum Electromagnetics, GBA Branch of Aerospace Information Research Institute, Chinese Academy of Sciences, Guangzhou 510700, Guangdong, China
^cInstrumental Analysis & Research Center, Sun Yat-sen University, Guangzhou 510275, Guangdong, China

Received:2024-06-30 Accepted:2024-09-03 Online:2024-11-18 Published:2024-11-10
Contact: *E-mail: nanwang@email.jnu.edu.cn (N. Wang),lixibo@jnu.edu.cn (X.-B. Li),tmh@jnu.edu.cn (H. Meng).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22478151);National Natural Science Foundation of China(22209056);National Natural Science Foundation of China(22075102);National Natural Science Foundation of China(22005120);National Natural Science Foundation of China(21576301);National Natural Science Foundation of China(51973244);National Natural Science Foundation of China(12174154);National Natural Science Foundation of China(21703081);Guangdong Basic and Applied Basic Research Foundation(2023A1515010270);Guangdong Basic and Applied Basic Research Foundation(2023A1515010921);Natural Science Foundation of Guangdong Province, China(2021A1515010090);Postdoctoral Research Foundation of China(2020M673071);National Innovation and Entrepreneurship Training Program for Undergraduate and the Science and Technology Planning Project of Guangzhou, China(201605030008);National Innovation and Entrepreneurship Training Program for Undergraduate and the Science and Technology Planning Project of Guangzhou, China(202102020963)

Abstract

Abstract:

The underlying spin-related mechanism remains unclear, and the rational manipulation of spin states is challenging due to various spin configurations under different coordination conditions. Therefore, it is urgent to study spin-dependent oxygen evolution reaction (OER) performance through a controllable method. Herein, we adopt a topochemical reaction method to synthesize a series of selenides with e_g occupancies ranging from 1.67 to 1.37. The process begins with monoclinic-CoSeO₃, featuring a distinct laminar structure and Co-O₆ coordination. The topochemical reaction induces significant changes in the crystal field's intensity, leading to spin state transitions. These transitions are driven by topological changes from a Co-O-Se-O-Co to a Co-Se-Co configuration, strengthening the crystalline field and reducing e_g orbital occupancy. This reconfiguration of spin states shifts the rate-determining step from desorption to adsorption for both OER and the hydrogen evolution reaction (HER), reducing the potential-determined step barrier and enhancing overall catalytic efficiency. As a result, the synthesized cobalt selenide exhibits significantly enhanced adsorption capabilities. The material demonstrates impressive overpotentials of 35 mV for HER, 250 mV for OER, and 270 mV for overall water splitting, indicating superior catalytic activity and efficiency. Additionally, a negative relation between e_g filling and OER catalytic performance confirms the spin-dependent nature of OER. Our findings provide crucial insights into the role of spin state transitions in catalytic performance.

Key words: Spin state configuration, e_g orbital occupancy, Intermediates adsorption, Topochemical transformation, Overall water splitting

Jinchang Xu, Yongqi Jian, Guang-Qiang Yu, Wanli Liang, Junmin Zhu, Muzi Yang, Jian Chen, Fangyan Xie, Yanshuo Jin, Nan Wang, Xi-Bo Li, Hui Meng. Manipulating the spin configuration by topochemical transformation for optimized intermediates adsorption ability in oxygen evolution reaction[J]. Chinese Journal of Catalysis, 2024, 66: 195-211.

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Figures/Tables 7

Fig. 1. Orbital occupancy characterizations. (a) Schematic diagram of the topochemical reaction process. (b) The dz2 orbits of m-CoSeO3 and the recombined CoSe1-xO3-n and illustration of the corresponding band structure. (c) The XRD patterns of m-CoSeO3, m-CoSeO3/Co(OH)2, c-CoSe2/o-CoSe2/Co(OH)2 and c-CoSe2/o-CoSe2-V. The plum flowers mark the (110), (002), (112) and (220) planes for monoclinic cobalt selenite hydrate (PDF#52-0048); the rhombuses mark the (001), (100), (101) and (102) planes of hexagonal phase of Co(OH)2 (PDF#30-0443); the triangles mark the (011), (120), (211), (002), (031) and (221) planes of orthorhombic phase CoSe2 (o-CoSe2, PDF#53-0449); and the pentacles mark the (200), (210), (220), (023) and (321) planes of cubic phase CoSe2 (c-CoSe2, PDF#89-2002). (d) The phase components of the four selenides according to the XRD results, listed from top to bottom: m-CoSeO3, m-CoSeO3/Co(OH)2, c-CoSe2/o-CoSe2/Co(OH)2, and c-CoSe2/o-CoSe2-V. (e) The temperature dependence inverse susceptibilities for the selenides. (f) The corresponding eg fillings.

Fig. 2. DFT calculations. (a) The side views of c-CoSe2(210), c-CoSe2/o-CoSe2(210) and c-CoSe2/o-CoSe2-V(210). (b) The free energy diagram of the four steps for the OER on c-CoSe2, c-CoSe2/o-CoSe2, c-CoSe2/o-CoSe2-V, and m-CoSeO3 at the potential U = 0 V. The insets are the adsorption configurations of the intermediates. (c) The free energy diagram for the HER on c-CoSe2, c-CoSe2/o-CoSe2, c-CoSe2/o-CoSe2-V and m-CoSeO3. The insets are configurations of adsorbing hydrogen atoms. (d) Free energy changes of H2O (l) + *O → *OOH + H+ + e- (PDS of c-CoSe2, c-CoSe2/o-CoSe2 and c-CoSe2/o-CoSe2-V) of OER and ΔGH of HER as a function of band centers εw and εp of site atoms, respectively. The site atoms are Co and O atoms, and Se or O atoms for OER and HER, respectively. (e) Partial density of states (PDOS) and schematic diagram of Co 3d orbit filling in m-CoSeO3 (left) and c-CoSe2/o-CoSe2 bulk (right). The dash lines mark the Fermi level.

Fig. 3. Electron microscope characterizations. (a-c) TEM image of m-CoSeO3. (d) The intensity pofiles of the two selected regions and the measured layer distances. (e) Schematic diagram of the double-layer structure of m-CoSeO3. (f) TEM image of c-CoSe2/o-CoSe2-V. (g, j, l and m) High-resolution TEM image of c-CoSe2/o-CoSe2-V. Insets in (l) give the fast Fourier transform (FFT) images of the two regions. Inset in (m) gives the inversed FFT image of (m). (h,n) Aberration corrected HAADF STEM c-CoSe2/o-CoSe2-V with atomic resolution. (i,k) FFT of (h) and (j). (o-q) Geometric phase analysis of the selected area of (n).

Fig. 4. Spectral characterizations. (a) Raman spectrum of m-CoSeO3 and c-CoSe2/o-CoSe2-V. Peak at around 252 cm-1 is indexed to amorphous Se8 rings; Peaks at around 226 and 143 cm-1 are trigonal phase of selenium; Peak at ~171 cm-1 is the bending mode of Se-Se in disordered CoSe; Peak at ~186 cm-1 is the stretching mode of Se-Se. The high-resolution XPS of Se 3d (b) and Co 2p (c) for m-CoSeO3 and c-CoSe2/o-CoSe2-V. The peaks at around 53.7, 54.9, and 58.7 eV corresponded to Se2-, Se0 and Seδ+; The peaks at around 778.8, 779.7, and 781.4 eV correspond to Co 2p3/2 of Co-Se, Co3+ and Co2+. (d) Co K-edge XANES for m-CoSeO3, c-CoSe2/o-CoSe2-V and other reference samples. (e) The fitting of oxidation state from the XANES results. (f) Fourier transform K-edge EXAFS spectra of m-CoSeO3, c-CoSe2/o-CoSe2-V and the corresponding fitting result. The inserted are the crystalline structures of m-CoSeO3 and c-CoSe2/o-CoSe2-V according to the EXAFS results (Blue for Co atoms, golden for Se atoms and red for O atoms.). (g-j) Wavelet transforms of k2-weighted EXAFS signals of m-CoSeO3, c-CoSe2/o-CoSe2-V, CoSe2 and Co3O4.

Fig. 5. Electrochemical OER and HER performance. (a) IR-corrected polarization curves for OER derived from the steady-state test in 1.0 mol-1 KOH. (b) Tafel slopes for as-prepared catalysts for OER derived from the steady-state tests. (c) Nyquist plots for OER at 1.53 V vs. RHE. (d) Cdl for the four selenides extracted from CV results. (e) IR-corrected LSV curves for HER. (f) I-t test at 1.50 V vs. RHE and chronopotentiometry test at j = 10 mA cm-2 for c-CoSe2/o-CoSe2-V. (g) eg filling, Tafel slope, charge-transfer resistance (Rct) and jgeo, 300 mV for the four studied selenides. (h) Relationship of OER catalytic performance with eg filling. (i) Relationship of HER catalytic performance with eg filling.

Fig. 6. Spin configuration of Co under OER condition. (a) Schematic diagram of further splitting of 3d orbits at the edge sites (CoX5 coordination). (b) Schematic diagram of OER coordinate and orbit overlap. (c) The formation of chemical bonds with oxygen-related intermediates in intermediate-spin Co3+ species at the edge sites. The bond order is defined as (nbonding - nanti-bonding)/2, where nbonding and nanti-bonding denote the number of electrons on the bonding or anti-bonding orbits. The bigger the bonder order, the stronger the bond strength. (d) Phase diagram of bond order for different intermediates in egxt2g6-x configuration. The schematic diagram of the selective removal process (e) and the formation of triplet O2 from singlet OH- (f).

Fig. 7. (a) LSV curves for OER and HER for c-CoSe2/o-CoSe2-V, Pt/C and RuO2. (b) η10 for HER, OER and overall water splitting from other recently reported literature. (c) LSV curves for overall water splitting. (d) Chronoamperometry test for overall water splitting.

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Manipulating the spin configuration by topochemical transformation for optimized intermediates adsorption ability in oxygen evolution reaction

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