Directional Reconstruction of Spent Lithium Cobalt Oxide by Microwave Plasma: Efficient Oxygen Evolution Catalyst from Closed‑Loop Recovered Resources
Corresponding Author: Guiyin Xu
Nano-Micro Letters,
Vol. 18 (2026), Article Number: 327
Abstract
The key challenge of water electrolysis is the high energy barrier of the oxygen intermediate of the oxygen evolution reaction (OER) and the unclear catalytic active sites. The recycling of valuable metals from spent batteries and their reconstruction into high-performance electrolytic water catalysts offers significant economic and environmental benefits. In this work, we report a Co3O4/NiFe-layered double hydroxide heterostructure electrocatalyst by reconstruction of spent LiCoO2 cathode material through microwave plasma treatment and then compositing with NiFe-layered double hydroxides through a simple hydrothermal method. This catalyst achieves a low overpotential of 235 mV at 10 mA cm−2 for OER and exhibits prolonged stability at high current densities when integrated into an alkaline electrolyzer, which surpasses commercial IrO2. In situ spectral analysis and density functional theory demonstrate that the presence of heterostructures between Co3O4 and NiFe-LDH optimizes the charge transport path and reduces the interface resistance. Specifically, the charge redistribution optimizes the adsorption energy of oxygenated intermediates on the Ni and Fe sites, thereby optimizing the reaction pathway and significantly improving the overall OER catalytic efficiency. This work provides a green and scalable way to convert spent metal sources into high-value electrocatalysts, while addressing critical challenges in energy storage and sustainable hydrogen production.
Highlights:
1 A closed-loop recycling route for spent LiCoO2 batteries, converting metal resources into high-value electrocatalysts with environmental and economic merits.
2 Synergistic microwave plasma etching and hydrothermal method enable precise construction of Co3O4/NiFe-LDH heterostructures, optimizing material surface and interface properties.
3 Charge redistribution at the heterointerface regulates oxygen intermediate adsorption, providing a new interfacial engineering idea for low-cost water electrolysis catalysts.
Keywords
Download Citation
Endnote/Zotero/Mendeley (RIS)BibTeX
- K.S. Bejigo, K. Bhunia, J. Kim, C. Lee, S. Back et al., Upcycling end of lithium cobalt oxide batteries to electrocatalyst for oxygen reduction reaction in direct methanol fuel cell via sustainable approach. J. Energy Chem. 82, 148–157 (2023). https://doi.org/10.1016/j.jechem.2023.03.042
- M. Huang, M. Wang, L. Yang, Z. Wang, H. Yu et al., Direct regeneration of spent lithium-ion battery cathodes: from theoretical study to production practice. Nano-Micro Lett. 16(1), 207 (2024). https://doi.org/10.1007/s40820-024-01434-0
- Y. Cao, J. Li, H. Ji, X. Wei, G. Zhou et al., A review of direct recycling methods for spent lithium-ion batteries. Energy Storage Mater. 70, 103475 (2024). https://doi.org/10.1016/j.ensm.2024.103475
- J.J. Roy, S. Rarotra, V. Krikstolaityte, K.W. Zhuoran, Y.D. Cindy et al., Green recycling methods to treat lithium-ion batteries E-waste: a circular approach to sustainability. Adv. Mater. 34(25), 2103346 (2022). https://doi.org/10.1002/adma.202103346
- Y. Zhang, J. Li, W. Zhao, T. Yan, L. Zhang et al., Complete metal recycling from lithium-ion batteries enabled by hydrogen evolution catalyst reconstruction. J. Am. Chem. Soc. 145(50), 27740–27747 (2023). https://doi.org/10.1021/jacs.3c10188
- J. Wang, K. Jia, J. Ma, Z. Liang, Z. Zhuang et al., Sustainable upcycling of spent LiCoO2 to an ultra-stable battery cathode at high voltage. Nat. Sustain. 6(7), 797–805 (2023). https://doi.org/10.1038/s41893-023-01094-9
- Y. Xu, Y. Tian, S. Guo, B. Xu, Y. He et al., Recycling of valuable metals from spent ternary Li-ion batteries for the multi-active site electrocatalysts with high-entropy coordination. Appl. Catal. B Environ. Energy 365, 124976 (2025). https://doi.org/10.1016/j.apcatb.2024.124976
- J. Zhu, Y. Wang, Y. Huang, R.B. Gopaluni, Y. Cao et al., Data-driven capacity estimation of commercial lithium-ion batteries from voltage relaxation. Nat. Commun. 13(1), 2261 (2022). https://doi.org/10.1038/s41467-022-29837-w
- Z. Wang, Y. Chen, F. Zhou, R. Qin, Y. Tian et al., Upcycling spent lithium-ion battery cathodes into cobalt-polyphenol networks by DES dissolution and solvent-induced crystallization. Green Chem. 26(10), 5988–5996 (2024). https://doi.org/10.1039/d4gc01036a
- L. Zhang, Q. Xu, S. Wen, H. Zhang, L. Chen et al., Recycling spent ternary cathodes to oxygen evolution catalysts for pure water anion-exchange membrane electrolysis. ACS Nano 18(33), 22454–22464 (2024). https://doi.org/10.1021/acsnano.4c07340
- K. Shen, T. Zhang, Y. Zhang, W. Tang, W. Dai et al., A sustainable net-negative carbon recycling strategy for spent batteries enabled by paired electrolysis. Chem. Eng. J. 516, 164000 (2025). https://doi.org/10.1016/j.cej.2025.164000
- T. Zhang, K. Yang, C. Wang, S. Li, Q. Zhang et al., Nanometric Ni5P4 clusters nested on NiCo2O4 for efficient hydrogen production via alkaline water electrolysis. Adv. Energy Mater. 8(29), 1801690 (2018). https://doi.org/10.1002/aenm.201801690
- C. Wang, M. Qiu, G. Liang, H. Yan, J. Ma et al., Interfacial electron modulation with ionic liquids: dual optimization of CO2 confinement and charge transfer for enhanced electroreduction on Cu. Langmuir 41(34), 22874–22885 (2025). https://doi.org/10.1021/acs.langmuir.5c02334
- G. Ding, Z. Wang, Z. Chen, Y. Xiao, X. Liu et al., Unsaturated coordination-regulated high-spin nickel sites for selective solar-driven carbon dioxide conversion in pure water. Energy Environ. Sci. 19(2), 486–495 (2026). https://doi.org/10.1039/d5ee04331j
- W. Zhao, Q. Zhang, Y. Zhu, P. Zhao, B. Chen et al., Boosting reaction kinetics and mass transfer of bifunctional co-based oxygen electrocatalyst prepared from CoAl-LDH. Adv. Energy Mater. 13(35), 2301580 (2023). https://doi.org/10.1002/aenm.202301580
- J. Huang, A.H. Clark, N. Hales, C.N. Borca, T. Huthwelker et al., Spectroscopic investigations of complex electronic interactions by elemental doping and material compositing of cobalt oxide for enhanced oxygen evolution reaction activity. Adv. Funct. Mater. 34(44), 2405384 (2024). https://doi.org/10.1002/adfm.202405384
- R. Lv, L. Wang, J. Lan, Z. Zhao, X. Liu et al., Nanoconfined Co3O4 in hollow carbon spheres unlocks synergistic nonradical pathways for superior persulfate activation. Chem. Eng. J. 526, 171344 (2025). https://doi.org/10.1016/j.cej.2025.171344
- Y. Gao, J. Zhang, H. Jin, G. Liang, L. Ma et al., Regenerating spent graphite from scrapped lithium-ion battery by high-temperature treatment. Carbon 189, 493–502 (2022). https://doi.org/10.1016/j.carbon.2021.12.053
- Z. Ren, H. Li, W. Yan, W. Lv, G. Zhang et al., Comprehensive evaluation on production and recycling of lithium-ion batteries: a critical review. Renew. Sustain. Energy Rev. 185, 113585 (2023). https://doi.org/10.1016/j.rser.2023.113585
- T. Ouaneche, L. Stievano, L. Monconduit, C. Guéry, M.T. Sougrati et al., The art of lithiation revisited: solvent-free room temperature reaction. Energy Storage Mater. 70, 103507 (2024). https://doi.org/10.1016/j.ensm.2024.103507
- Z. Wang, Z. Li, J. Zhong, B. Zhou, J. Liu et al., A low-temperature solid-to-solid reaction for lithium-ion battery recycling and the utilization of defect-enriched Co3O4 from spent LiCoO2 batteries for efficient oxygen evolution reaction. Appl. Catal. B Environ. Energy 349, 123873 (2024). https://doi.org/10.1016/j.apcatb.2024.123873
- G. Chen, B. Yuan, J. Dang, L. Xia, C. Zhang et al., Recycling the spent LiNi1−x−yMnxCoyO2 cathodes for high-performance electrocatalysts toward both the oxygen catalytic and methanol oxidation reactions. Small 20(15), 2306967 (2024). https://doi.org/10.1002/smll.202306967
- M. Shan, S. Xu, Y. Cao, B. Han, X. Zhu et al., Rapid regeneration of graphite anodes via self-induced microwave plasma. Adv. Funct. Mater. 34(48), 2411834 (2024). https://doi.org/10.1002/adfm.202411834
- Y. Zhang, Z. Li, H. Jang, M.G. Kim, J. Cho et al., In situ grown RuNi alloy on ZrNiNx as a bifunctional electrocatalyst boosts industrial water splitting. Adv. Mater. 37(16), e2501586 (2025). https://doi.org/10.1002/adma.202501586
- H. Shi, T.-Y. Dai, X.-Y. Sun, Z.-L. Zhou, S.-P. Zeng et al., Dual-intermetallic heterostructure on hierarchical nanoporous metal for highly efficient alkaline hydrogen electrocatalysis. Adv. Mater. 36(38), 2406711 (2024). https://doi.org/10.1002/adma.202406711
- G. Ding, J. Zhang, D. Yan, Y. Yu, L. Shuai et al., High-entropy regulation of lattice oxygen p-band toward sustainable electrocatalytic biomass valorization. Nano Lett. 25(22), 8984–8992 (2025). https://doi.org/10.1021/acs.nanolett.5c01259
- X. Li, M. Chen, Y. Ye, C. Chen, Z. Li et al., Electronic structure modulation of nickel sites by cationic heterostructures to optimize ethanol electrooxidation activity in alkaline solution. Small 19(18), e2207086 (2023). https://doi.org/10.1002/smll.202207086
- P.A. Shinde, V. Mahamiya, M. Safarkhani, N.R. Chodankar, M. Ishii et al., Unveiling the nanoarchitectonics of interfacial electronic coupling in atomically thin 2D WO3/WSe2 heterostructure for sodium-ion storage in aqueous system. Adv. Funct. Mater. 34(41), 2406333 (2024). https://doi.org/10.1002/adfm.202406333
- J. Zhang, Y. Yang, G. Ding, Z. Wang, P. Wang et al., Electrooxidation of biomass-derived 5-hydroxymethylfurfural over sulfur-doped nickel–iron layered double hydroxides nanosheets. Chem. Eng. J. 505, 159165 (2025). https://doi.org/10.1016/j.cej.2024.159165
- J. Zhang, D. Yan, G. Ding, X. Wang, C. Li et al., Dual co sites in n─n type heterojunction enable selective electrochemical co-valorization of HMF and CO2. Angew. Chem. Int. Ed. 64(37), e202511448 (2025). https://doi.org/10.1002/anie.202511448
- D. Malhotra, D.T. Tran, S. Prabhakaran, D.H. Kim, N.H. Kim et al., Heterogeneous interface mismatch-manipulated ruthenium-immobilized binary metal phosphide-layered 2D V2CTx for high-efficiency water electrolysis. Chem. Eng. J. 512, 162665 (2025). https://doi.org/10.1016/j.cej.2025.162665
- N. Manivelan, J. Piao, J. Kim, S. Lee, Y. Kim et al., Unveiling the aluminum doping effects of in-situ transmogrified dual-LDH heterostructure and its Fermi-level alignment to water splitting potentials. Adv. Energy Mater. 15(14), 2403889 (2025). https://doi.org/10.1002/aenm.202403889
- Y. Zhang, J. Liu, Y. Xu, C. Xie, S. Wang et al., Design and regulation of defective electrocatalysts. Chem. Soc. Rev. 53(21), 10620–10659 (2024). https://doi.org/10.1039/d4cs00217b
- Y. Zeng, M. Zhao, Z. Huang, W. Zhu, J. Zheng et al., Surface reconstruction of water splitting electrocatalysts. Adv. Energy Mater. 12(33), 2201713 (2022). https://doi.org/10.1002/aenm.202201713
- Z.-Q. Ge, J. Li, H.-J. Zhang, C. Liu, G. Che et al., P–d orbitals coupling heterosites of Ni2P/NiFe-LDH interface enable O─H cleavage for water splitting. Adv. Funct. Mater. 34(40), 2411024 (2024). https://doi.org/10.1002/adfm.202411024
- X. Li, T. Wu, N. Li, S. Zhang, W. Chang et al., Vertically staggered porous Ni2P/Fe2P nanosheets with trace Ru doping as bifunctional electrocatalyst for alkaline seawater splitting. Adv. Funct. Mater. 34(34), 2400734 (2024). https://doi.org/10.1002/adfm.202400734
- W. Luo, Y. Yu, Y. Wu, Z. Ma, X. Ma et al., Realizing efficient oxygen evolution at low overpotential via dopant-induced interfacial coupling enhancement effect. Appl. Catal. B Environ. 336, 122928 (2023). https://doi.org/10.1016/j.apcatb.2023.122928
- J.N. Hausmann, B. Traynor, R.J. Myers, M. Driess, P.W. Menezes, The pH of aqueous NaOH/KOH solutions: a critical and non-trivial parameter for electrocatalysis. ACS Energy Lett. 6(10), 3567–3571 (2021). https://doi.org/10.1021/acsenergylett.1c01693
- B. Zhang, Y. Xu, B. Makuza, F. Zhu, H. Wang et al., Selective lithium extraction and regeneration of LiCoO2 cathode materials from the spent lithium-ion battery. Chem. Eng. J. 452, 139258 (2023). https://doi.org/10.1016/j.cej.2022.139258
- V.S. Sikarwar, M. Hrabovský, G. Van Oost, M. Pohořelý, M. Jeremiáš, Progress in waste utilization via thermal plasma. Prog. Energy Combust. Sci. 81, 100873 (2020). https://doi.org/10.1016/j.pecs.2020.100873
- J. Lv, L. Wang, R. Li, K. Zhang, D. Zhao et al., Constructing a hetero-interface composed of oxygen vacancy-enriched Co3O4 and crystalline-amorphous NiFe-LDH for oxygen evolution reaction. ACS Catal. 11(23), 14338–14351 (2021). https://doi.org/10.1021/acscatal.1c03960
- Z. Liu, H. Yuan, Z. Wan, Z. Ma, X. Deng et al., Nanostructured Co3O4@NiFe-LDH heterojunction catalysts for improving oxygen evolution reaction in alkaline environment. J. Alloys Compd. 983, 173837 (2024). https://doi.org/10.1016/j.jallcom.2024.173837
- B. Wang, X. Chen, Y. He, Q. Liu, X. Zhang et al., Fe2O3/P-doped CoMoO4 electrocatalyst delivers efficient overall water splitting in alkaline media. Appl. Catal. B Environ. 346, 123741 (2024). https://doi.org/10.1016/j.apcatb.2024.123741
- D. Li, D. Xu, Y. Pei, Q. Zhang, Y. Lu et al., Isolated octahedral Pt-induced electron transfer to ultralow-content ruthenium-doped spinel Co3O4 for enhanced acidic overall water splitting. J. Am. Chem. Soc. 146(42), 28728–28738 (2024). https://doi.org/10.1021/jacs.4c07089
- S. Nagappan, H. Gurusamy, H. Minhas, A. Karmakar, S. Ravichandran et al., Unraveling the synergistic role of Sm3+ doped NiFe-LDH as high-performance electrocatalysts for improved anion exchange membrane and water splitting applications. Small Methods 9(5), 2401655 (2025). https://doi.org/10.1002/smtd.202401655
- S. Ye, W. Chen, Z. Ou, Q. Zhang, J. Zhang et al., Harnessing the synergistic interplay between atomic-scale vacancies and ligand effect to optimize the oxygen reduction activity and tolerance performance. Angew. Chem. Int. Ed. 64(2), e202414989 (2025). https://doi.org/10.1002/anie.202414989
- R. Wang, X. Sun, J. Zhong, S. Wu, Q. Wang et al., Low-temperature plasma-assisted synthesis of iron and nitrogen Co-doped CoFeP-N nanowires for high-efficiency electrocatalytic water splitting. Appl. Catal. B Environ. 352, 124027 (2024). https://doi.org/10.1016/j.apcatb.2024.124027
- S. Zhang, C. Tan, R. Yan, X. Zou, F.-L. Hu et al., Constructing built-in electric field in heterogeneous nanowire arrays for efficient overall water electrolysis. Angew. Chem. Int. Ed. 62(26), e202302795 (2023). https://doi.org/10.1002/anie.202302795
- L. Chong, J. Wen, E. Song, Z. Yang, I.D. Bloom et al., Synergistic Co─Ir/Ru composite electrocatalysts impart efficient and durable oxygen evolution catalysis in acid. Adv. Energy Mater. 13(37), 2302306 (2023). https://doi.org/10.1002/aenm.202302306
- X. Teng, Z. Wang, Y. Wu, Y. Zhang, B. Yuan et al., Enhanced alkaline hydrogen evolution reaction of MoO2/Ni3S2 nanorod arrays by interface engineering. Nano Energy 122, 109299 (2024). https://doi.org/10.1016/j.nanoen.2024.109299
- Y. Shi, L. Song, Y. Liu, T. Wang, C. Li et al., Dual cocatalytic sites synergize NiFe layered double hydroxide to boost oxygen evolution reaction in anion exchange membrane water electrolyzer. Adv. Energy Mater. 14(46), 2402046 (2024). https://doi.org/10.1002/aenm.202402046
- T. Zhao, B. Gong, G. Xu, J. Jiang, L. Zhang, in situ surface reconstruction of heterostructure Ni2P/CoP/FeP4 nanowires network catalyst for high-current-density overall water splitting. Chin. J. Catal. 61, 269–280 (2024). https://doi.org/10.1016/S1872-2067(24)60037-9
- H. Liu, Z. Li, J. Hu, Z. Qiu, W. Liu et al., Self-supported cobalt oxide electrocatalysts with hierarchical chestnut burr-like nanostructure for efficient overall water splitting. Chem. Eng. J. 435, 134995 (2022). https://doi.org/10.1016/j.cej.2022.134995
- J. Zhang, X. Zhang, Z. Ma, K. Fang, L. Wang et al., POM-intercalated NiFe-LDH as enhanced OER catalyst for highly efficient and durable water electrolysis at ampere-scale current densities. ACS Catal. 15(8), 6486–6496 (2025). https://doi.org/10.1021/acscatal.5c00448
- X. Liu, Q. Yu, X. Qu, X. Wang, J. Chi et al., Manipulating electron redistribution in Ni2P for enhanced alkaline seawater electrolysis. Adv. Mater. 36(1), e2307395 (2024). https://doi.org/10.1002/adma.202307395
References
K.S. Bejigo, K. Bhunia, J. Kim, C. Lee, S. Back et al., Upcycling end of lithium cobalt oxide batteries to electrocatalyst for oxygen reduction reaction in direct methanol fuel cell via sustainable approach. J. Energy Chem. 82, 148–157 (2023). https://doi.org/10.1016/j.jechem.2023.03.042
M. Huang, M. Wang, L. Yang, Z. Wang, H. Yu et al., Direct regeneration of spent lithium-ion battery cathodes: from theoretical study to production practice. Nano-Micro Lett. 16(1), 207 (2024). https://doi.org/10.1007/s40820-024-01434-0
Y. Cao, J. Li, H. Ji, X. Wei, G. Zhou et al., A review of direct recycling methods for spent lithium-ion batteries. Energy Storage Mater. 70, 103475 (2024). https://doi.org/10.1016/j.ensm.2024.103475
J.J. Roy, S. Rarotra, V. Krikstolaityte, K.W. Zhuoran, Y.D. Cindy et al., Green recycling methods to treat lithium-ion batteries E-waste: a circular approach to sustainability. Adv. Mater. 34(25), 2103346 (2022). https://doi.org/10.1002/adma.202103346
Y. Zhang, J. Li, W. Zhao, T. Yan, L. Zhang et al., Complete metal recycling from lithium-ion batteries enabled by hydrogen evolution catalyst reconstruction. J. Am. Chem. Soc. 145(50), 27740–27747 (2023). https://doi.org/10.1021/jacs.3c10188
J. Wang, K. Jia, J. Ma, Z. Liang, Z. Zhuang et al., Sustainable upcycling of spent LiCoO2 to an ultra-stable battery cathode at high voltage. Nat. Sustain. 6(7), 797–805 (2023). https://doi.org/10.1038/s41893-023-01094-9
Y. Xu, Y. Tian, S. Guo, B. Xu, Y. He et al., Recycling of valuable metals from spent ternary Li-ion batteries for the multi-active site electrocatalysts with high-entropy coordination. Appl. Catal. B Environ. Energy 365, 124976 (2025). https://doi.org/10.1016/j.apcatb.2024.124976
J. Zhu, Y. Wang, Y. Huang, R.B. Gopaluni, Y. Cao et al., Data-driven capacity estimation of commercial lithium-ion batteries from voltage relaxation. Nat. Commun. 13(1), 2261 (2022). https://doi.org/10.1038/s41467-022-29837-w
Z. Wang, Y. Chen, F. Zhou, R. Qin, Y. Tian et al., Upcycling spent lithium-ion battery cathodes into cobalt-polyphenol networks by DES dissolution and solvent-induced crystallization. Green Chem. 26(10), 5988–5996 (2024). https://doi.org/10.1039/d4gc01036a
L. Zhang, Q. Xu, S. Wen, H. Zhang, L. Chen et al., Recycling spent ternary cathodes to oxygen evolution catalysts for pure water anion-exchange membrane electrolysis. ACS Nano 18(33), 22454–22464 (2024). https://doi.org/10.1021/acsnano.4c07340
K. Shen, T. Zhang, Y. Zhang, W. Tang, W. Dai et al., A sustainable net-negative carbon recycling strategy for spent batteries enabled by paired electrolysis. Chem. Eng. J. 516, 164000 (2025). https://doi.org/10.1016/j.cej.2025.164000
T. Zhang, K. Yang, C. Wang, S. Li, Q. Zhang et al., Nanometric Ni5P4 clusters nested on NiCo2O4 for efficient hydrogen production via alkaline water electrolysis. Adv. Energy Mater. 8(29), 1801690 (2018). https://doi.org/10.1002/aenm.201801690
C. Wang, M. Qiu, G. Liang, H. Yan, J. Ma et al., Interfacial electron modulation with ionic liquids: dual optimization of CO2 confinement and charge transfer for enhanced electroreduction on Cu. Langmuir 41(34), 22874–22885 (2025). https://doi.org/10.1021/acs.langmuir.5c02334
G. Ding, Z. Wang, Z. Chen, Y. Xiao, X. Liu et al., Unsaturated coordination-regulated high-spin nickel sites for selective solar-driven carbon dioxide conversion in pure water. Energy Environ. Sci. 19(2), 486–495 (2026). https://doi.org/10.1039/d5ee04331j
W. Zhao, Q. Zhang, Y. Zhu, P. Zhao, B. Chen et al., Boosting reaction kinetics and mass transfer of bifunctional co-based oxygen electrocatalyst prepared from CoAl-LDH. Adv. Energy Mater. 13(35), 2301580 (2023). https://doi.org/10.1002/aenm.202301580
J. Huang, A.H. Clark, N. Hales, C.N. Borca, T. Huthwelker et al., Spectroscopic investigations of complex electronic interactions by elemental doping and material compositing of cobalt oxide for enhanced oxygen evolution reaction activity. Adv. Funct. Mater. 34(44), 2405384 (2024). https://doi.org/10.1002/adfm.202405384
R. Lv, L. Wang, J. Lan, Z. Zhao, X. Liu et al., Nanoconfined Co3O4 in hollow carbon spheres unlocks synergistic nonradical pathways for superior persulfate activation. Chem. Eng. J. 526, 171344 (2025). https://doi.org/10.1016/j.cej.2025.171344
Y. Gao, J. Zhang, H. Jin, G. Liang, L. Ma et al., Regenerating spent graphite from scrapped lithium-ion battery by high-temperature treatment. Carbon 189, 493–502 (2022). https://doi.org/10.1016/j.carbon.2021.12.053
Z. Ren, H. Li, W. Yan, W. Lv, G. Zhang et al., Comprehensive evaluation on production and recycling of lithium-ion batteries: a critical review. Renew. Sustain. Energy Rev. 185, 113585 (2023). https://doi.org/10.1016/j.rser.2023.113585
T. Ouaneche, L. Stievano, L. Monconduit, C. Guéry, M.T. Sougrati et al., The art of lithiation revisited: solvent-free room temperature reaction. Energy Storage Mater. 70, 103507 (2024). https://doi.org/10.1016/j.ensm.2024.103507
Z. Wang, Z. Li, J. Zhong, B. Zhou, J. Liu et al., A low-temperature solid-to-solid reaction for lithium-ion battery recycling and the utilization of defect-enriched Co3O4 from spent LiCoO2 batteries for efficient oxygen evolution reaction. Appl. Catal. B Environ. Energy 349, 123873 (2024). https://doi.org/10.1016/j.apcatb.2024.123873
G. Chen, B. Yuan, J. Dang, L. Xia, C. Zhang et al., Recycling the spent LiNi1−x−yMnxCoyO2 cathodes for high-performance electrocatalysts toward both the oxygen catalytic and methanol oxidation reactions. Small 20(15), 2306967 (2024). https://doi.org/10.1002/smll.202306967
M. Shan, S. Xu, Y. Cao, B. Han, X. Zhu et al., Rapid regeneration of graphite anodes via self-induced microwave plasma. Adv. Funct. Mater. 34(48), 2411834 (2024). https://doi.org/10.1002/adfm.202411834
Y. Zhang, Z. Li, H. Jang, M.G. Kim, J. Cho et al., In situ grown RuNi alloy on ZrNiNx as a bifunctional electrocatalyst boosts industrial water splitting. Adv. Mater. 37(16), e2501586 (2025). https://doi.org/10.1002/adma.202501586
H. Shi, T.-Y. Dai, X.-Y. Sun, Z.-L. Zhou, S.-P. Zeng et al., Dual-intermetallic heterostructure on hierarchical nanoporous metal for highly efficient alkaline hydrogen electrocatalysis. Adv. Mater. 36(38), 2406711 (2024). https://doi.org/10.1002/adma.202406711
G. Ding, J. Zhang, D. Yan, Y. Yu, L. Shuai et al., High-entropy regulation of lattice oxygen p-band toward sustainable electrocatalytic biomass valorization. Nano Lett. 25(22), 8984–8992 (2025). https://doi.org/10.1021/acs.nanolett.5c01259
X. Li, M. Chen, Y. Ye, C. Chen, Z. Li et al., Electronic structure modulation of nickel sites by cationic heterostructures to optimize ethanol electrooxidation activity in alkaline solution. Small 19(18), e2207086 (2023). https://doi.org/10.1002/smll.202207086
P.A. Shinde, V. Mahamiya, M. Safarkhani, N.R. Chodankar, M. Ishii et al., Unveiling the nanoarchitectonics of interfacial electronic coupling in atomically thin 2D WO3/WSe2 heterostructure for sodium-ion storage in aqueous system. Adv. Funct. Mater. 34(41), 2406333 (2024). https://doi.org/10.1002/adfm.202406333
J. Zhang, Y. Yang, G. Ding, Z. Wang, P. Wang et al., Electrooxidation of biomass-derived 5-hydroxymethylfurfural over sulfur-doped nickel–iron layered double hydroxides nanosheets. Chem. Eng. J. 505, 159165 (2025). https://doi.org/10.1016/j.cej.2024.159165
J. Zhang, D. Yan, G. Ding, X. Wang, C. Li et al., Dual co sites in n─n type heterojunction enable selective electrochemical co-valorization of HMF and CO2. Angew. Chem. Int. Ed. 64(37), e202511448 (2025). https://doi.org/10.1002/anie.202511448
D. Malhotra, D.T. Tran, S. Prabhakaran, D.H. Kim, N.H. Kim et al., Heterogeneous interface mismatch-manipulated ruthenium-immobilized binary metal phosphide-layered 2D V2CTx for high-efficiency water electrolysis. Chem. Eng. J. 512, 162665 (2025). https://doi.org/10.1016/j.cej.2025.162665
N. Manivelan, J. Piao, J. Kim, S. Lee, Y. Kim et al., Unveiling the aluminum doping effects of in-situ transmogrified dual-LDH heterostructure and its Fermi-level alignment to water splitting potentials. Adv. Energy Mater. 15(14), 2403889 (2025). https://doi.org/10.1002/aenm.202403889
Y. Zhang, J. Liu, Y. Xu, C. Xie, S. Wang et al., Design and regulation of defective electrocatalysts. Chem. Soc. Rev. 53(21), 10620–10659 (2024). https://doi.org/10.1039/d4cs00217b
Y. Zeng, M. Zhao, Z. Huang, W. Zhu, J. Zheng et al., Surface reconstruction of water splitting electrocatalysts. Adv. Energy Mater. 12(33), 2201713 (2022). https://doi.org/10.1002/aenm.202201713
Z.-Q. Ge, J. Li, H.-J. Zhang, C. Liu, G. Che et al., P–d orbitals coupling heterosites of Ni2P/NiFe-LDH interface enable O─H cleavage for water splitting. Adv. Funct. Mater. 34(40), 2411024 (2024). https://doi.org/10.1002/adfm.202411024
X. Li, T. Wu, N. Li, S. Zhang, W. Chang et al., Vertically staggered porous Ni2P/Fe2P nanosheets with trace Ru doping as bifunctional electrocatalyst for alkaline seawater splitting. Adv. Funct. Mater. 34(34), 2400734 (2024). https://doi.org/10.1002/adfm.202400734
W. Luo, Y. Yu, Y. Wu, Z. Ma, X. Ma et al., Realizing efficient oxygen evolution at low overpotential via dopant-induced interfacial coupling enhancement effect. Appl. Catal. B Environ. 336, 122928 (2023). https://doi.org/10.1016/j.apcatb.2023.122928
J.N. Hausmann, B. Traynor, R.J. Myers, M. Driess, P.W. Menezes, The pH of aqueous NaOH/KOH solutions: a critical and non-trivial parameter for electrocatalysis. ACS Energy Lett. 6(10), 3567–3571 (2021). https://doi.org/10.1021/acsenergylett.1c01693
B. Zhang, Y. Xu, B. Makuza, F. Zhu, H. Wang et al., Selective lithium extraction and regeneration of LiCoO2 cathode materials from the spent lithium-ion battery. Chem. Eng. J. 452, 139258 (2023). https://doi.org/10.1016/j.cej.2022.139258
V.S. Sikarwar, M. Hrabovský, G. Van Oost, M. Pohořelý, M. Jeremiáš, Progress in waste utilization via thermal plasma. Prog. Energy Combust. Sci. 81, 100873 (2020). https://doi.org/10.1016/j.pecs.2020.100873
J. Lv, L. Wang, R. Li, K. Zhang, D. Zhao et al., Constructing a hetero-interface composed of oxygen vacancy-enriched Co3O4 and crystalline-amorphous NiFe-LDH for oxygen evolution reaction. ACS Catal. 11(23), 14338–14351 (2021). https://doi.org/10.1021/acscatal.1c03960
Z. Liu, H. Yuan, Z. Wan, Z. Ma, X. Deng et al., Nanostructured Co3O4@NiFe-LDH heterojunction catalysts for improving oxygen evolution reaction in alkaline environment. J. Alloys Compd. 983, 173837 (2024). https://doi.org/10.1016/j.jallcom.2024.173837
B. Wang, X. Chen, Y. He, Q. Liu, X. Zhang et al., Fe2O3/P-doped CoMoO4 electrocatalyst delivers efficient overall water splitting in alkaline media. Appl. Catal. B Environ. 346, 123741 (2024). https://doi.org/10.1016/j.apcatb.2024.123741
D. Li, D. Xu, Y. Pei, Q. Zhang, Y. Lu et al., Isolated octahedral Pt-induced electron transfer to ultralow-content ruthenium-doped spinel Co3O4 for enhanced acidic overall water splitting. J. Am. Chem. Soc. 146(42), 28728–28738 (2024). https://doi.org/10.1021/jacs.4c07089
S. Nagappan, H. Gurusamy, H. Minhas, A. Karmakar, S. Ravichandran et al., Unraveling the synergistic role of Sm3+ doped NiFe-LDH as high-performance electrocatalysts for improved anion exchange membrane and water splitting applications. Small Methods 9(5), 2401655 (2025). https://doi.org/10.1002/smtd.202401655
S. Ye, W. Chen, Z. Ou, Q. Zhang, J. Zhang et al., Harnessing the synergistic interplay between atomic-scale vacancies and ligand effect to optimize the oxygen reduction activity and tolerance performance. Angew. Chem. Int. Ed. 64(2), e202414989 (2025). https://doi.org/10.1002/anie.202414989
R. Wang, X. Sun, J. Zhong, S. Wu, Q. Wang et al., Low-temperature plasma-assisted synthesis of iron and nitrogen Co-doped CoFeP-N nanowires for high-efficiency electrocatalytic water splitting. Appl. Catal. B Environ. 352, 124027 (2024). https://doi.org/10.1016/j.apcatb.2024.124027
S. Zhang, C. Tan, R. Yan, X. Zou, F.-L. Hu et al., Constructing built-in electric field in heterogeneous nanowire arrays for efficient overall water electrolysis. Angew. Chem. Int. Ed. 62(26), e202302795 (2023). https://doi.org/10.1002/anie.202302795
L. Chong, J. Wen, E. Song, Z. Yang, I.D. Bloom et al., Synergistic Co─Ir/Ru composite electrocatalysts impart efficient and durable oxygen evolution catalysis in acid. Adv. Energy Mater. 13(37), 2302306 (2023). https://doi.org/10.1002/aenm.202302306
X. Teng, Z. Wang, Y. Wu, Y. Zhang, B. Yuan et al., Enhanced alkaline hydrogen evolution reaction of MoO2/Ni3S2 nanorod arrays by interface engineering. Nano Energy 122, 109299 (2024). https://doi.org/10.1016/j.nanoen.2024.109299
Y. Shi, L. Song, Y. Liu, T. Wang, C. Li et al., Dual cocatalytic sites synergize NiFe layered double hydroxide to boost oxygen evolution reaction in anion exchange membrane water electrolyzer. Adv. Energy Mater. 14(46), 2402046 (2024). https://doi.org/10.1002/aenm.202402046
T. Zhao, B. Gong, G. Xu, J. Jiang, L. Zhang, in situ surface reconstruction of heterostructure Ni2P/CoP/FeP4 nanowires network catalyst for high-current-density overall water splitting. Chin. J. Catal. 61, 269–280 (2024). https://doi.org/10.1016/S1872-2067(24)60037-9
H. Liu, Z. Li, J. Hu, Z. Qiu, W. Liu et al., Self-supported cobalt oxide electrocatalysts with hierarchical chestnut burr-like nanostructure for efficient overall water splitting. Chem. Eng. J. 435, 134995 (2022). https://doi.org/10.1016/j.cej.2022.134995
J. Zhang, X. Zhang, Z. Ma, K. Fang, L. Wang et al., POM-intercalated NiFe-LDH as enhanced OER catalyst for highly efficient and durable water electrolysis at ampere-scale current densities. ACS Catal. 15(8), 6486–6496 (2025). https://doi.org/10.1021/acscatal.5c00448
X. Liu, Q. Yu, X. Qu, X. Wang, J. Chi et al., Manipulating electron redistribution in Ni2P for enhanced alkaline seawater electrolysis. Adv. Mater. 36(1), e2307395 (2024). https://doi.org/10.1002/adma.202307395