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Ternary NiFeM-LDHs prepared by a scalable epoxide route as active catalysts for alkaline water oxidation
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DOI：10.1016/j.electacta.2026.148890.png)
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Abstract
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The development of highly active and scalable oxygen evolution reaction (OER) catalysts based on earth-abundant elements is essential for the deployment of anion exchange membrane water electrolyzers (AEMWE). NiFe layered double hydroxides (NiFe-LDHs) are recognized as state-of-the-art non-PGM catalysts in alkaline conditions, yet their practical implementation remains limited by the challenges associated with scalable synthesis and restricted compositional tunability. Here, we extend the epoxide-driven homogeneous alkalinization route-recently demonstrated as an industrially compatible method for NiFe-LDH synthesis-to the preparation of a broad library of ternary NiFeM-LDHs (M = divalent or trivalent cations). Time-resolved pH analysis reveals a precipitation behavior governed by the intrinsic hydrolysis constants, solubility products, and water-exchange kinetics of each cation, enabling the incorporation of most transition-metal dopants while highlighting clear limitations for alkaline-earth and soft divalent metals. Structural and compositional analysis (XRD, FTIR, Raman, ICP-MS and SEM-EDX) confirms the formation of low crystalline LDH phases for the majority of compositions, with homogeneous metal distribution except in systems containing Sn, Cu, Ca, and Ba. Electrochemical testing under alkaline conditions shows that all ternary LDHs outperform bare Ni foam, and only Co-, Al-, and Cr-doped samples deliver statistically significant improvements over NiFe-LDH (Welch's t-test, n = 3, alpha = 0.02). Scanning flow cell coupled ICP-MS measurements show that NiFeAl and NiFeCo catalysts remain highly stable with no detectable metal dissolution, while NiCr and NiFeCr display Cr loss. Notably, NiFeCr exhibits increased activity despite some Cr dissolution, likely due to enhanced porosity and electroactive surface area. This work establishes the epoxide route as a versatile and scalable platform for accessing ternary LDHs, paving the way toward multimetallic LDH catalysts optimized for alkaline water splitting.
Keywords:
Anion exchange membrane water electrolysis
Oxygen evolution reaction
Ternary LDHs
Scalable synthesis
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