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Developing bifunctional electrocatalysts from earth-abundant first-row transition metals for large-scale hydrogen production through water electrolysis is both promising and challenging. This study presents a ternary layered double hydroxide (LDH) as a bifunctional electrocatalyst for the hydrogen evolution reaction (HER) and benzyl alcohol oxidation (BAOR). The synergy between 2D NiFeCo LDH and non-Ti-based Nb 2 CT x MXene enhances electrochemical performance. The electrocatalyst achieves excellent results with a low potential of 1.5 V versus RHE at 100 mA cm⁻ 2 for BAOR, an overpotential of 320 mV at 50 mA cm⁻ 2 for HER, and stability over 100 h. A solar cell-powered HER||BAOR system shows faradaic efficiency of ≈73.92% for benzaldehyde production and solar-to-hydrogen (STH) efficiency of ≈39.67%. In situ Raman analysis identifies the oxyhydroxide group as the real catalytic active site during BAOR. These findings offer valuable insights for linking fundamental research with technological innovation to address global challenges., (© 2024 Wiley‐VCH GmbH.)

Photocatalytic hydrogen evolution is an environmentally friendly means of energy generation. Although g-C 3 N 4 possesses fascinating features, its inherent shortcomings limit its photocatalytic applications. Therefore, modifying the intrinsic properties of g-C 3 N 4 and introducing cocatalysts are essential to ameliorate the photocatalytic efficiency. To achieve this, metal-like Ti 3 C 2 T x is integrated with crystalline g-C 3 N 4 via a combined salt-assisted and freeze-drying approach to form crystalline g-C 3 N 4 /Ti 3 C 2 T x (CCN/TCT) hybrids with different Ti 3 C 2 T x loading amounts (0, 0.2, 0.3, 0.4, 0.5, 1, 5, 10 wt.%). Benefiting from the crystallization of CN, as evidenced by the XRD graph, and the marvelous conductivity of Ti 3 C 2 T x supported by EIS plots, CCN/TCT/Pt loaded with 0.5 wt.% Ti 3 C 2 T x displays an elevated H2 (2) should be subscripted evolution rate of 2651.93 µmol g -1 h -1 and a high apparent quantum efficiency of 7.26% (420 nm), outperforming CN/Pt, CCN/Pt, and other CCN/TCT/Pt hybrids. The enhanced performance is attributed to the synergistic effect of the highly crystalline structure of CCN that enables fleet charge transport and the efficient dual cocatalysts, Ti 3 C 2 T x and Pt, that foster charge separation and provide plentiful active sites. This work demonstrates the potential of CCN/TCT as a promising material for hydrogen production, suggesting a significant advancement in the design of CCN heterostructures for effective photocatalytic systems., Competing Interests: The authors declare no conflict of interest., (© 2024 The Authors. Global Challenges published by Wiley‐VCH GmbH.)