Nanozymes, owing to their high stability and cost-effectiveness, present themselves as appealing alternatives to natural enzymes. The rational design of complex metal-organic frameworks (MOFs) hybridization precursors offers significant opportunities for constructing diverse functional nanostructures. This paper introduces a novel strategy, assisted by MOF hybridization, for synthesizing Co3O4/Fe2O3 dual-layer hollow nanoboxes (DLHNBs) via anion exchange, coupled with low-temperature pyrolysis, employing ZIF-67 as the original template. This approach maximizes the advantages of hollow nanostructures, functioning as both nanoreactors and substrate channels, thereby mimicking the action of natural enzymes. The Co3O4/Fe2O3 DLHNBs exhibited the lower steady-state kinetic parameters, indicating a superior affinity between Co3O4/Fe2O3 DLHNBs and H2O2. Furthermore, the sensing application of Co3O4/Fe2O3 DLHNBs nanozymes for the determination of H2O2 and ascorbic acid (AA) was explored by using a colorimetric method. The linear range for H2O2 detection was established at 100-1000 μM, with a limit of detection (LOD) of 2.13 μM. For AA, the linear range was determined to be 5-40 μM, with a calculated LOD of 0.15 μM. This work not only demonstrates the potential of peroxidase-like nanozymes for sensing applications but also provides a valuable reference for the design and synthesis of MOFs-based nanozymes.

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