We describe here for the first time a new morphology of BiOF nanoparticles with a cotton‐like structure, made using a hydrothermal synthesis method. We also prepared heterogeneous nanosheets of BiOF@ZIF‐8 by a one‐pot synthesis under hydrothermal conditions. We demonstrate that in this method the morphology of BiOF and one‐pot synthesis conditions are the main factors for the preparation of the nanosheet BiOF@ZIF‐8. Fourier transform infrared (FTIR), X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy‐dispersive X‐ray (EDX), thermogravimetry‐differential thermal analysis (TG‐DTA), and BET surface area were used to characterize the samples prepared. XRD, SEM, and adsorption–desorption analysis showed that the structure of ZIF‐8 and BiOF form intact only in one‐pot synthesis of BiOF (with nano‐cotton‐like morphology) with Zn(NO3)3, while spectral techniques show the successful encapsulation of the sheet BiOF on ZIF‐8. Nanosheet BiOF@ZIF‐8 was found to be a highly efficient heterogeneous catalyst for the selective oxidation of alcohols. BiOF@ZIF‐8 could be reused several times although it got less active with recycling.
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