Influence of tert-butyl hydroperoxide on VOx nanostructures via hot-injection synthesis

Data of VOx nanostructures with complex morphologies which were synthesized via hot injection using chemically modified VO(acac)₂ precursors. The influence of tert-butyl hydroperoxide (TBHP) on precursor chemistry and structure formation was investigated. Upon hot injection at 300 °C, the modified precursor yields well-defined VOx nanoflower-like and nanocalix-like structures, whereas the unmodified precursors produce irregular morphologies, as confirmed by electron microscopy techniques. Electron energy loss spectroscopy analysis indicates a predominant oxidation state consistent with VO₂-like electronic structure. In situ heating X-ray diffraction shows a monoclinic-to-rutile phase transition, confirming the VO₂ character. Together, these findings show that TBHP-driven precursor modification governs nucleation pathways and enables access to complex VOx nanostructures. More broadly, the precursor manipulation strategy outlined here offers design principles that can be extended to the controlled synthesis of diverse metal oxide nanomaterials.