We report a comprehensive study of two-dimensional (2D) valentinite antimony oxide (β-Sb2O3) exfoliated from its natural bulk form. The flakes exhibit well-defined morphology, low surface roughness, and preserved orthorhombic structure. Raman and infrared nano-spectroscopy reveal distinct vibrational modes, confirming the crystallinity and vibrational anisotropy of the material. Conductive atomic force microscopy shows dielectric breakdown at ⁓0.18 V/nm, consistent with insulating out-of-plane b