Quasi-two-dimensional (Q2D) Nb 2 O 5 nanoflakes were synthesized by combined sol–gel/exfoliation method with the average thickness of 10–25 nm. Their structural, surface- and electro-chemical properties were closely studied and analyzed by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), conductive atomic force microscopy (AFM), Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy techniques.