Vanadium carbide (VC) nanoparticles were synthesized by a novel refluxing-derived precursor. The organic/inorganic hybrid precursor was prepared by a two-step refluxing method using hydrous V2O5 as vanadium source and n-dodecane as carbon source. The reaction process, phase composition, microstructure, and element composition of VC were investigated by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy (XPS). The results showed that VC nanoparticles could be obtained at 900 A degrees C for 1 h in flowing Argon (Ar), which was much lower than those of conventional synthesis methods. XRD pattern indicated that the product was face-centered cubic VC with a lattice constant a = 4.1626 and average crystallite size of 22.3 nm. Raman spectra indicated that long time refluxing resulted in alkane dehydrogenation and the formation of coke on V2O5 nanoparticles. XPS investigations confirmed oxygen presence in VC lattice. Electron microscopy photographs showed the particle size ranged from 20 to 50 nm. All these results confirmed that the two-step refluxing method was a novel and feasible method to synthesize VC nanoparticles.