Vanadium films were prepared on zinc surfaces by using a solution containing vanadate. Corrosion protection properties of vanadium-treated (V-treated), chromium-treated (Cr-treated), and untreated zinc surfaces in contact with a 3.5 wt.% NaCl solution were studied using potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and neutral salt spray (NSS) tests. According to these results, the V-treated layer significantly improved the corrosion resistance of zinc surfaces. In comparison with the Cr-treated layer, the V-treated layer exhibited a better corrosion resistance. The composition of the V-treated layer was studied using X-ray photoelectron spectroscopy (XPS). XPS measurements indicated that the vanadium layer formed on zinc surfaces and the vanadium-rich coating was a hydrated oxide with a composition of V 2 O 5 , VO 2 , and its hydrates such as V 2 O 5 ⋅nH 2 O and VO(OH) 2 .