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• Investigation of native and passive surface films formed on Ni-20 at.% Cr alloy surfaces. • Surface analysis by in situ electrochemical measurements combined with advanced ex situ surface analysis. • Mechanistic understanding of the effects of high-temperature hydrogen annealing pretreatment. • Enhanced corrosion resistance of electrochemically passivated surface by high-temperature hydrogen annealing pretreatment. • Increase in Cr enrichment of initially weakly protected sites of the inner barrier layer. The effect of high-temperature annealing under hydrogen gas (H 2) surface preparation on a binary polycrystalline Ni-20 at.% Cr alloy was investigated in comparison with conventional mechanical grinding surface preparation. Duplex surface films with inner Cr(III) oxide and outer Ni(II) and Cr(III) hydroxide layers natively formed before and after H 2 annealing were characterized by X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectroscopy. A thinner and less homogeneous inner barrier layer formed after H 2 annealing caused an oxidation peak at the active/passive transition in the linear sweep voltammetry measurement in a 0.5 M H 2 SO 4 solution. Despite this high oxidation peak, passivation of the H 2 annealed surface resulted in the formation of a more corrosion resistant inner layer than on the mechanically ground surface, as demonstrated by electrochemical impedance spectroscopy. The corrosion resistant passive film formation of the H 2 annealed surface is attributed to the increased Cr enrichment of the inner layer caused by the selective Ni dissolution providing corrosion resistance to the initially weakly protected sites of the natively formed surface film. [ABSTRACT FROM AUTHOR]