The steam reforming of glycerol over supported nickel catalysts is a promising and costeffective method for producing hydrogen. The activity of nickel catalysts supported on g-Al 2 O 3 is low, primarily due to the formation of inactive nickel species during high temperature calcination in air. In order to address this problem, a Ni/g-Al 2 O 3 catalyst was prepared by calcination at 700 C in a nitrous oxide (N 2 O) environment. The N 2 O calcined catalyst showed an enhanced activity for the steam reforming of glycerol. A variety of characterization techniques (XRD, TPR, XPS and H 2 Chemisorption) confirmed that the high temperature N 2 O calcination resulted in a significant decrease in the levels of nickel aluminate. The N 2 O calcination also led to an enhancement in the amount of NiO as well as nickel ions present on the surface of the catalyst. Interestingly, compared to an air calcined catalyst, the N 2 O calcined catalyst contained larger nickel particles after reduction but the N 2 O calcined catalyst had a much larger nickel surface area and dispersion, which resulted in higher glycerol conversion and hydrogen yield.