Despite different analysis thicknesses, XPS analysis globally confirmed the ToF-SIMS results in terms of Ni/Ti surface ratio. Indeed, a higher reduction temperature increased the Ni/Ti ratio in the case of the Ni(pre)/TiO2(ALG) materials. This agreement between both surface techniques was also observed for the two other samples Ni(post)/TiO2(ALG) and Ni/TiO2(PC500) .