Spark Discharge Generation (SDG) was used to produce powders of 10–20nm of Sb and antimony oxides. Different composite materials with different textures were obtained either with an amorphous passive layer of antimony oxide or with crystalline cubic Sb2O3. The composition and shape of the different mixtures, depending on the production and collection conditions, were analysed via XRD and HRTEM coupled with EDX. The effect of the nature and the content of the oxides on the electrode performances were studied using Swagelok cells, cycled galvanostatically with a MACCOR cycler.