Li4Ti5O12 was prepared by a solid-state reaction of ternary precursor materials TiO2, Li2CO3 and carbon. The precursors were mixed by two methods—a dry and wet process. Different types of carbons (carbon black, high-surface-area carbon, graphite and carbonized polymer) were used. The particle shape and size of the product were connected to the carbon type used in the synthesis. The electrochemical performance and the role of particle shape and size were investigated. The weight loses of ternary powder was monitored by TGA to establish the optimum synthesis temperature. XRD diffraction was used to study the TiO2 residue in the final powder.