Single-phased spinel-related titanium-substituted Li0.5Fe2.5O4 has been synthesized by sintering in air a mechanically pre-milled mixture of lithium carbonate, corundum-related iron (III) oxide and the rutile polymorph of titanium (IV) oxide at 700 degrees C (12 h). This temperature is ca. 450-500 degrees C less than the temperatures at which the material is normally prepared by conventional ceramic techniques. On replacing the rutile polymorph of titanium (IV) oxide in the pre-milled mixture by the anatase form the formation of single-phased titanium-substituted Li0.5Fe2.5O4 was not achieved even after sintering the mixture at 1,000 degrees C (12 h).