The influence of ball milling and subsequent calcination of a 1: 1 molar mixture of alpha-Fe2O3 and Li2CO3 on the formation of LiFeO2 has been investigated. Pre-milling was found to lower the temperature of ferrite formation by ca. 200degreesC and a thermally stable gamma-LiFeO2 phase was found to form in the temperature range 500-600degreesC. Slow cooling of the pre-milled mixture calcined at higher temperatures resulted in the formation of some LiFe5O8.