Iron fluoride is a kind of high-capacity conversion-type cathode material for lithium-ion batteries (LIBs) and shows attractive practical application potential. However, it still faces many challenges, such as poor electronic conductivity and volume change while cycling. Reducing particle size to nanoscale has been proved to be an effective way to address the poor electronic conductivity and huge volume change of iron fluoride cathodes for LIBs. In this study, a low temperature nanotailoring (LTNT) strategy is proposed to realize the conversion of microsized FeF3 center dot 3H(2)O to nanosized FeF3 center dot 0.33H(2)O by one-step treating with the assistance of alcohols. Meanwhile, the particle size and morphology of iron fluorides can be controlled by regulating the processing conditions. When evaluated as a cathode material for LIBs, the as-prepared bare FeF3 center dot 0.33H(2)O shows a high capacity of 190 mAh g(-1) after 50 cycles with excellent rate capability. This LTNT method is applicable,to hydrates and even can be extended to easily hydrated compounds.