Mn-Fe oxide and Mn-Fe oxide/(50wt%/50wt%) were prepared by ball milling method. XRD data of the prepared samples revealed that hematite and ferrite phase coexisted. Water splitting at 1273K, after thermal reduction at 1573K, was performed 4 times for the samples. Hydrogen production amount was analyzed by GC with TCD detector. Water splitting capacity of Mn-Fe oxide was improved by ball milling with .