The pure intermetallic compounds (Tb1-xDyx)Fe-2 are super-magnetostriction materials, which were produced from DyFe2 and TbFe2 in this paper. The thermodynamic possibility and kinetic feasible conditions for DyFe2 and TbFe2 preparation by reduction-diffusion in Ca-Dy2O3-Fe and Ca-Tb4O7-Fe systems were analyzed and the products of DyFe2 and TbFe2 were confirmed by XRD. The contracting core model was applied to describe the reduction-diffusion process in which the diffusion is a rate-controlled step. The apparent activation energies of DyFe2 and TbFe2 processes are 45 and 39 kJ/mol respectively.