. A series of gels with 3Al2O3•2SiO2 were prepared by Sol-gel method and heated at several temperatures for 2 h to synthesize Ti, Fe-doped mullite. The received powers with highest amount of TiO2 and Fe2O3 additive in range of 3.7-5.6 % and 12.5-15.9 % respectively as starting materials were characterized using X-ray powder diffraction (XRD), scanning electron microscopies (SEM) and energy dispersive spectrometry(EDX). Fe3+ and Ti4+ cation has been incorprated into the crystal lattice of mullite unevenly. The overall trend of Ti, Fe-doped mullite powers with additive amount changing is Δa>Δb>Δc(Except sample 5.6Ti-1350 is Δb>Δa>Δc owing to its excess amount of TiO2), and the relative change of Ti, Fe-doped mullite powers is Δc（%）>Δb（%）>Δa（%）(Except sample 5.6Ti-1350 and 15.9Fe-1350 is Δb（%）>Δc（%）>Δa（%） with the maximum amount of dopant ions).