Abstract. Thermally stable macroporous CaSiO 3 , Fe 3! -and Ni 2! -doped (0.5 to 5 mol%) ceramics have been prepared by solution combustion process by mixing respective metal nitrates (oxidizers), fumed silica. Diformol hydrazine is used as a fuel. The combustion products were identified by their X-ray diffraction and thermal gravimetry/differential thermal analysis. Single phases of b-CaSiO 3 and a-CaSiO 3 were observed at 950 and 1200 °C, respectively. The phase transition temperatures of combustion-derived CaSiO 3 were found to be lower compared to those obtained via solid-state reaction method. It is interesting to note that with an increase in the calcination temperature the samples become more porous with an increase in the pore diameter from 0.2 to 8 µm. The electron paramagnetic resonance (EPR) spectrum of Fe 3! ions in CaSiO 3 exhibits a weak signal at g " 4.20 ) 0