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It is normally difficult to prepare nano-sized Ba0.5Sr0.5Co0.8Fe0.2O3-δ(BSCF) oxide at high temperature due to its high surface activity. The complexing process, which has successfully applied in the synthesis of nano Sm0.15Ce0.85O1.925 with crystallite size down to 5 nm1, just resulted in a coarse BSCF with crystallite size of 41.9 nm at 900℃. We applied a novel process by simply modifying the solid precursor from the complexing process with concentrated nitric acid treatment.The obtained BSCF powder had a crystallite size of ～25 nm even calcined at 1000C. The small crystallite size is extremely promising to enhance the electrochemical performance of cathode for solid oxide fuel cell dramatically.