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Ultra-fine barium carbonate powders were successfully synthesized using barium chloride dihydrate (BaCl2·2H2O), sodium hydroxide (NaOH) and (NH2)2CO as raw materials, with the help of different guide reagents, by the homogeneous precipitation method using response surface methodology (RSM) and central composite design (CCD). Their phases of prepared BaCO3 powders under the optimal conditions were characterized by X-ray powder diffraction (XRD). The characterization results showed that different guide reagents have an effect on the phase structure and composition of products, while they play significant roles in determining the morphology of products. All of the synthesized ultra-fine barium carbonate powders had typical orthorhombic structures, which were well-crystallized.