The synthesis mechanism of Al 3 BC 3 through carbo-thermal reduction process was investigated and the processing conditions were optimized using Al(OH) 3 B 2 O 3 C as starting materials. The mass change and phase formation of the compacts were analyzed with varying temperature. Excess Al(OH) 3 and B 2 O 3 were required compared to the stoichiometric composition due to the loss of the source materials by vaporization at 1,5001,600°C. At 1,600°C, Al 2 O gas began to actively react with carbon to form Al 4 C 3 on the carbon particles. Al, Al 2 O and B 2 O 3 gases diffused through Al 4 C 3 layer and reacted with carbon at and above 1,650°C to form Al 3 BC 3 . The formation of hexagonal terrace at the surface of synthesized powder indicated that the gases also reacted at the particle surface with carbon which diffused through the carbide layers. The reactions were completed after calcination at 1,725°C for 4 h or at 1,800°C for 1 h. Gas-solid reactions were the major synthesis mechanism. The optimum composition for the synthesis of the ternary compound was Al(OH) 3 :B 2 O 3 :carbon = 0.7:1.4:0.25 by weight.