Abstract In this work, the carbon fibers-reinforced carbon matrix composites made with different carbon char yields of phenolic resin matrix have been characterized by mechanical flexural tests for acoustic emission properties. The composites had been fabricated in the form of two-dimensional polyacrylonitrile based carbon fibers during the carbonization process. It was found that the composites made with the carbon char yield-rich of resin matrix result in better mechanical interfacial properties, i.e., the interlaminar shear strength (ILSS) of the composites. The data obtained from the acoustic emission monitored appeared to show that the composites made with carbon char yield-rich were also more ductile. From the acoustic emission results, the primary composite failure was largely depended on the debonding at interfaces between fibers and matrix. The interlaminar shear strengths of the composites were correlated with the acoustic emission results