Interfacial and microfailure properties of carbon fiber/epoxy matrix composites were evaluated using both tensile fragmentation and compressive Broutman tests with acoustic emission (AE). Amino-silane and maleic anhydride polymeric coupling agents were used via the dipping and electrodeposition (ED), respectively. Both coupling agents exhibited higher improvements in interfacial shear strength (IFSS) under tensile tests than compressive cases. However, ED treatment showed higher IFSS improvement than dipping case under both tensile and compressive test. The typical microfailure modes including fiber break, matrix cracking, and interlayer failure were observed during tensile test, whereas the diagonal slippage in fiber ends was observed during compressive test. For both the untreated and treated cases AE distributions were separated well under tensile testing. On the other hand, AE distributions were rather closer under compressive tests because of the difference in failure energies between tensile and compressive loading. Under both loading conditions, fiber breaks occurred around just before and after yielding point. Maximum AE voltage fur the waveform of carbon or basalt fiber breakage under tensile tests exhibited much larger than those under compressive tests.