N,N'-Diethyl-3,3'-bicarbazyl (DEBC) and N,N'-Diphenyl-3,3'-bicarbazyl (DPBC) was synthesized by the oxidative coupling reaction. The electrochemical properties of DEBC avd DPBC were characterized by cyclic voltammetric technique. The oxidation of DEBC occurred at 0.56 V and 0.8 V (vs. Ag/Ag(+)) and the reduction also at 0.47 V and 0.72 V, where the carbazole unit might be oxidized and coupled each other irreversibly to from the paired molecules of DEBC. DPBC also showed the reversible oxidation at 0.74 V and 0.97 V and reduction at 0.53 V and 0.77 V respectively. The bandgap energy of DEBC and DPBC were estimated to be 3.16 eV and 3.19 eV, respectively, according to each UV-Vis spectra.