The material based on 9-bis[4-(thiophen-3,4-yloxy)biphenyl)]-9H-carbazole was successfully synthesized with the oxidative method by using FeCl3 oxidant. A solution of FeCl3 oxidant in chloroform was used for oxidative polymerization process. The obtained compounds had different colors like purple and light yellow. The obtained compounds were characterized by FT-IR and H-1 NMR analyses. The thermal and morphological properties of these compounds were also investigated, and their thermal stabilities were determined by TGA-DTA measurements. Additionally, surface properties of the named polymer as B2 were investigated by scanning electron microscopy. Furthermore, the elemental analysis of the compounds was performed for a more detailed investigation. According to TGA-DTA results, the obtained polymer with FeCl3 oxidant was thermally more stable than its monomer. According to GPC analysis, it can be clearly said that the obtained polymer was a real mono-disperse due to its PDI value. After fluorescence measurements, the synthesized polymer could be used as a material to produce new polymeric or organic light emitting diodes.