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Poly(3-hexylthiophene) (P3HT) is a semiconductor polymer that has been proved to be a good electron donor in organic or hybrid solar cells. In this work, a detailed study of P3HT synthesis in CH2Cl2solvent by oxidative method with and without MW assistance has been conducted. Effects of synthesis process parameters on the physical properties of P3HT products and their application in hybrid CdS/P3HT photovoltaic devices were studied. It is observed that the use of MW as well as the reaction time affected the reaction yield and properties of the polymer products. It was found that, by the traditional method (without MW), the maximum yield and the properties of the polymer products were similar after 2 h or 24 h of synthesis. The optimal reaction time with MW for P3HT polymerization in CH2Cl2solvent was 1 h, and the obtained P3HT product showed similar or better properties than those P3HT polymers synthesized by the traditional method in the same solvent. The effect of using MW during the synthesis was to increase yield and crystal size of P3HT. Larger energy conversion efficiency of ITO/CdS/P3HT/CP-Au devices was obtained when the P3HT product had higher molecular weight and head/tail-head/tail (HT-HT) triad contents.