In the recent years, rare earth metal (REM) sulfide thin film materials have great attentions due to their unique physical and chemical properties. The porous nanostructured morphology and wide potential window of electrode materials are very important aspects for supercapacitor applications. Therefore, REM sulfides are widely used for gas sensing, photocatalyst, glucose sensing, energy conversion and supercapacitor applications. Among the REM sulfide, ytterbium sulfide (Yb2S3) composite with graphene oxide (GO) is considered as a best candidate for negative electrode material in supercapacitor due to multiple oxidation state, better redox activity, wide potential window and excellent area under the curve. Present book describes a chemical synthetic approaches of successive ionic layer adsorption and reaction (SILAR) and chemical bath deposition (CBD) method for Yb2S3 composite with GO thin film electrodes and their application in supercapacitor. This research highlighted crucial role of the synthesis methods on morphology of Yb2S3 composite with GO electrode materials for supercapacitors.