This research paper presents a comprehensive study on the synthesis and characterization of Ester-Siloxane multi block copolymers. Two different synthesis methods, namely the one-prepolymer method and the two-prepolymer method, were employed to prepare the copolymers. The distribution of the Ester segment within the copolymers was analyzed using refractive index and ultraviolet detectors coupled with size exclusion chromatography (SEC). SEC-FTIR spectroscopy was utilized to investigate the distribution and composition of the Siloxane segment. Gel permeation chromatography (GEC) was employed to assess copolymer purity based on Siloxane content. Atomic force microscopy (AFM) was utilized to visualize the morphology of Siloxane domains in the copolymers. The results revealed the presence of well-defined Siloxane-rich domains in the form of spheres. Moreover, the occurrence of spherulitic crystal structures was observed in random copolymers with low Siloxane content and small Siloxane segment length. This research provides valuable insights into the manufacturing process, characterization, and structural aspects of multi-block ester-siloxane polymers, and contributes to the understanding of polymer design, the relationship between composition and molecular structure, and the material properties. Key words: Copolymer, -Siloxane multiblock, One-prepolymer, Two-prepolymer, Polycondensate.