The polymeric material of PCBM-Pd was prepared using both electrochemical and chemical synthesis. The electrochemical formation was performed in acetonitrile/toluene (1:4, v:v) solution containing PCBM, palladium acetate, and tetra(n-C4H9)4NClO4 as the supporting electrolyte. Polymeric film was grown at the Au electrode surface under cyclic voltammetry conditions. Chemical synthesis was done in a benzene solution containing PCBM and Pd2(dba)3∙CHCl3. This study investigates the morphology, structural properties, and photochemical generation of singlet oxygen in this synthesized n-polymer. The morphology of the PCBM-Pd was observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and nitrogen adsorption/desorption isotherms (BETs) were used for the structural characterization of this polymeric material. The formation 1O2 by the photoactive PCBM-Pd polymer was confirmed with 2,3,4,5-tetraphenylcyclopentadienone (TPCPD) as a specific singlet oxygen quencher. Under these conditions, the photo generation of singlet oxygen differs depending on the molar ratio PCBM to Pd. The photochemical generation of singlet oxygen for the PCBM-Pd polymer electrochemically deposited on an ITO electrode and gold foil does not depend on the thickness of the deposited layer.