Magister Scientiae - MSc / In this research, novel hybrid perovskite materials were synthesized, characterized and applied in photovoltaic cells (PVCs) to enhance the performance of PVCs. Mixed-organic-cations tin halide perovskites (MOCTPs) were successfully synthesized using sol-gel method. These MOCTPs include guanidinium dimethylammonium tin iodide ([GA][(CH3)2NH2]SnI3) and guanidinium ethylmmonium tin iodide ([GA][CH3CH2NH3]SnI3). The MOCTPs were studied in comparison to their single-organic-cation tin perovskites (SOCTPs), which include guanidinium tin iodide (GASnI3), ethylammonium tin iodide ([CH3CH2NH3]SnI3) and dimethylammonium tin iodide [(CH3)2NH2]SnI3. High Resolution Scanning Electron Microscopy (HR SEM) of the five perovskite materials showed good crystallinity and tetragonal and hexagonal cubic shapes, characteristic of perovskites. These shapes were also confirmed from High Resolution Transmission Electron Microscopy (HR TEM), and the internal structure of the perovskites gave similar zone axes (ZAs) with those obtained from X-ray Diffraction (XRD). XRD showed tetragonal lattice shape for these perovskite materials. Fourier Transform Infrared (FTIR) demonstrated similar functional groups for both the SOCTPs and MOCTPs. FTIR bands that were observed are; N-H, C-H sp3, C-H aldehyde, N-H bend, C-N sp3 and N-H wag. From the 13C Nuclear Magnetic Resonance (NMR) results, the carbon atom of guanidinium iodide precursor shifts from downfield to upfield position, e.g. from 110.57 ppm to 38.49 ppm in GASnI3 SOCTP. This confirms a shift upfield of the carbon atom in guanidinium iodide precursor as it bonded to Sn metal in the perovskite chemical structure. Similar behavior was also observed for the NMR spectra of [GA][CH3CH2NH3]SnI3 MOCTP, where C-2 and C-3 atoms of ethylammonium iodide precursor shifted upfield from 37.03 ppm to 15.69 ppm and 16.06 ppm to 14.39 ppm respectively.