Semiconductor type Cu2ZnTiS4 (CZTiS) and Cu2ZnSnS4 (CZTS),were synthetized starting from a hydrothermal route from precursor powders such as copper, zinc, tin, titanium isopropoxide and tiocarbammide metal nitrates dissolved in deionized water in concentrations of 1molL-1. Dosed and placed in a steel autoclave equipped with a Teflon jacket under magnetic stirring (150rpm) and at a temperature of 300°C for 24 hours in order to promote the formation of the respective ceramic phases. Segregates have been repeatedly washed with ethanol at all times until obtaining crystalline-looking solids. Subsequently, in order to promote the production of pure crystalline phases, the materials were subjected to a second reaction stage in a tubular furnace at 400°C in flow (50mLmin-1) for the purpose of Reduce the concentration of secondary phases of sulphides. The characterization of the CZTiS and CZTS materials was performed by X-ray Diffraction (XRD) and Raman spectroscopy where the presence of Kesterite type crystalline structures was confirmed in the two materials revealing that the effect of titanium with a higher ionic radius than tin produces a distortion in the cell of the CZTiS material compared to the report for the CZTS system. The results of Scanning Electron Microscopy (SEM), confirm the regular aggregates obtained with composition consistent with the proposal theoretically and validated by Energy-Dispersion X-ray Spectroscopy (EDX) techniques and comparison between secondary emission spectra and Retro-dispersed.