Single crystal of tristhiourea cadmium sulphate (TTCS) was grown by slow cooling technique. Grown crystals have been characterized using single crystal XRD, Fourier Transform Infrared (FTIR) and Raman spectroscopy, TGA/DTA, UV-vis-NIR and etching studies. Optically transparent and defect free single crystals of size up to 13×08×07 mm3 were harvested in a period of 25 days. Presence of different functional groups in the TTCS crystal was discussed through FTIR and Raman spectra. Transmittance of the crystal revealed that the crystal suitable candidates for optoelectronic applications. The thermal character of TTCS was analyzed by TGA/DTA.