Single crystals of zinc thiosemicarbazide (ZTSCS) sulfate have been grown from solution growth method using slow evaporation technique. The functional groups, structure, mechanical and dielectric behavior have been verified by FT-Raman, powder X-ray diffraction, Vicker’s microhardness and dielectric studies. The functional group present in the title compound was found by FT-Raman studies. The grown crystal was subjected to powder XRD which confirmed that the crystal has monoclinic crystal system. The hardness of the ZTSCS was studied by Vicker’s hardness tester. The dielectric measurements on the powdered sample have been carried out and the variation of dielectric constant and dielectric loss at different frequencies of the applied field has been studied. The results of all the characterization are discussed in detail. © 2015, Sphinx Knowledge House. All rights reserved.