This paper deals with the synthesis of pure and Zn doped samples of Sodium Hexa-titanate (NHT, an Alkali Titanate) by solid-state reaction method and characterization by XRD, SEM and Thermal analysis. The phase of the synthesized samples has been confirmed by XRD and the particle size was estimated using the Debye-Scherrer equation. X-ray diffraction patterns of the samples reveal a single phase with monoclinic structure for both pure and doped samples. Surface morphology and the dimensions of the synthesized materials have been analysed with the help of field emission-scanning electron microscopy at different magnification. To explore the various phases of the samples under thermal conditions thermal analysis (DSC/TGA) has also been performed