Pure and nickel doped alkali titanates Na 2 Ti 6-x Ni x O 13 (where x = 0, 0.04, 0.08, 0.12 mol percentage) were synthesized using conventional solid-state reaction method. Phase of the synthesized samples have been confirmed with the help of X-ray diffraction (XRD) patterns recorded at room temperature (RT). Peak positions of all samples (Na 2 Ti 6-x Ni x O 13 ) exhibited the monoclinic structure. FE-SEM of these samples has been done at 10kV acceleration voltage, in secondary electron mode, at different magnifications to observe morphology (microstructure) and they have been found as rod shaped. Thermal stability of pure and nickel doped titanates was done with the help of differential scanning calorimetry (DSC) in presence of inert gas (nitrogen) from ambient temperature to 800°C, keeping heating and cooling rates 10°C/minute.