Abstarct: Gas sensors are devices that can be used to detect the precence of the certain gas. Nickel Ferrite(NiFe2O4) is an important mextal oxide semiconductor which has been indicated good sensitivity. In the experiment work, Ni-Ferrite Nanostructures doped with Zn were prepared by Microwave and Sol-Gel Methods and their Nanostructures Morghology, structure and sensing properties were studied. In this methods mextal nitrats and Urea (CO(NH2)2) are as starting materials. The structural properties of synthesized samples were characterized by Field Emission Scanning Electron Microscopy(FESEM) and X-ray diffraction(XRD) and the results show the samples have a cubic spinel structure. The sensing performance of the synthetic Zn-Ni Ferrite (Ni0.6Zn0.4Fe2O4) nanostructures were investigated by three gases: LPG, Acetone and Methanol vaporand. We first investigated the sensing performance of each samples at different working temperatures and the optimized working temperature were for each gases were found. Then the sensing performance of the samples were investigated at various concentrations at optimized temperatures. It was found that the samples have a good selectivity and sensitivity to the aceton vapor compared to the Methanol vapore and LPG gas.