Abstract： TM0.15Co0.1Zn0.75O nanoparticles with (TM=Ni and Mn) has been successfully synthesized by microwave assisted combustion synthesis method using urea as a fuel. The structural, morphological, compositional and Magnetic properties of these nanoparticles were investigated by X-ray Diffraction Machine (XRD), Scanning Electron Microscopes (FE-SEM JEOL-7001), Energy-Dispersive X-ray Spectroscopy (EDX), and Quantum Design Vibrating Sample Magnetometre (QD-VSM) respectively. The structural properties of both sample showed the formation of Wurtzite structure of ZnO, with nine prominent peaks in which the strong diffraction peaks appear in (100), (002) and (101), respectively, though there is a trace related to the Ni ions observed in the Ni samples. The average sizes of the nanoparticles were estimated using Debye-Scherrer’s equation. There is an increase in the average size between 32.65-34.23nm for Ni ion and a decrease in the size from 32.65-25.71nm for Mn ion. Scanning Electron Microscopes (SEM) showed that smaller crystallites of both samples have sizes smaller than 100nm, no indication of phase separation and little agglomeration was observed. Energy-dispersive X-ray Spectroscopy (EDX) confirmed that all the chemical composition of the samples tallies with the synthesis results. Moreover Magnetic measurement reveal that both samples exhibit a room temperature ferromagnetism though its higher in the sample doped by Ni ions.