The iron and Nickel co-doped in zinc oxide nano-particle, Zn1-x-yFexNiyO {(x=0, y=0), (x=0.05, y=0), (x=0, y=0.05), (x=0.03, y=0.02)} were prepared by Sol-Gel technique. This type of synthesis is used for the manufacture of a Field Effect Transistor (FET) detector which is extremely sensitive, secure, and capable of reproducing. It is also used for the detection of the Piperidine (CH2)5NH (hexahydro pyridone) chemical. The well-closed pack spherical nano-particles of the identified crystalline structure of the usual wurtzite hexagonal phase were achieved by characterization of X-Ray Diffraction (XRD). The blue shift was well observed of Co-doped samples as compared to un-doped or single-doped ZnO nanoparticle samples by UV-visible absorption spectrum. The Fourier Transform Infrared Spectroscopy (FTIR) reveals the existence of chemical bonding and functional groups are established and the occurrence of iron Fe in modes associated with iron Fe in addition to ZnO.  The room temperature ferromagnetism was achieved in single or co-doped (Fe-Ni) with ZnO nanoparticles and is confirmed by magnetic characterization (VSM). It was perceived that magnetic saturation was improved in Fe-Ni Co-doped samples relative to pure or single doped. Also, the characterizations of samples show that the exchange interaction of Ni and Fe dominates over Ni-Ni and Fe-Fe interactions.