Pure and (Ni, Al) co-doped ZnO nanostructures are prepared lucratively by chemical co-precipitation process at room temperature by means of poly ethylene glycol (PEG) as stabilizing agent. Zinc acetate dehydrate and potassium hydroxide are used as preliminary materials. The synthesized samples are characterized by XRD, Scanning Electron Microscopy (SEM) with EDS, Photoluminescence (PL), and Transmission Electron Microscopy (TEM). X-RAY Diffraction pattern reveals that both pristine and co-doped samples acquire hexagonal wurtzite crystal structure with no secondary phase and nonappearance of secondary phase indicates the nonexistence of impurities. SEM descriptions illustrate that all the particles are almost spherical shape and EDAX analysis reveals that doing well incorporation of dopants and lack of impurities. PL spectrum shows that all the samples containing peaks in the visible region, which will be defect related peaks. Doped samples show high intensity peaks compared with the undoped sample. TEM images reveals the nature of the particles as spherical and size of nanoparticles are confirmed the XRD data. HRTEM images plainly be evidence for nanoparticles are about 5nm with unambiguous lattice fringes. Copyright © 2018 VBRI Press.