Transition metal containing ZnO powders(Zn1−xMxO,0≤x≤0.30;M = Ni, Mn, Co) have been synthesized by a sol–gel process using zinc acetatedihydrate, respective acetate and oxalic acid as precursors with ethanolas a solvent. The process essentially involves gel formation, drying at80 °C for 24 h to provide the oxalate, and calcination at500 °C for 2 h to undergo an exothermic reaction and yieldZn1−xMxO powder. Their XRD patterns correspond to a wurtzite hcp structure similar to that of pureZnO, but with the lattice parameters varying slightly with type and extent of doping. It isshown that the dissolution of nickel and cobalt in ZnO is less than 10 at.%, whereas that ofmanganese lies between 10 and 15 at.%. Other phases that emerge include NiO (hexagonal,a = 2.954 Å,c = 7.236 Å),ZnCo2O4 (cubic,a = 8.094 Å)and ZnMnO3 (cubic, a = 8.35 Å) in the Ni, Co and Mn containing ZnO systems, respectively. Observations ofhysteresis loops both at 10 and 320 K and the nature of ESR spectra provideevidence for the ferromagnetic state in nickel containing ZnO powder. Besides,the deviation occurs in the magnetization versus temperature curves in zerofield cooled (ZFC) and field cooled (FC) conditions (blocking temperatureTB being 32 K for 5 at.% Ni). The magnetic behaviour of manganese and cobaltdoped zinc oxide is, however, different, namely, (i) no hysteresis loops, (ii)decrease in magnetization with increase of Mn or Co content, and (iii) identicalM–T curves under ZFC and FC conditions. The inverse susceptibility versus temperature curves ofZn1−xMnxO compounds reveal ferrimagnetism with Néel temperatureTN of 4 Kfor x = 0.02, butantiferromagnetism for x = 0.15 and 0.25 with Curie–Weiss temperature of−43 and −30 K, respectively.