An aqueous solution-based doping strategy was developed for controlled doping impurity atoms into a ZnO nanowire (NW) lattice. Through this approach, antimony-doped ZnO NWs were successfully synthesized in an aqueous solution containing zinc nitrate and hexamethylenetetramine with antimony acetate as the dopant source. By introducing glycolate ions into the solution, a soluble antimony precursor (antimony glycolate) was formed and a good NW morphology with a controlled antimony doping concentration was successfully achieved. A doping concentration study suggested an antimony glycolate absorption doping mechanism. By fabricating and characterizing NW-based field effect transistors (FETs), stable p-type conductivity was observed. A field effect mobility of 1.2 cm 2 V− 1 s− 1 and a carrier concentration of 6× 10 17 cm− 3 were achieved. Electrostatic force microscopy (EFM) characterization on doped and undoped ZnO NWs further illustrated the shift of the metal–semiconductor barrier due to Sb doping. This work provided an effective large-scale synthesis strategy for doping ZnO NWs in aqueous solution.