Indium and gallium doped ZnO nanoparticles have been prepared by a hydrothermal reaction in ethanol and methoxyethanol. A comprehensive study of the preparation process, including a thorough investigation by TG-FTIR and TG-MS of the thermal-purification procedure, is presented. Moreover, the effect of thermal conditions and dopant concentration on the structural and optical properties is discussed on the basis of XRD, TEM and UV-vis-NIR results. Reported data indicated that the use of methoxyethanol as a solvent allows an enhanced control of nanoparticle size and favours dopant incorporation into zinc oxide. Near infrared absorption of these materials can be strongly affected by increasing the doping level and upon treating nanoparticles under reducing atmosphere. Preliminary study indicated that this effect is greatly enhanced for gallium-doped zinc oxide.