Powders of ZnO and ZnO:M (M = Al 3+ and Sr 2+) with 1 and 4% of M nominal content were synthetized by a hydrothermal method in a diethanolamine (DEA) medium. The samples were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), micro-Raman and photoluminescence (PL). The powder particles were spherical with average radius decreasing from 1 µm down to 70 nm with increasing Al 3+ nominal content but nearly independent on the Sr 2+ nominal content. The XRD and micro-Raman results indicate that both Al 3+ and Sr 2+ mostly incorporated substitutionally into the ZnO lattice, giving rise to compressive and tensile strain, respectively, as a result of ionic radii differences. The PL spectra for ZnO:Al exhibit a dopant-induced contribution at ∼3.1 eV, which is not observed for ZnO:Sr, due to radiative transitions involving trapping of photocarriers at theoretically expected substitutional Al 3+ donor states or at Zn interstitial defects.