By nitriding electrospun ZnO/ZnGa2O4 composite nanofibers with ammonia gas under different temperatures, (Ga1-xZnx)(N1-yOy) alloy nanostructures (GZNO A-NSs) were obtained. With increasing the nitriding temperature (T-N) from 650 degrees C to 850 degrees C, the morphologies of the products transformed from nanofibers to short fibers and then nanoparticles, while the compositions of gallium and nitrogen (zinc and oxygen) in the products were increased (decreased). Both X-ray diffraction and Raman spectra confirmed the formation and evolvements of the GZNO A-NSs. The formation temperature of alloys was remarkably decreased due to the nanosize effect. At low T-N of 650 degrees C, zinc loss was very small and Ga0.5Zn0.5N0.3O0.7 alloy nanofibers were obtained. It indicated that nitriding electrospun nanofibers at low temperature is a new method to prepare zinc rich GZNO A-NSs. Interestingly, the Raman spectra exhibited one mode and two modes behaviors under the excitation of 488 and 325 nm lasers, respectively. Our results also indicated that Raman spectra excited by 325 nm laser can also be applied to evaluate the compositions of (Ga1-xZnx)(N1-yOy) alloys. (C) 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.