Well-dispersed Nd1.6Eu0.4Zr2O7 solid solutions were successfully prepared by a convenient salt-assisted combustion process using glycine as fuel. The samples were characterized by XRD, Raman, TEM and HRTEM. The results showed that the Nd ion can be partially replaced by Eu ion. The substituted product was still single-phase solid solutions and the crystal form remained unchanged. TEM images showed that the Nd1.6Eu0.4Zr2O7 solid solutions were composed of well-dispersed sphere-shaped nanocrystals with an average size of 30 nm, which is consistent with the value obtained from XRD patterns using the Scherrer formula. Moreover, the fluorescent characterization of the Nd1.6Eu0.4Zr2O7 nanocrystals at 385 nm upon excitation was carried out at room temperature, and the results showed that there were some intense and prevailing emission peaks located at 590-650 nm.