Nanocrystalline Fe3+-doped La2Zr2O7 series solid solutions were prepared by a convenient salt-assisted combustion process using glycine as fuel. The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The results showed the La ion can be partially replaced by Fe ion. The partial substituted products were still single-phase solid solutions and the crystal form remained unchanged. TEM images reveal that the products are composed of well-dispersed square-shaped nanocrystals. The method provides a convenient and low-cost route for the synthesis of nanostructures of oxide materials. The fluorescence of La1.8Fe0.2Zr2O7 nanocrystals was evaluated by the UV-visible absorption spectra and the fluorescence spectra. The results indicate that (LaxFe1-x)2Zr2O7 nanocrystals prepared by this method are a kind of potential fluorescent-emitted material.