Mg0.33Zn0.67Ofilms were prepared on quartz glass substrates by Sol-Gel method. Structures and optical properties of Mg0.33Zn0.67Ofilms were studied. The results of XRD analysis indicates that the Mg0.33Zn0.67Ofilm is hexagonal wurtzite structure and the lattice constants a and c are 0.3265nm and 0.5218 nm respectively. Lattice constants a and c of the Mg0.33Zn0.67O film increased because of the addition of Mg. The image of SEM shows that the Mg0.33Zn0.67O film is homogeneous and its average grain size is about 40nm. The absorption spectrum of the sample reveals that the absorption edge of Mg0.33Zn0.67O film located at 312.3nm and the corresponding forbidden band width is 3.97eV. is by three peaks ，which located at 383.9nm，442.6nm and 532.9nm respectively，constitute the luminescence spectrum of the film. The excitation peak located at 379.9nm.