alpha-Al(2)O(3) nanocrystalline powder was prepared via precipitation method, and the effect of reactant concentration on the nanocrystal structure was investigated by X-Ray diffraction. Firstly, alpha-Al(2)O(3) phase was analyzed by continuous scanning, first strong peaks of all alpha-Al(2)O(3) phase were step scanned then to determinate the most perfect crystal structure, and the crystal lattice constants and average crystal size of the best crystal structure were calculated finally. The result showed that X-ray diffraction was an elementary and necessary means for the crystal structure study, it also offered a new way to select preparation process, and the application of it would develop along with the develop of new materials. The most perfect alpha-Al(2)O(3) nanocrystal structure was obtained with the reactant solution of 0.65mol/L, and its lattice constants were a-4.746xc-12.917 angstrom and the average crystal size was 59nm.