Graphite powders were irradiated by pulsed laser at room temperature and normal pressure and then boiled in perchloric acid. Samples were characterized by high-resolution transmission electron microscopy (HRTEM), electron diffraction pattern (EDP), X-ray diffraction (XRD) pattern, and Raman spectroscopy. The analyses on the HRTEM images, EDP, and XRD show that the diamond particles with a size of about 5 nm are obtained. The shifting and broadening of the diamond peak in Raman spectrum indicate that there are high defect density and residual internal stress in synthetic diamond.