A simple one-pot solvothermal procedure was employed to synthesize N/Al co-doped carbon dots(CDs) with a red emission photoluminescence quantum yield up to 30% in aqueous solution. The particle size, surface functional groups and fluorescent properties of the as-prepared CDs were characterized by atomic force microscopy (AFM), dynamic light scattering (DLS) granulometer, fluorescence spectrometer, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FTIR). The average diameter of the as-prepared N/Al co-doped carbon point particles is 6.5 nm, and CD particles have strong anti-bleaching ability under the influences of high concentration salt ion solution, UV irradiation and temperature change. Meanwhile, these CDs can be developed as a novel fluorescence probe for the detection of H₂O₂ with a detection limit of 1.3 μmol/L. Moreover, there exists a linear correlation between the quenching efficiency of CD fluorescence and the concentration of H₂O₂ within 0.12?1 mmol/L.