The electroless nickel-phosphor deposition on quartz optical fiber surface was carried out by single factor test. The optimum NiSO4·6H2O, NaH2PO2·H2O , C3H6O2 and H3BO3 concentrations, pH value and temperature were determined to be: 0.1331 mol/L, 0.3019 mol/L, C3H6O20.3761 mol/L, H3BO3 0.4520 mol/L, 4.5 and 84°C, respectively. Scanning electron microscope, stereomicroscope and thermal shock rest were applied to measure the morphology and strength of adhesion of the deposited Ni-P coating. The result showed that a desired Ni-P coating with good smoothness and adhesion was prepared under the optimal conditions. The thermodynamic models were established and proven by the current study.