Quaternary Ni 63 Cu 9 Fe 8 P 20 alloy was prepared using 99.95wt% Ni, 99.95wt% Cu, 99.95wt% Fe and Ni–P master alloy. The precursors were induction melted in quartz tubes under vacuum (10 −2 bar). The microstructure of the alloy was investigated by the use of a light microscope, scanning electron microscope (SEM) with energy dispersive spectroscope (EDS). Analysis of morphology was carried out and volume fraction of microstructural constituents in as-cast state was assessed. Melt spinning was used to produce ribbons from the alloy. The ribbons were then investigated by means of differential scanning calorimetry (DSC) and differential thermal analysis (DTA). High temperature X-ray studies of melt-spun ribbon as a function of temperature were carried in order to characterize thermal stability of the alloy. The results were discussed and compared with other experimental data.