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This paper presents structure investigations of the rapidly cooled Fe66Cu6B19Si5Nb4 alloy. A proper selection of chemical composition enabled in-situ formation of the amorphous-crystalline composite during the melt spinning process. Liquid phase separation into the Fe-rich and the Cu-rich phases was confirmed. The microstructures of alloy, melt-spun from 1723 and 1773 K, are composed of the Fe-rich amorphous matrix and Cu-rich spherical crystalline precipitates. For the higher melt-ejection temperature, no coarse precipitates could be observed. Amorphous nature of the Fe-rich matrix was confirmed by presence of a broad diffraction maximum on the X-ray diffraction patterns, a halo ring on the electron diffraction pattern as well as presence of exothermic effects, related to the crystallization of the Fe-rich amorphous matrix, in the differential scanning calorymetry. Beside presence of copper, revealing positive heat of mixing with iron, relatively large supercooled liquid region, was noticed.