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Abstract: Anisotropic SmCo5 nanoflakes prepared by high-energy ball-milling with surfactants have great potential in applications for high-performance nanocomposite magnets. For such “nanocomposite” applications, the surface structure and chemistry of nanoflakes are crucial for achieving high coercivity. In this study, hot-pressed samples from anisotropic SmCo5 nanoflakes, ball-milled with different surfactants, oleic acid (OA) and oleylamine (OY), were investigated. Interface layers between the SmCo5 nanoflakes were found to consist of samarium oxides and a soft magnetic Co phase. These surface layers contribute to the degradation of hard magnetic performance, which is confirmed by scanning transmission electron microscopy-energy dispersive X-ray spectroscopy analysis of the cross-section of a single flake ball-milled with OA. Samples milled with OY show a much thinner interface layer in compacted samples, which means that the surface degradation during ball-milling with OY is much less than that with OA. The results show clearly that the choice of proper surfactant and the control of processing parameters are the key factors for improving the surface condition of the nanoflakes and the resulting hard magnetic properties. [Copyright &y& Elsevier]