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A new approach for in-situ synthesis of crystalline Co–Fe–B nanoparticles was presented in which low temperature methods were developed by using metal chlorides and NaBH4 in an inorganic molten salt environment. Effects of different reaction systems/conditions on the phase formation, thermal behavior and microstructure were investigated. The melting point of reactants and impurities in final powders were reduced by the use of molten salt technique. After a reaction of CoCl2, FeCl3 and NaBH4 at 850 °C in sealed tubes, CoB and Fe3B phases formed separately. After a reaction under Ar flow; however, CoFeB2 solid solution nano powders were obtained in one step at 850 °C with an average size of 60 nm. After annealing at 1100 °C, stable and highly crystalline (CoFe)B2 solid solution phase with a Co:Fe molar ratio of 1:1 was achieved. As-synthesized particles exhibited ferromagnetic property, and possessed a narrow hysteresis curve characteristic of soft magnetic materials. Extended reaction temperature from 650 to 850 °C is seen to produce coercivity enhancement up to 500 Oe without significant reduction in saturation magnetization. On the other hand, after an annealing process and subsequent phase and chemical change, crystalline (CoFe)B2 particles exhibited superparamagnetic property. © 2019 Elsevier B.V.
