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Mechanochemical synthesis of submicron RFeB particles with R = Dy, Nd, Pr has been performed successfully via high energy ball milling of rare-earth oxides, iron oxide and boron oxide in the presence of a reducing agent (Ca) and a dispersant material (CaO), followed by annealing at 800 - 900 °C. In the R = Nd system, we were able to fabricate particles embedded in a CaO matrix with coercivity () of 10.3 kOe after annealing at 900 °C for 5 min. After washing off the dispersant, the was decreased to below 1 kOe because of hydrogen absorption that leads to the formation of the hydrated RFeBH phase that has a lower anisotropy. Upon removal of the hydrogen the coercivity was increased to 3.3 kOe. The average size of the NdFeB particles increases from 100 nm in a sample synthesized at 800 °C to 158 nm at 900 °C. The isotropic DyFeB particles showed a higher coercivity of 21 kOe in washed samples after annealing at 900 °C for 5 min. An average size of 1 nm is measured in samples synthesized at 800 °C and 10 nm at 900 °C. Fitting the high field () measurements in NdFeB to the law of approach to saturation gave values for the magnetocrystalline anisotropy for the washed sample 2.23 × 107 erg/cm3 and for the vacuum annealed sample 4.15 × 107 erg/cm3, both of which are lower than the bulk values. This would explain the lower values of observed in the particles.


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