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Samples of cobalt-doped neodymium orthoferrite compounds, NdCoxFe1-xO3 (0.0 ≤ x ≤ 0.5) were synthesized via glycine auto-combustion between 250 and 300°C and calcined at 500°C for 2 h. X-ray diffraction showed that all compounds had an orthorhombic perovskite structure with space group Pbnm. Increasing cobalt doping gradually reduced the lattice parameters and contracted the unit cell volume. Both X-ray diffraction and scanning electron microscopy showed that the particles were spherical and in the nano-sized range (19-52 nm) with pores