Abstract The mechanochemical synthesis of a La 0.67 Ce 0.21 Nd 0.08 Pr 0.04 Ni 5 intermetallic is studied. The intermetallic is synthesised from a mixture of LaNi 5 and La 0.25 Ce 0.52 Nd 0.17 Pr 0.06 Ni 5 . The processes controlling the mechanical alloying are characterised as a function of integrated milling time ( t m ). Effects of fracture and cold welding on the sample are identified by scanning electron microscopy. Compositional, microstructural and structural changes are analysed by energy dispersive spectroscopy and X-ray diffraction. The powder obtained has a particle size distribution of 9 ± 1 μm with an average crystallite size of 370 ± 10 A and strain >10%. The intermetallic compound is annealed in Ar to increase crystallite size and to release strain. The structure is refined by the Rietveld method. Cell parameters are a = 4.982(2) A and c = 3.980(9) A, respectively. The advantage of the synthesis method using intermetallics instead of metals/alloys is discussed along with the characteristics of the powder obtained.