A series of Bi substituted yttrium iron garnet (Bi-YIG) nanoparticles with nominal formula of Bi x Y 3-x Fe 5 O 12 , in which x varied in the steps of 0.0, 0.5, 1.0 and 1.5, were prepared via mechanochemical processing (MCP). A milling time of 5 hours was found to be suitable for all the samples. Minimum annealing temperature for completion of the phase formation was determined for each sample. The optimum annealing temperature of each sample is much lower than the annealing temperature for the completion of the related phases in the conventional ceramic technique. The average sizes of the particles were determined by Scherrer's formula and were in the range of 30 nm to 40 nm. The effect of Bi 3+ substitution for Y 3+ on lattice parameters and magnetic properties of pure YIG has been investigated.