A high pressure gas atomization (HPGA) process has been employed to study microsegregation in LaNi4.75 Sn0.25 and LaNi4.6Si0.4 alloy powders to serve as a basis for further investigations of low cost production of multicomponent alloys in combination with mishmetal (Mm). This investigation is an attempt to produce high quality powders for battery cathode fabrication that can be used in an as-atomized condition without prolong annealing, hydridingdehydriding, and grinding. Argon atomizing gas was used in the HPGA process of the LaNi4.75Sn0.25 and LaNi4.6Si0.4 alloys to investigate rapid solidification effects on microsegregation. Short annealing treatments of 5 minutes at 900°C were able to homogenize both alloy compositions, eliminating solidification micro-segregation along the grain boundaries phases. The rapid homogenization can be attributed primarily to the refined cell structures in gas-atomized particles that provide short diffusion pathways for the dissolving elements.