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The Ni-11Mo-8Al-3Ta-2Cr-1Re spherical powders of <150 μm were successfully prepared by the novel technique called supreme-speed plasma rotating electrode process (SS-PREP). The morphology of the atomized powders was observed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). A formation mechanism of some irregular particles appeared in the powders was described and the differences of their microstructures were analyzed by the image-replicating method. The composition differences of the irregular particles were multi-confirmed by EDS. The particle size distribution (PSD) data of the SS-PREP Ni-11Mo-8Al-3Ta-2Cr-1Re powders were well simulated with the newly reported double peak atomization assumption. The relationship between the particle size of the atomized Ni-based powders and the rotating speed of SS-PREP was also discussed and recorded.