Nb-based powder was fabricated via mechanical grinding. The influence of stearic acid on the grinding process was studied. The structural evolution and morphological evolution of the milled powder were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) analysis. It is indicated that an appropriate amount of stearic acid accelerates the particle refinement process and favors the production of superfine Nb-based particles with good dispersivity and high activity. However, an inappropriate amount of stearic acid has an adverse effect on the refinement process. The influence of stearic acid on the grinding process was studied. The structural evolution and morphological evolution of the milled powder were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), And energy dispersive spectroscopy (EDS) analysis. It is that appropriate amount of stearic acid accelerates the particle refinement process and favors the production of superfine Nb-based particles with good dispersivity and high activity. However, an inappropriate amount of stearic acid has an adverse effect on the refinement process.