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In this paper, the effect of alloy composition on the microstructural development of devitrified Nd–Fe–B-based alloys is investigated. While crystallization of simple ternary Nd2Fe14B resulted in a highly variable microstructure and relatively poor demagnetization behavior, alloying additions, notably Ti and C, were found to significantly refine and homogenize the crystallized microstructure. High spatial resolution energy dispersive X-ray spectroscopy revealed that partitioning to the grain boundaries led to the grain refinement by slowing interface kinetics. The more homogeneous grain structure resulted in improved demagnetization behavior, but segregating elements isolated grains and limited intergranular exchange coupling.