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Access to well-defined, model-like, non-noble metal intermetallic compound nanomaterials (<10 nm) with phase pure bulk, bulk-like 1st-atomic-layer surface composition, and unique electronic and surface chemical properties is critical for the fields of catalysis, electronics, and sensor development. Non-noble metal intermetallic compounds are compositionally ordered solid compounds composed of transition metals and semimetals or post-transition metals. Their synthesis as model-like high-surface-area supported nanoparticles is challenging due to the elevated reactivity of the constituent elements and their interaction with the support material. In this study, we have developed a systematic understanding of the fundamental phenomena that control the synthesis of these materials such that phase pure bulk nanoparticles (<10 nm) may be produced with bulk-like surface terminations. The effects of the precursor and support choice, chemical potential of H 2 , reduction temperature, and annealing procedures were investigated to understand the fundamental kinetics of particle formation and interactions that dictate phase purity and stability and 1st-atomic-layer surface composition. The understanding developed may serve as a foundation for further developing advanced synthesis procedures for well-defined nanoparticles with increasing compositional complexity.