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This study addresses the challenge of low-temperature synthesis of the high-performance L10 Fe-Pt intermetallic phase, which is critical for applications in ultra-high-density data storage and advanced magnetic devices. We demonstrate that the choice of iron precursor is a decisive factor in directing the phase composition and thermal evolution of Fe-Pt nanostructures, ultimately determining their suitability as functional composite materials. Fe-Pt systems were synthesized from aqueous solutions using platinum(IV) chloric acid (H2PtCl6) with either iron(III) ammonium sulfate (NH4Fe(SO4)2) or iron(II) sulfate (FeSO4). Comprehensive characterization using X-ray diffraction and high-resolution transmission electron microscopy revealed distinct composite formations. The iron(III) precursor yielded homogeneous, thermally stable nanocomposites: as-synthesized nanoparticles formed a Pt-based FCC solid solution (~5 nm), which upon annealing at 500 °C transformed into a biphasic nanocomposite of FCC solid solution and an L12 Fe21Pt79 intermetallic phase with minimal grain growth (~7 nm). In stark contrast, the system derived from iron(II) sulfate resulted in a heterogeneous composite of 4 nm Pt nanoparticles, an FCC solid solution, and discrete 1–3 nm Fe nanoparticles with L12-ordered FePt3 domains. Annealing this heterogeneous mixture caused phase segregation, forming significantly coarsened Pt-rich crystals (~30 nm) that were approximately 4–6 times larger than the crystallites in the annealed homogeneous composite, with negligible Fe incorporation. Our findings establish that precursor chemistry dictates the initial nanocomposite architecture, which in turn controls the pathway and success of low-temperature intermetallic phase formation. This work provides a crucial design principle for fabricating tailored Fe-Pt composite nanomaterials, moving beyond simple alloys to engineered multiphase systems for practical application.