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Metastable intermolecular composites are widely used in energy-demanding fields, where metal fluorides/fluoropolymers as oxidants have been a hot research topic in recent years. In this study, Si/NiF2/PVDF ternary energetic composites were prepared by the electrostatic spraying method for the first time, where NiF2 functions as the oxidant. At the same time, PVDF serves as both the oxidant and the binder. The energetic characteristics of the samples were studied through thermal analysis and preliminary ignition and combustion tests. It is found that the prepared samples are generally in the form of microspheres, in which PVDF binds Si and NiF2 particles together. The addition of Si nanopowder can promote the early decomposition of NiF2, which can improve reactivity. Compared with a physically mixed counterpart, the exothermic reaction between Si and PVDF in microspheres starts at lower temperatures and proceeds to more completion. The electrostatically sprayed sample also shows a shorter combustion time and a more intense luminescence phenomenon.