The aim of this study was to investigate the synthesis of Co, Ni, and Cu nanoparticles from dimeric surfactants (12–2–12)[MBr4], M = Co, Ni, Cu using chemical reduction method, in two different media: water and a hexane/water emulsion. An important property of dimeric surfactants containing metals is their ability to form metallomicelles, which can act both as a source of metal ions and as a template for the synthesis of metallic nanoparticles. The synthesis of metallic nanoparticles has attracted considerable attention because of their distinctive physicochemical properties, which enable a broad spectrum of applications across diverse industries, particularly in medicine and pharmaceuticals. Chemical reduction is one of the simplest methods for synthesizing metallic nanoparticles, although it often requires toxic chemicals. By using dimeric surfactants as both a source of nanoparticles and as stabilizers, the need for additional chemicals is reduced. Microscopic techniques, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to determine the size and morphology of the synthesized metallic nanoparticles, while energy dispersive spectroscopy (EDS) was employed to identify the chemical elements present. Dynamic light scattering (DLS) and electrophoretic light scattering (ELS) were used to measure particle size and zeta potential. The findings indicate that while synthesis in water is more environmentally friendly, it is a less effective synthetic route compared to the hexane/water emulsion. In all synthesis attempts, metallic oxide nanoparticles were isolated, as shown by the recorded EDS spectra. TEM and DLS analyses revealed that individual nanoparticles were very small, approximately the size of the dimeric surfactant micelles, but they tended to aggregate despite relatively high zeta potentials.