We report the synthesis of nanocomposite films of bismuth nanoparticles (Bi NP) in a hydrogenated amorphous carbon, a-C:H, matrix. The bismuth nanoparticles were generated within a toroidal planar hollow cathode (TPHC) system using a pulsed DC power of 200 W, and the a-C:H was simultaneously produced by plasma enhanced chemical vapour deposition (PECVD) of acetylene, or methane, in the exit-plasma from the TPHC. The concurrent nanoparticle and amorphous film formation meant that the distribution of nanoparticles within the deposits was uniform and avoided problems of agglomeration of the nanoparticles. The advantage of this synthesis method is that any material which can be sputtered, including magnetic materials, can be used to produce the nanoparticle phase of the nanocomposite. The exhaust plasma from the TPHC can be used to simultaneously deposit the amorphous phase through a suitable plasma enhanced chemical reaction.The Bi/a-C:H films were deposited on glass and Si substrates, and the gas flow of acetylene, or methane, was varied from 20 to 120 sccm. The morphology, size, and distribution of the nanoparticles were measured by SEM and STEM. Additionally, X-ray diffraction, Raman and EDS were used to determine the structure and chemical composition of the samples. Resistivity measurements were performed using the four-point method.