Boron carbide is one of the most important non-metallic materials. Amorphous BCx films were synthesized at room temperature by single- and dual-target magnetron sputtering processes. A B4C target and C target were operated using an RF signal and a DC signal, respectively. The effect of using single- and dual-target deposition and process parameters on the chemical bonding and composition of the films as well as their functional properties were characterized by Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, X-ray energy dispersive analysis, X-ray diffraction, ellipsometry, and spectrophotometry. It was found that the film properties depend on the sputtering power and the used targets. EDX data show that the composition of the samples varied from B2C to practically BC2 in the case of using an additional C target. According to the XPS data, it corresponds to the different chemical states of the boron atom. A nanoindentation study showed that the film with a composition close to B2C deposited with the highest B4C target power reached a hardness of 25 GPa and Young’s modulus of 230 GPa. The optical properties of the films also depend on the composition, so the band gap (Eg) of the BCx film varied in the range of 2.1–2.8 eV, while the Eg of the carbon-rich films decreased to 1.1 eV.