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The stoichiometry of boron carbide thin films was controlled in the range of 0.1–8.9 via pulsed laser deposition by using boron-carbon dual-targets. The amorphous films sized 50 nm in thickness. The reaction rate of boron and carbon atoms increased with the increasing of target rotating speed. Carbon atoms preferentially substituted boron atoms within the chain site as sp2 hybridization at lower carbon concentrations and then within the icosahedrons site as sp3 hybridization at higher carbon concentrations.