We report a successful selective technique for preparing single-phase boron-rich silicon borides (SiB
x) films employing a pulsed Nd: YAG laser ablation method for multi-layer deposition, the results of which are designed for use in thermo-electric energy conversion device. In this process, SiB
x films on silicon substrates were produced by the pulse laser ablation method using a multi-target (single bulk material target: Si and B) in 0.1 Torr argon gas. Nano-meter order silicon particles and boron particles were ablated by different shots numbers of Nd: YAG laser pulses, which deposited several hundred alternating layers of the particles. After the films were heated to about 1670 K for 10 hours under argon gas, x-ray diffraction patterns and electron probe micro analyzer (EPMA) analysis of these films showed a single-phase composition. As a result of the laser ablation process under several processing conditions, thin films of SiB
4 or SiB
6 are selectively presented about three microns thick and about six centimeters square. The influence of process parameters on morphology, phase diagram, electrical conductivity, thermal conductivity and Seebeck coefficient of the films were also discussed.
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