Optical Emission Spectroscopic Study of the Synthesis of Titanium Boride Nanoparticles in RF Thermal Plasma Reactor

Thermal plasma processes have been investigated by optical emission spectroscopy during the synthesis of TiB x nanoparticles from TiO 2 , B and C precursors using argon and helium both as plasma and sheath gases. Line-rich emission spectra were observed both in Ar–He–TiO 2 –B and Ar–He–TiO 2 –B–C cases. Emissions detected in the spectral region of 300–1000 nm were attributed to the electronic relaxation of excited Ti(I) and ionic fragments Ti(II), as well as the molecular species of TiO. The plasma temperature was calculated from the vibration–rotation temperature of the A–X electronic transition of TiO molecule by the least-squares fitting of experimental data to theoretical spectra. The temperatures at 100 mm downstream the torch outlet were found to be between 3800 and 2700 K for the Ar–He–TiO 2 –B system, and between 5100 and 4300 K for the Ar–He–TiO 2 –B–C system, respectively. The morphology of as-formed nanoparticles was characterized by transmission electron microscopy. Measurements of specific surface area, evaluated on the basis of Brunauer, Emmett and Teller equation, revealed that in all experimental setups titanium boride nanoparticles were formed with a mean particle size of 17–85 nm. On the basis of X-ray diffraction patterns, the solid reaction products were composed of TiB 2 , boron doped titanium indicated as Ti(B), Ti 2 O 3 , H 3 BO 3 and TiC. The actual composition of products depended on the synthesis conditions.