Synthesis of TiB₂ Powders with Hexagonal Morphology by Sol-Gel Method

TiB₂ powders were successfully synthesized by carbothermal reduction of Ti-C-O-B precursor in argon at 1450 °C for 2 h. And the Ti-C-O-B precursor was formed by sol-gel method using titanium butyrate (Ti(OC₄H₉)₄), fructose (C₆H₁₂O₆), boric acid (H₃BO₃), and acetyl acetone (acac). Furthermore, thermogravimetric analysis-differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), Raman, scanning electron microscope (SEM) and energy dispersive spectrum (EDS) were employed to analyze and characterize the precursor and TiB₂ powders. Here, acac as stabilizer was studied using FITR when it reacted with Ti(OC₄H₉)₄ and the stable six-member ring was formed in order to prevent the nucleophilic attack of water, which reduced the hydrolysis rate of Ti(OC₄H₉)₄. Besides, the composition of TiB₂ phase was tested by the Raman spectra, and the results showed that the peaks at 263 cm^-1, 410 cm^-1, and 598 cm^-1 were ascribed to the characteristic peaks of TiB₂. Finally, the photomicrograph revealed TiB₂ powders with a hexagonal morphology and the average grain size of TiB₂ particles was ca. 1 um. The EDS indicated that the particles contain elements of Ti and B according to dot and line scan.