The formation of titanium diboride (TiB2) whiskers through carbothermal reduction of TiO2 and B2O3 was studied in the temperature range of 900°C to 1600°C at one atmospheric pressure of argon and one atmospheric pressure of nitrogen. K2CO3 and NiCl2 were used to aid the whisker formation. TiO2, NiCl2, K2CO3, carbon black and B2O3 were taken in a definite proportion. TiN was formed as a major phase in nitrogen, whereas TiB2 was the major phase in argon. Small quantities of TiC were also formed in argon. Whiskers of TiB2 were observed at 940°C-1200°C. Above 1400°C, the formation of particulates was the dominant process. A vapour-liquid-solid growth mechanism was identified for TiB2 whisker formation.