Potassium hexatitanate (K2Ti6O13) whiskers with an average thickness of less than 100 nm were synthesized by calcinating KF and TiO2 mixtures and subsequent boiling water treatment and reheating. The influences of heating temperature and weight ratio of KF to TiO2 in the mixture on the formation of K2Ti6O13 whiskers were investigated. The suitable experiment condition for whisker formation is a weight ratio of KF to TiO2 of about 2:1 and a heating temperature of about 720 degrees C. The resultants of reactions between KF and TiO2 at 720 degrees C were investigated by selected area diffraction (SAD) technique. Some new structures having a monoclinic structure with b = 0.38 nm were found. All these compounds transformed into K2Ti6O13 after boiling water treatment and reheating,