In this study, AlN whiskers were prepared in a tube furnace at 1000˚C for 1h with 500 nitrogen gas flow. Al powders with particle size of 3 μm and 45 μm and NH4Cl were used as raw materials. SEM, TEM and XRD analysis were used to characterize AlN whiskers. The results showed that the diameters of AlN whiskers would range from 140 nm to 340 nm if different amounts of NH4Cl and 3 μm Al powder were used. In the case of using NH4Cl more than 40wt%, pure AlN without any unreacted Al was formed as the final product. Using NH4Cl and Al with particle size of 45 μm led to AlN whiskers with 630 nm to 870 nm in diameter. By adding 50%wt NH4Cl, pure AlN was formed. The diameter of the whiskers was increased by increasing NH4Cl content in starting materials (about 200 nm). Also, an increase in the diameter of AlN whisker resulted from coarse Al powder. By adding NH4Cl to Al, thermodynamically spontaneous cholororination - nitridation reactions were increased in vapor phase and whiskers and pure AlN powder were produced.