Phase pure boehmite particles were prepared by microwave assisted hydrolysis of aluminium sheets. These particles were calcined in air to produce g Al 2 O 3 particles with specific surface area of~210 m 2 /g. The alumina particles were characterized by studying X-ray diffraction, transmission electron microscopy and Fourier transform infrared spectroscopy. For comparison, the aluminium hydroxide particles were also prepared by normal hydrolysis of aluminium metal. Normal hydrolysis yielded a mixture of boehmite and bayerite particles whereas microwave assisted hydrolysis produced phase pure boehmite particles. The importance of using microwave radiation for the hydrolysis of aluminium metal is also manifested in a shorter reaction time.