Spherical granules of aluminum nitride (AlN) with an average particle size of about 50m were produced from aqueous suspensions using an AlN powder surface treated against hydrolysis with aluminum dihydrogenphosphate [Al(H2PO4)3]. Two different amounts of Al(H2PO4)3 were tested and the effects of surface treatment and aging time were evaluated by various techniques (XRD, TG-DTA, zeta potential and pH measurements). The treated powder exhibited antihydrolytic property and good dispersing behavior, enabling the preparation of low-viscosity and high-concentration aqueous AlN slurries for freeze granulation. The spherical AlN granules were sintered in a boron nitride (BN) powder bed followed by ultrasonic washing of the AlN granulates/BN mixture to remove BN. The sintered spherical AlN granules present excellent crystallinity and high sphericity as observed from SEM micrographs.