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Spherical granules of aluminum nitride (AlN) with an average particle size of about 50 μm 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.