A sol-gel process for producing microspheres of low density alumina has been developed. A Dispal alumina sol and aluminum monohydrate were used as starting materials. Microspheres with spherical shape and controllable size have been produced by using a drop generation technique, The technique consists of producing a continuous stream Of uniform droplets of alumina sol and then converting the drops into a rigid form by exposing them to an ammonium hydroxide gelation medium. By using this technique. alumina spheres with surface area 351 m(2)g(-1) and pore size 10.7 Adegrees have been prepared. (C) 2002 Elsevier Science B.V. All rights reserved.