This paper describes some simple investigations of the effects of milling condition and milling technique on powder particle size distribution and morphology. Experiments were performed on brittle alumina and ductile Al. Three types of ball-mill were used; a vibrational mill containing one large ball, a planetary Fritsch mill, and a horizontal Uni ball-mill with external magnets used to control ball movement and milling mechanism. For alumina, dry and wet milling was carried out, while Al was milled in vacuum, Ar, He, H-2, NH3 and under wet conditions. Milling of alumina powder in a dry atmosphere using vibratory, planetary and magneto techniques periods was found to result in the evolution of similar particle size distributions, all tending to bimodal for extended milling times. Compared with controlled milling in a dry atmosphere, wet milling of alumina powder under the same conditions was found to result broadening of the size distribution curves, including the formation of nanoparticles. High energy milling of Al powder, using vibratory, planetary and magneto-milling under impact, was found to result in excessive cold welding preventing particle evolution. Magneto-milling of Al powder under He using low energy shearing mode resulted in the evolution of spheroidal Al particles. The latter process involved, 1, the shearing and flattening of irregular particles leading to the formation of flakes, 2, bending of flakes and, 3, subsequent formation via cold welding and compaction of spheres. Increasing the pulling force on the balls resulted, firstly, in finer deformed flakes comprising the spheres while further increases in pulling force resulted in the formation of hollow spheres. Low energy magneto-milling Al powder under Ar and under wet milling conditions both resulted in the production of Al flakes, however, there was no tendency for spherodisation.