Alumina and aluminosilicate flakes with compositions Al2O3, 3Al(2)O(3) center dot 2SiO(2) and Al2O3 center dot 2SiO(2) have been produced from commercial raw materials using a direct current plasma spray process in air. The microstructure and phase constitution of the as-sprayed flakes were examined with optical microscopy, scanning electron microscopy (SEM) and X-ray diffraction (XRD). Changes in phase constitution of the flakes with heat-treatment were examined using differential thermal analysis (DTA) and XRD of heat-treated samples. The as-sprayed Al2O3 flakes consisted of alpha-Al2O3 phase plus a minor gamma- Al2O3 phase. The. - phase could be removed by heat treating the flakes at 1300 degrees C for 2 h. The aluminosilicate flakes consisted of 3Al(2)O(3): 2SiO(2) ( mullite) and an amorphous phase which crystallised to 3Al(2)O(3): 2SiO(2) ( mullite) after heat treatment at 1100 degrees C for 2 h. These flakes may find applications as high temperature thermal insulation materials. (C) 2005 Springer Science + Business Media, Inc.