Impact of ball milling on the cubic Sb2O3 into orthorhombic Sb2O3 and SbO2 materials – Structural and other characterization studies

Abstract

The present investigation adds new information about the cubic Sb2O3 and orthorhombic Sb2O3 and SbO2 phases to the scientific society. In this work, the Sb2O3 (commercial) powder was ball-milled in a tungsten carbide (WC) jar using WC balls with different diameters at 300 ​rpm for several time intervals (1, 3, 5, 10, 20, and 30 ​min and 1, 2, 5, 10, 20, and 30 ​h) and reported their findings of structural, thermal, optical, and morphology. Interestingly, the ball-milled powder undergoes phase transformation from cubic Sb2O3 into orthorhombic Sb2O3 and SbO2 in a short duration (3–30 ​min) of ball milling. While the 0, 1, and 3 ​min ball milled samples preserve the cubic Sb2O3 structure, the 5 ​min ball milled sample exhibits a nearly single-phase orthorhombic Sb2O3 structure. Mixed phases of orthorhombic Sb2O3 and SbO2 phases are seen for the 10–20 ​min ball milled samples. For a 30 ​min ball milled sample, an orthorhombic SbO2 phase is observed. Furthermore, the 1, 3, 5, 10, 20, and 30 ​h ball milled samples retain the orthorhombic SbO2 phase. Maximum weight loss of 34.4 ​% is noted for the commercial Sb2O3 powder, whereas the 1 and 3 ​min of ball-milled samples reveal the weight loss of 9.3 and 4.7 ​%, respectively. The other ball-milled samples exhibit both weight loss and weight gain in the thermogravimetric analysis (TGA) curves. The Raman features of ball-milled orthorhombic SbO2 are quite different from those of other types of antimony-based oxides. Bar/bundle-shaped and spherical-shaped with agglomerated particles are seen for the commercial Sb2O3 phase and ball-milled (1 and 30 ​h) SbO2 phase samples.