Synthesis and characterization of pure nanocrystalline magnesium aluminate spinel powder

Synthesis of nanocrystalline magnesium aluminate spinel (MgAl₂O₄) by mechanical activation of a powder mixture containing Al₂O₃ and MgCO₃ with subsequent annealing was investigated. Simultaneous thermal analysis (STA), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques were utilized to characterize the as-milled and annealed samples. Results showed that pure nanocrystalline spinel could be fabricated completely by 5 h of mechanical activation with subsequent annealing at 1200 °C for 1 h with a crystallite size of about 45 nm. Further milling had no significant effects on structure or phase composition of spinel phase after subsequent annealing. The nanocrystalline spinel powder obtained after 60 h of milling and subsequent annealing at 1200 °C for 1 h had a crystallite size of about 25 nm according to Williamson-Hall approach and particle sizes smaller than 200 nm. Enhanced mechanical properties were observed in samples prepared from the powder mixture and milled for a longer period.