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One natural and two synthetic spinels with compositions Mg(Al 1-z Fe z  3+ ) 2 O 4  (with 2z = 0.078, 0.138, and 0.200, respectively) were studied by in situ, high-temperature, single-crystal X-ray diffraction. All samples were heated from room temperature to 1050 °C. Thermal expansion was monitored by measuring the cell edge variation. Cation disorder was monitored by measuring the variation of the oxygen positional parameter u, which is closely correlated with the inversion parameter i. All samples showed extensive Al reordering at the M site between 550 and 650 °C, followed by an increase of disorder at T &gt; 650 °C due to both Mg-Al and Mg-Fe 3+  intersite exchanges.

Thermodynamics and kinetics of cation ordering in natural and synthetic Mg(Al,Fe 3+ ) 2 O 4 spinels from in situ high-temperature X-ray diffraction