Compounds of the composition Co
xNi
1-xAl
2O
4 (x = 0, 0.25, 0.5, 0.75, 1) were synthesized by high-temperature reactions in the solid phase at 1200°C. The compounds crystallize in the mineral spinel structure type. The crystal structures of the individual compounds and solid solution with equimolar content of components were refined by the Rietveld method (space group Fd3m). The temperature dependencies of unit cell parameters were investigated using a high-temperature XRD method. The thermal expansion coefficients of five compounds with the structure of spinel were determined.
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