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Fine crystalline spinel MgAl2O4 was synthesized from mixture of AlOOH or Al(OH)3 and MgO with addition of activator, using stepwise heating of mixture precursors in water fluid: at 230oC, PH2O=2,3 MPa, and then at 400oC, PH2O=26 MPa. The spinel formation is realized through a stage of deep hydration of reagents and with the advent of intermediate product of interaction of components, containing the magnesium and aluminum - Mg2Al(OH)7. On the heating stage of hydrated intermediates in supercritical conditions SCWF the spinel crystals were formed. Depending on the type of activator, size of crystals can be changed from nanometers up to several microns. The habitus of crystals spinel can be changed from spherical up to octahedral.