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An important cause of deactivation of alumina supported transition metal (oxide) catalysts is a solid state reaction between the active component and the support. We therefore studied the hightemperature behavior of Me layers (Me = Co, Ni, Cu and Fe) on polycrystalline α-A12O3 and γ- Al2O3 substrates. The samples were first oxidized at moderate temperatures and then annealed at high temperatures (up to 1000 °C) in O2, N2, or N2/O2 mixtures. The interfacial reaction to MeA12O4 was assessed using Rutherford Backscattering Spectrometry and X-ray diffraction. The reaction rate strongly depends on the transition metal element Me: Fe < Ni < Co < Cu. Low oxygen pressures favour spinel formation. γ-A12O3 shows a much higher reactivity towards the MeOx overlayers than α-Al2O3.