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Aluminum-doped diamond samples were synthesized using the conventional microwave plasma chemical vapor deposition method. The electronic structures were measured using an electron probe microanalyzer and by X-ray photoelectron spectroscopy. The area intensity of the partial profile of Al-3p near the Fermi level increased with increasing aluminum concentration in the sample. The partial profile of Al-3p resembles that of C-2p at high aluminum concentrations, which suggests strong hybridization between Al-3p and C-2p. Additionally, the temperature dependence of the electric resistance yields an activation energy of 8.2 meV at room temperature. The present results suggest the metal–insulator transition of aluminum-doped diamond, similar to that of boron-doped diamond. However, with increasing aluminum concentration, a considerable amount of carriers is not doped to C-2p orbitals in aluminum-doped diamond. The present results indicate that superconductivity in aluminum-doped diamond with the same mechanism as...