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Diamond homoepitaxial films were grown on an off‐angle (001) substrate with a misorientation of 4.3° toward the  direction by microwave plasma‐assisted chemical vapor deposition from a methane‐hydrogen gas mixture. The single domain 2×1 surface was observed by low‐energy electron diffraction (LEED) and scanning tunneling microscopy, after growth with methane concentration of 2%. With a methane concentration of 6%, the LEED superstructure spot intensity from another domain increased, suggesting a higher rate of two‐dimensional nucleation.