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We succeeded for the first time in preparing a high-quality (101)-oriented epitaxial β-FeSi2 film on Si(111) wafer by metal-organic chemical vapor deposition (MOCVD) using Fe(CO)5 and SiH4 as source materials. The full width at half maximum (FWHM) of the rocking curve of the β-FeSi2 (202) peak was 0.46 degree for the film deposited at 750°C at a rate of 4 nm/min. Moreover, a smooth-surface film of up to 650 nm thickness could be deposited by this method. Carbon content in the film was less than 0.1 at%.