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Thin carbon nanofibers with less than 100 nm diameter were variously prepared over MgO-supported nickel and bimetallic nickel catalysts with iron, copper, and molybdenum. The second metal effects on the carbon yield and structure were investigated by using electron microscopic and gas chromatographic methods. Further, the active catalysts were examined by powdered X-ray diffraction to elucidate correlation between the catalyst and nanofiber growth. The surface composition of catalysts appeared to govern the catalyst activity and the resulting CNF structure. The second metal effects on the catalyst activity and resulting nanofiber structure is discussed in terms of the formation mechanism of carbon nanofibers, on the basis of the results.