Quantitative characterizational methods are required to optimize vapor‐deposited diamond thin films for optical applications. In this work, spectroellipsometry has been applied to deduce two important characteristics of diamond films: the volume fraction of sp2‐bonded defects in the bulk and the thickness of the roughness layer on the surface. We have determined these characteristics versus substrate temperature and CH4:H2 flow ratio for optical quality films prepared to 1000–4000 Å by microwave plasma‐assisted chemical vapor deposition. Under optimum conditions, uniform films with ∼100 Å roughness and 3 vol.% bulk sp2C are obtained.

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