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The ability to characterize the phase of the intrinsic (i) layers incorporated into amorphous silicon [a-Si:H] and microcrystalline silicon [μc-Si:H] thin film solar cells is critically important for cell optimization. In this research, a new method has been developed to extract the thickness evolution of the μc-Si:H volume fraction in mixed phase amorphous + microcrystalline silicon [(a+μc)-Si:H] i-layers. This method is based on real time spectroscopic ellipsometry measurements performed during plasma-enhanced chemical vapor deposition of the films. In the analysis, the thickness at which crystallites first nucleate from the a-Si:H phase can be estimated, as well as the nucleation density and microcrystallite cone angle. The results show very good correlations with structural and electronic device measurements.