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In situ observation of the formation process of a mesophase of isotactic polypropylene is reported from a structural point of view. A very rapid transformation from the molten state to the mesophase has, for many years, made in situ observation difficult. In the present study, a rapid temperature jump and high-flux synchrotron radiation X-ray scattering techniques were combined effectively to observe this transformation. Fast time-resolved wide-angle X-ray diffraction during rapid cooling clearly shows the time evolution of the transformation from the molten state to the mesophase. The transformation proceeded very quickly in a narrow temperature range below ca 35 °C. Furthermore, the transformation was accompanied by instantaneous density fluctuations throughout the system, as visualized by microscopic observations. These observations suggest that the mesophase formation proceeds similarly to spinodal decomposition

In situ observations of the mesophase formation of isotactic polypropylene—A fast time-resolved X-ray diffraction study