Time-Resolved Imaging of the Phase Transition in the Melt-Grown Spherulites of Isotactic Polybutene-1 as Detected by the Two-Dimensional Polarized IR Imaging Technique

In order to visualize the 2D spatial distribution of the structural change in the phase transition from crystal form II to I of isotactic polybutene-1 spherulite grown from the melt, the time-dependent measurement of the 2D polarized FTIR spectra has been performed. At a melt-isothermal crystallization temperature of 103 °C, the square-shape spherulite appeared from the melt and grew with time. When the isothermal crystallization occurred at 98 °C, the round-shaped spherulite was observed. In both cases, after the temperature jump to an ambient temperature, the 2D images changed clearly in the process of the phase transition from form II to form I, but the spherulite morphology itself was not changed detectably. The polarized IR imaging has revealed the preferential orientation of the crystallites in the spherulite. In the case of the spherulite grown at 103 °C, the ab plane is oriented in parallel to the spherulite plane and the molecular chains stand along the normal to the surface. On the other hand, in the spherulite grown at 98 °C, the chains were found to lie on the spherulite plane preferentially. Such a difference in the crystal orientation in the spherulite is related intimately with the outer shape of the spherulite and also with the growth mechanism of the spherulite. In this way, the polarized 2D IR imaging was found to be quite useful for the in situ detection of the time-dependently changing 2D spatial distribution of the crystallites in the spherulite.