We study the morphological change of crystalline polymer films by annealing using atomic force microscope, X-ray diffraction, and Fourier transform infrared spectroscopy techniques. As typical samples, we employ high-density and low-density polyethylene films prepared by the cast method. After annealing at 135°C for 4 h, the surface roughness of polyethylene films by the atomic force microscope significantly increases, and the crystallite size by the X-ray diffraction also shows some increase, while the Fourier transform infrared spectroscopy spectrum hardly exhibits any change. This can be well explained as a result of the growth of crystal structure by recrystallization during annealing. More interestingly, we find that the choice of the substrate and also the heating/cooling rates for annealing significantly influences the surface roughness of the films.

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We report the real-time observation of entire structural change in dye-doped semi-crystalline polymer (polyethylene) films through mid-IR transmission spectroscopy. The laser-heated dye molecules heat the polymer film through thermal diffusion, and accordingly the polymer film undergoes the structural change from the crystalline to amorphous structures, which is followed by the reverse structural change, namely recrystallization, during the natural cooling. By tuning the mid-IR probe pulse to one of the few structure-sensitive vibrational modes and varying the time delay between the pump and probe pulses we can monitor the structural change of the polymer film and time-varying film temperature during recrystallization through the transmission change of the resonant mid-IR probe pulse with the time-resolution of sub-μs.