DYNAMICAL OBSERVATION OF STRUCTURAL TRANSITION OF POLYMERS USING AN X-RAY-DIFFRACTION SYSTEM WITH IMAGING PLATES .1. REVERSIBLE HELIX HELIXTRANSFORMATION OF POLY(VINYL CYCLOHEXANE)/
Y. Nishikawa et al., DYNAMICAL OBSERVATION OF STRUCTURAL TRANSITION OF POLYMERS USING AN X-RAY-DIFFRACTION SYSTEM WITH IMAGING PLATES .1. REVERSIBLE HELIX HELIXTRANSFORMATION OF POLY(VINYL CYCLOHEXANE)/, Macromolecules, 29(17), 1996, pp. 5558-5566
Two different crystalline forms were caused by drawing an unoriented i
sotactic poly(vinylcyclohexane) film, Form I and Form II, depending on
the drawing temperature. Form II was changed into Form I thermally an
d Form I was converted into Form II by drawing. This reversible phase
transformation was followed by dynamical X-ray observation. The X-ray
measurements were carried out with an X-ray diffraction system with im
aging plates, which was designed to record X-ray diffraction patterns
over a series of short time spans while the samples were being heated
or drawn. When samples were drawn at temperatures below about 110 degr
ees C, Form I was produced, and Form II was formed at higher temperatu
res. Through dynamical observations with the X-ray diffraction system,
it was found that Form I occurred at an early stage of drawing indepe
ndently of the drawing temperature and that the crystalline form was c
hanged into Form II by further drawing at high temperatures, e.g., 130
degrees C. Form II was transformed into Form I by heat treatment at t
emperatures above 248 degrees C. When the heat-treated sample of Form
I was drawn at, e.g., 133 degrees C, the crystalline form was transfor
med into Form II. Thus, the transformation of Form II into Form I occu
rred thermally at temperatures above 248 degrees C and the inverse tra
nsformation was induced by applying the stress at temperatures above a
bout 110 degrees C.