W. Wang et al., TIME-RESOLVED SIMULTANEOUS SAXS WAXS STUDIES OF PEEK DURING ISOTHERMAL CRYSTALLIZATION, MELTING, AND SUBSEQUENT COOLING/, Journal of macromolecular science. Physics, B37(5), 1998, pp. 667-682
Time-resolved simultaneous small- and wide-angle x-ray scattering (SAX
S and WAXS, respectively) of poly(aryl ether ether ketone) (PEEK) duri
ng isothermal crystallization, melting, and subsequent cooling were co
nducted using synchrotron radiation. Unit cell parameters were determi
ned using WAXS measurements, and the dimensions of lamellar-level moie
ties were extracted from SAXS profiles. It was found that the changes
in unit cell parameters were reversible on heating and cooling, and th
ere were remarkable differences in the thermal expansion coefficients
in different lattice directions. The long period L, the lamellar thick
ness l(c), and the thickness of amorphous layers l(a) were calculated
from the correlation function, and the changes of these dimensions dur
ing the processes mentioned above were traced. Sharp decreases in L an
d l(c) in the initial stage of isothermal crystallization and cooling
from melt were observed, and a corresponding continuous distributed mo
del is proposed. When cooling from the melt, the invariant Q exhibited
a maximum. The maximum is attributed to a change in the difference of
the densities of crystalline and amorphous phases (rho(c) - rho(a)) w
ith decreasing temperature.