Sx. Lu et al., NEW-TPI THERMOPLASTIC POLYIMIDE - STRUCTURE AND RELAXATION USING SAXSAND TSDC, Journal of applied polymer science, 57(11), 1995, pp. 1359-1372
The thermoplastic polyimide Regulus(TM) NEW-TPI has been studied using
small-angle X-ray scattering (SAXS) and thermally stimulated depolari
zation current (TSDC). SAXS was used to study the development of lamel
lar structure during isothermal or nonisothermal crystallization. The
one-dimensional electron-density correlation function was used to dete
rmine structural parameters. The long period, lamellar thickness, and
amorphous layer thickness increase as crystallization temperature incr
eases from 300 to 360 degrees C. By combining melting-point data with
SAXS results, we report the side and fold surface free energies of NEW
-TPI crystals, which are 29 +/- 3 and 41 +/- 3 erg/cm(2), respectively
. Real-time SAXS was carried during nonisothermal cold-crystallization
at 5 degrees C/min. The long period decreases, while lamellar thickne
ss, linear crystallinity, and interphase thickness increase, with incr
easing temperature. These changes are explained by a crystal-insertion
model. TSDC was used as a more sensitive probe of the amorphous phase
structure below 300 degrees C. Both semicrystalline and amorphous NEW
-TPI exhibit complex TSDC behavior. Above the glass transition, amorph
ous NEW-TPI has a strong TSDC peak attributed to short-range-ordered s
tructures, which may serve as nucleation sites for subsequent crystall
ization. This peak was not seen in semicrystalline material. At the gl
ass transition, both amorphous and semicrystalline NEW-TPI have a stro
ng TSDC peak. In the semicrystalline polymer, relaxation of the amorph
ous dipoles is slightly restricted by the crystals, which results in a
smaller relaxation peak and a shift to higher temperature. Below T-g,
another TSDC peak occurs which is not due to dipolar relaxation. This
peak is attributed to the combined effects of space charge, electrode
type, ionizable species, and interfacial charges. (C) 1995 John Wiley
& Sons, Inc.