G. Freddi et al., STRUCTURE AND MOLECULAR-CONFORMATION OF TUSSAH SILK FIBROIN FILMS - EFFECT OF HEAT-TREATMENT, Journal of polymer science. Part B, Polymer physics, 35(5), 1997, pp. 841-847
Structural changes of tussah (Antheraea pernyi) silk fibroin films ind
uced by heat treatment were studied as a function of the treatment tem
perature in the range 200-250 degrees C. The DSC curve of tussah films
with alpha-helix molecular conformation displayed characteristic endo
and exo peaks at 216 and 226 degrees C, respectively. These peaks fir
st weakened and then completely disappeared after heating at 230 degre
es C. Accordingly, the TMA thermal shrinkage at 206 degrees C disappea
red when the films were heated at 230 degrees C. The onset of weight l
oss was monitored at 210 degrees C by means of TG measurements. X-ray
diffraction profiles gradually changed from alpha-helix to beta-sheet
crystalline structure as the treatment temperature increased from 200
to 250 degrees C. On raising the heating temperature above 200 degrees
C, the intensity of IR and Raman bands characteristic of beta-sheet c
onformation increased in the whole ranges of amide and skeletal modes.
The sample treated at 200 degrees C showed a spectral pattern interme
diate between alpha-helix and beta-sheet molecular conformation. The I
R marker band for random coil structure, still detectable at 200 degre
es C, disappeared at higher treatment temperatures. Spectral changes a
ttributable to the onset of thermal degradation appeared at 230 degree
s C. (C) 1997 John Wiley & Sons, Inc.