E. King et Re. Cameron, A STUDY OF MICROSTRUCTURAL CHANGES DURING DEHYDRATION OF HYDROLYTICALLY DEGRADED POLY(GLYCOLIC ACID), Macromolecular symposia, 130, 1998, pp. 19-43
The effect of dehydration on the microstructure of hydrolytically degr
aded, unoriented semi-crystalline poly(glycolic acid), PGA, was examin
ed using environmental scanning electron microscopy (ESEM), thermograv
imetric analysis (TGA) and simultaneous small and wide angle x-ray sca
ttering (SAXS/WAXS). Samples were degraded in phosphate-buffered salin
e solution at 37 degrees C and monitored during dehydration. Few micro
structural changes were observed on drying PGA after 1 hour degradatio
n. However, on drying the hydrolytically damaged PGA, the lamellar rep
eat distance decreased as crystal lamellae collapsed together. The SAX
S intensity profile showed voids simultaneously opening. Cracks became
visible at the surface and the crystallites became more strained. The
changes in surface microstructure on dehydration were found to be dep
endent on both the extent of hydrolytic attack and on the rate of remo
val of water. Significant differences in microstructure and degree of
hydration were observed between degraded PGA analysed wet, after freez
e-drying and after vacuum-drying. These findings indicate the importan
ce of sample preparation in the study of degradable materials.