Crystals of the uniform, long, alkane C246H494 have been grown from dilute
solution in extended chain and a number of integer folded forms, following
our earlier work on solution crystallization and thickening of C294H590 and
C198H398 Crystallization rates have been measured using DSC, and minima in
growth rates found at both the transition between primary growth in the tw
ice-folded (2F) and once-folded (1F) forms, and at the transition between p
rimary growth in the 1F and extended (E) forms. Isothermal thickening has b
een followed both in the DSC and by TEM examination of the resultant crysta
l morphologies; allowing direct correlations to be made between the thicken
ing kinetics and the changes in morphology. Different modes of thickening h
ave been observed depending on the particular integer folded forms studied.
Thickening between 2F and if crystals is accompanied by screw dislocation
growth at crystal edges, and appears to occur largely through a solid state
process resulting in a small scale roughness. Thickening between 1F and E
crystals is likewise accompanied by screw dislocation growth at crystal edg
es but appears to proceed, at least partially, through a larger scale re-or
ganization resulting in small, crystallographic, lozenge shaped, multiple t
wins. Differences between the thickening behaviour observed when samples ar
e prepared in the DSC (using aluminium pans) or in oil baths (using glass t
ubes) are also discussed. (C) 2000 Elsevier Science Ltd. All rights reserve
d.