Crystallization and isothermal thickening of single crystals of C246H494 in dilute solution

Citation
Jk. Hobbs et al., Crystallization and isothermal thickening of single crystals of C246H494 in dilute solution, POLYMER, 42(5), 2001, pp. 2167-2176
Citations number
16
Categorie Soggetti
Organic Chemistry/Polymer Science
Journal title
POLYMER
ISSN journal
00323861 → ACNP
Volume
42
Issue
5
Year of publication
2001
Pages
2167 - 2176
Database
ISI
SICI code
0032-3861(200103)42:5<2167:CAITOS>2.0.ZU;2-R
Abstract
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.