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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Colloid & polymer science 262 (1984), S. 22-45 
    ISSN: 1435-1536
    Keywords: Isotactic polystyrene ; gels ; structure ; morphology ; conformation ; X-ray diffraction ; electron microscopy ; DSC ; FTIR ; crystallization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The thermoreversible gelation phenomena exhibited by isotactic polystyrene (i-PS) was examined in depth, utilising a variety of experimental techniques. The primary aims were identification, relationship, description and visualisation of the morphologies corresponding to the two types of crystallization as diagnosed by the different crystal structures revealed by X-ray diffraction. While centred on electron microscopy the investigation used X-ray and electron diffraction, differential scanning calorimetry and Fourier transform infra-red spectroscopy in combination. A satisfactory correlation between all these techniques was established, including the important reassurance that the characteristics of the gel state are preserved on drying, a feature necessitated by most structure methods. Thei-PS gel system as a whole displays particularly clearly the distinction between gel forming and chain folded lamellar crystallization and the coexistence, morphological relationship and competition between the two crystallizable species. In addition, and most significantly, the gel crystals possess a crystal structure involving extended chains, close to an all-trans conformation, which are quite different to those obtained from conventionally crystallizedi-PS (31 helix). This former extended conformation in itself has become the starting point for new geometric and stereochemical considerations and in addition offers a convenient diffraction based fingerprint to delineate between the two modes of crystallization. Thus the conversion of the gel crystal structure to the conventional 31 helix structure on heating could be monitored. Further, that in the processes of heat annealing, remnants of these gel fibres initiate the development and dictate the orientation of a shish-kebab type platelet growth with the 31 helix crystal structure. This conversion process has been followed by electron microscopy and supplemented infra-red spectroscopy, low angle X-ray diffraction and differential scanning calorimetry. The different roles of fibres and platelets on stretching have been identified. Conditions for the existence of the gel crystals in their different variants are specified with relevance to ongoing arguments and discussions in the subject. Further, it was established that passing through the gel phase significantly enhanced the crystallization in the conventional crystal form making the normally slowly crystallizingi-PS into a fast crystallizable polyolefin.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Colloid & polymer science 271 (1993), S. 328-342 
    ISSN: 1435-1536
    Keywords: Polyethylene ; crystallization ; morphology ; single crystal ; spherulite ; axialite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Three-dimensional shape of polyethylene single crystals grown from the melt has been studied. Two distinct types of lateral habit have been obtained: lenticular shape (type A) and truncated lozenge (type B) in the range of regime I and II. Electron microscopy has revealed chair-like shape of type B crystal and reconfirmed the planar shape of type A crystal. In the type B crystal, spiral growth has occurred frequently in the {110} sectors and the sense of the handedness of spiral terraces has been maintained. It has been, suggested that the frequens occurrence of spiral growth is responsible for a morphological change (axialite-spherulite) accompanying the regime I–II transition. The origin of the chair-like crystals has been discussed and, a possible mechanism has been suggested for the formation of spiral terraces; the mechanism is based on a distortion caused by the three-dimensional shape of chair-like crystals. It has been found that the chair-like crystals are curved in the opposite way to S-shaped lamellae observed by Bassett and Hodge in banded spherulites. In fact, the present work has led to the recognition of further classes of crystal with curving cross-sections and of distinctions between them. In final analysis, a unifying thread has been identified between lateral habits, growth kinetics and three-dimensional shape of lamellae, in turn, leading to some rationalization of multilayer developments including twisting in banded spherulites, the latter based on existing suggestions in the literature.
    Type of Medium: Electronic Resource
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