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  • 1
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 32 (1994), S. 2705-2713 
    ISSN: 0887-6266
    Schlagwort(e): crystal unit cell ; morphology ; polyimide ; structure ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: An aromatic polyimide oligomer, poly(1,4-phenyleneoxy-1,3-phenylene pyromellitimide) (PMDA-3,4'-ODA), was synthesized from pyromellitic dianhydride (PMDA) and 3,4'-oxydianiline (3,4'-ODA) via a melt-polymerization method. This method permits growth of PMDA-3,4'-ODA lamellar crystals and the crystal structure can be studied via electron diffraction (ED) and wide-angle x-ray diffraction (WAXD) experiments. Our structure analysis indicates that this polyimide possesses a two-chain orthorhombic crystal lattice with dimensions of a = 0.848, b = 0.562, and c = 3.365 nm. It has also been found that poly(amic acid) precursors with little imidization possess the same ab lateral lattice packing, but statistical departure from the ordered packing along the c-direction. Upon increasing the degree of imidization through annealing at elevated temperatures, the order along the c-axis was progressively enhanced. Increasing the annealing temperature caused the dimensions of the a- and the b-axes to expand while the crystal correlation lengths decreased laterally. Simultaneously the dimension of the c-axis shrinks with an increase of the crystal correlation length along the chain direction. Crystal morphological study via transmission electron microscopy (TEM) indicates a mainly lamellar crystal texture with different thicknesses depending upon the polymerization conditions. The end lamellar surface is usually smooth. After annealing at elevated temperatures, the lamellar end surfaces become rough, which may be due to chain motion along the c-axis. The annealed PMDA-3,4'-ODA lamellar crystals still show a large amount of defects. © 1994 John Wiley & Sons, Inc.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    ISSN: 0959-8103
    Schlagwort(e): polyimide ; m-cresol ; phase structure ; morphology ; phase boundary diagram ; gel/sol transition ; DSC ; polarized light microscopy ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Maschinenbau , Physik
    Notizen: An organo-soluble aromatic polyimide has been synthesized from 3,3′, 4,4′-bis(phenyltetracarboxylic) dianhydride (BPDA) and 2,2′-bis (trifluoromethyl)-4,4′-diaminobiphenyl (PFMB) via a one-step polymerization in m-cresol. The phase boundary diagram for this system has been established by differential scanning calorimetry, polarized light microscopy (PLM) and wide angle X-ray diffraction (WAXD) experiments. A crystallosolvate form I has been found over the entire concentration region at low temperatures. When the temperature is increased, an isotropic phase has been observed below concentrations of about 40%. In the relatively high concentration region between 45 and 95%, a transition from the crystallosolvate from I to a crystallosolvate form II has been observed. Form II exhibits a different WAXD pattern. In a narrow concentration region between the isotropic and the crystallosolvate form II (40-45%), a biphase behavior has been found. The birefringence of this region may be an indication of a liquid crystalline phase. The BPDA-PFMB polymer crystal has been found in the very high concentration region (〉95%) for temperatures 〉250°C. The morphologies of these phases have been investigated via PLM and transmission electron microscopy. Above the gel/sol transition temperature, the form I shows negative birefringent spherulites consisting of thin lamellae. The form II exhibits a tendency of positive birefringent spherulites. Possible mechanisms of the formation of the metastable phase morphology and their associations with the mechanical gel/sol transition are also discussed.
    Zusätzliches Material: 13 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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