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  • 1
    Electronic Resource
    Electronic Resource
    [s.l.] : Macmillian Magazines Ltd.
    Nature 402 (1999), S. 162-165 
    ISSN: 1476-4687
    Source: Nature Archives 1869 - 2009
    Topics: Biology , Chemistry and Pharmacology , Medicine , Natural Sciences in General , Physics
    Notes: [Auszug] Synthetic diamond is used in applications ranging from abrasives, tool coatings, bearing surfaces, microelectronics and optics to corrosion protection. The first artificial synthesis used high-pressure techniques to produce diamond as the thermodynamically stable form, but it can also be grown ...
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 30 (1997), S. 921-931 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: This paper describes a variant of the Rietveld refinement procedure applied to the characterization by X-ray scattering of disordered and small crystals as found in semicrystalline polymers. The program essentially focuses on the profile of the reflections and allows one to obtain the size, unit-cell parameters and lattice distortions (atomic displacements and paracrystallinity) of crystals in isotropic samples. The detailed influence of instrumental aberrations on the scattering is also considered. To illustrate the usefulness of the method, results obtained on PEEK [poly(ether-ether-ketone)] samples, cold-crystallized at various temperatures are presented. As the crystallization temperature increases, a closer packing of the chains in the 〈100〉 direction, a decrease in paracrystallinity along 〈100〉 and a thickening of the crystalline lamellae (〈001〉 direction) are observed. The lamellae are strongly microfragmented perpendicularly to the chain axis, resulting in coherently diffracting regions of sizes between 700 and 2000 nm3 only.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: In a previous paper [Dupont, Jonas & Legras (1997). J. Appl. Cryst. 30, 921–931], a variant of the Rietveld method was applied to the characterization by X-ray scattering (powder diffractometry) of disordered and small crystals as found in semicrystalline polymers. In the present study, a new version of the model is described, which is designed to take into account the possible existence of a non-zero tilt angle (ψ) of the chain axes versus the large faces of the lamellar crystals. Fits of this model to the diffractograms of various samples of cold-crystallized PEEK [poly(ether-ether-ketone)] and of a monodisperse PEEK oligomer are presented. For the oligomer, the fits converged only towards ψ = 0°. For the polymers, two equivalent solutions were found, one with thick lamellae and ψ = 0°, another with thinner lamellae and ψ = 20°. Models with and without chain tilt give similar goodness-of-fit parameters, indicating that results coming from other techniques than X-ray diffractometry are required in order fully to characterize the dimensions and shape of crystals in isotropic polymer samples. Comparing the present values with results obtained by such other techniques suggests the existence of a tilt angle for cold-crystallized PEEK samples.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1435-1536
    Keywords: Poly(ethylene terephthalate) ; lamellar morphology ; melting-recrystallization ; annealing
    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 Structural changes occurring during crystallization of quenched amorphous poly(ethylene terephthalate) (PET) and subsequent cooling/heating cycles have been studied by real-time small-angle x-ray scattering (SAXS), using synchrotron radiation. Initial crystallization is found to occur by insertion of new lamellae between the existing ones, while rapid continuous melting/recrystallization happens when the cold-crystallized PET samples are heated above the previous highest annealing temperature. Such melting/recrystalization results in irreversible increases in the lamellar long period, the crystal thickness and the density difference between the crystalline and amorphous regions; in contrast, at temperatures below the prior highest crystallization temperature, the structural changes are dominated by reversible effects such as thermal expansion. However, throughout the entire temperature range up to the melting point around 250 °C, the crystal core thickness remains quite small, less than ca. 50 Å, and the linear crystallinity of lamellar stacks remains nearly constant around 0.3. Such a low crystallinity indicates the presence of thick order-disorder interfacial layers on the lamellar surface, whose thickness increases with temperature.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 2565-2570 
    ISSN: 0887-6266
    Keywords: Semicrystalline morphology ; lamellar structure ; poly(aryl-ether-ether-ketone) (PEEK) ; poly(ether-imide) (PEI) ; staining ; TEM ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: No abstract.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 919-930 
    ISSN: 0887-6266
    Keywords: α-relaxation ; cold crystallization ; poly(aryl-ether-ether-ketone) (PEEK) ; poly(ether-imide) (PEI) ; vitrification ; devitrification ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: We have established time-temperature transformation and continuous-heating transformation diagrams for poly(ether-ether-ketone) (PEEK) and PEEK/poly(ether-imide) (PEI) blends, in order to analyze the effects of relaxation control on crystallization. Similar diagrams are widely used in the field of thermosetting resins. Upon crystallization, the glass transition temperature (Tg) of PEEK and PEEK/PEI blends is found to increase significantly. In the case of PEEK, the shift of the α-relaxation is due to the progressive constraining of amorphous regions by nearby crystals. This phenomenon results in the isothermal vitrification of PEEK during its latest crystallization stages for crystallization temperatures near the initial Tg of PEEK. However, vitrification/devitrification effects are found to be of minor importance for anisothermal crystallization, above 0.1°C/min heating rate. In the case of PEEK/PEI blends, amorphous regions are progressively enriched in PEI upon PEEK crystallization. This promotes a shift of the α-relaxation of these regions to higher temperatures, with a consequent vitrification of the material when crystallized below the Tg of PEI. The data obtained for the blends in anisothermal regimes allow one to detect a region in the (temperature/heating rate) plane where crystallization proceeds in the continuously close proximity of the glass transition (dynamic vitrification). These experimental findings are in agreement with simple simulations based on a modified Avrami model coupled with the Fox equation. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 919-930, 1998
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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