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  • 1
    Digitale Medien
    Digitale Medien
    Springer
    Journal of thermal analysis and calorimetry 61 (2000), S. 661-679 
    ISSN: 1572-8943
    Schlagwort(e): differential scanning calorimetry (DSC) ; infrared thermography ; phase angle ; temperature gradient ; temperature-modulated differential scanning calorimetry (TMDSC)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract Temperature gradients within the sample and furnace in temperature-modulated differential scanning calorimetry (TMDSC) are studied for a power-compensation calorimeter of the Perkin Elmer type. The temperature measurements were made with a high-speed, high-resolution infrared camera. Differences between programmed and actual temperature amplitudes are determined as a function of sample thickness for a sawtooth modulation with up to 48 K min−1 heating and cooling rates. Phase angles have been established, and the effect of open and sealed sample pans has been analyzed. A simple one-dimensional description of the observed effects is made and a three-dimensional one is suggested based on a model available in the literature.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Journal of thermal analysis and calorimetry 59 (2000), S. 187-203 
    ISSN: 1572-8943
    Schlagwort(e): atomic force microscopy ; microcalorimetry ; polymers ; temperature-modulation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract A newly developed Micro-Thermal Analyzer affords images based on thermal properties such as thermal conductivity, thermal diffusivity, and permits localized thermal analyses on samples of a square micrometer area by combining the imaging ability of the atomic force microscope and the thermal characterization ability of temperature-modulated differential scanning calorimetry. Since thermal penetration depth depends on frequency, one can obtain depth profiles of thermal conductivity and thermal diffusivity by varying the modulation frequency. Also, the analyzer can be used to characterize phase-transition temperatures, such as glass and melting transitions, of small sample regions with a precision of about ±3 K. Heating rates can be varied between 1 and 1500 K min−1. Modulation frequencies can be applied in the range from 2 to 100 kHz. We applied this new type of instrument to characterize microscopic thermal and structural properties of various polymer systems. The operation principles of the instrument are described, application examples are presented, and the future of the technique is discussed.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Journal of thermal analysis and calorimetry 61 (2000), S. 75-89 
    ISSN: 1572-8943
    Schlagwort(e): DSC ; Fourier transformation ; heat capacity ; sawtooth-modulation ; TMDSC
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Abstract The determination of heat capacity data with sawtooth-type, temperature-modulated differential scanning calorimetry is analyzed using the Mettler-Toledo 820 ADSC™temperature-modulated differential scanning calorimeter (TMDSC). Heat capacities were calculated via the amplitudes of the first and higher harmonics of the Fourier series of the heat flow and heating rates. At modulation periods lower than about 150 s, the heat capacity deviates increasingly to smaller values and requires a calibration as function of frequency. An earlier derived correction function which was applied to the sample temperature-controlled power compensation calorimeter enables an empirical correction down to modulation periods of about 20 s. The correction function is determined by analysis of the higher harmonics of the Fourier transform from a single measurement of sufficient long modulation period. The correction function reveals that the time constant of the instrument is about 5 s rad−1 when a standard aluminum pan is used. The influence of pan type and sample mass on the time constant is determined, the correction for the asymmetry of the system is described, and the effect of smoothing of the modulated heat flow rate data is discussed.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 4
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Materialwissenschaft und Werkstofftechnik 22 (1991), S. 427-433 
    ISSN: 0933-5137
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Maschinenbau
    Beschreibung / Inhaltsverzeichnis: It is the aim of the investigations on a PBTP-glass-spherecomposite to get experimental well-founded informations about the state of stress in the polymer matrix of the composite. The used method was the x-ray-lattice strain-stress measurement.The result of the measurements is the proof of a 3-axial state of tension stress in the polymer matrix in the unloaded state as well as under an uniaxial tension load. The reason are differences in the elastic properties of the two components in this heterogenous built up composite.
    Notizen: Die Untersuchungen an einem PBTP-Glaskugel-Verbundwerkstoff haben das Ziel, experimentell begründete Aussagen über den Spannungszustand in der Polymermatrix des Verbundwerkstoffes zu gewinnen. Als Meßverfahren wurde die röntgenographische Spannungsmessung verwendet.Im Ergebnis der Messungen konnte in der Polymermatrix des Verbundwerkstoffes sowohl im unbelasteten Zustand als auch bei einachsiger äußerer Zugbeanspruchung ein mehrachsiger Zugspannungszustand nachgewiesen werden. Er ist durch die Unterschiede in den elastischen Eigenschaften der beiden Komponenten des heterogenen aufgebauten Verbundwerkstoffes bedingt.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 5
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 214 (1994), S. 179-196 
    ISSN: 0003-3146
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Beschreibung / Inhaltsverzeichnis: The crystallization behavior of PBT as well as PC is changed in the controlled-processed blend due to intermolecular interactions between the different macromolecules in molten state.If the kinetics of the crystallization process prevents a crystallization-induced separation, the partial miscibility of the amorphous phases, measured by the glass transition temperatures, will lead to a decrease of the crystallinity of PBT. The crystallinity, normalized to the concentration of PBT in the blend, is independent from the concentration of PC at low coolling rates.At high cooling rates, PBT is crystallizing stepwise in the blend PBT/PC 40/60 wt.-%. The crystallization temperature in the anisothermic crystallization process is increased at low contents of PC due to a changed nucleation mechanism. The half-time of crystallization is increasing in blends with an increasing PC-content in isothermic crystallization experiments.The normally amorphous PC crystallizes considerably fast in presence of PBT in PC-rich blends. The crystallization or change in the state of order of PC was measured in situ by X-ray diffraction. Calorimetric experiments confirm this result and allow a quantitative estimation of the PC-crystallinity, which amounts to some 20% in the blend PBT/PC 5/95 wt.-%.
    Notizen: Das Kristallisationsverhalten sowohl von PBT als auch von PC ist im definiert verarbeiteten Blend infolge intermolekularer Wechselwirkungen zwischen den unterschiedlichen Molekülen in der Schmelze verändert.Die über die Glasübergangstemperaturen gemessene teilweise Mischbarkeit der amorphen Phasen führt bei PBT zu einer Erniedrigung des Kristallinitätsgrades, wenn die kinetischen Bedingungen des Kristallisationsprozesses keine kristallisationsbedingte Entmischung zulassen. Der auf den PBT-Anteil normierte Kristallinitätsgrad ist bei kleinen Abkühlgeschwindigkeiten vom PC-Anteil unabhängüg.In der Mischung PBT/PC 40/60 Gew.-% kommt es bei hohen Kühlraten zu einer fraktionierten Kristallisation. Die Kristallisationstemperatur bei anisothermer Kristallisation ist bei geringen PC-Gehalten durch Änderung des Keimbildungsmechanismus erhöht. Bei isothermer Kristallisation steigt mit zunehmendem PC-Anteil die Kristallisationshalbwertszeit des PBT an.Das normalerweise amorphe PC kann in Gegenwart von PBT in den PC-reichen Mischungen besonders schnell kristallisieren, wobei der Kristallisations- bzw. Ordnungsprozeß des PC in situ mittels der Röntgenbeugung gemessen wurde. Kalorimetrische Untersuchungen bestätigen dieses Ergebnis und erlauben eine quantitative Abschätzung des PC-Kristallinitätsgrades zu ca. 20% im Blend PBT/PC 5/95 Gew.-%.
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 6
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Acta Polymerica 47 (1996), S. 99-104 
    ISSN: 0323-7648
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The general crystallization behavior of amorphous polyamides during heating treatment was measured by wide angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) to get information on (1) the temperature range where the crystallization in an anisothermic process takes place and (2) the type of the crystalline phases (α or γ) considering the Brill transition and the state of order in the α-crystal. Various polyamides (PA 6, 6.10 and 6.6) were quenched and cooled to 200 K and then heated until they melted. During heating from the glassy state the crystallization starts rapidly at the glass transition temperature and then the crystallinity slowly increases until the melting point. The crystallinity was calculated on the basis of the separation of the amorphous and crystalline scattering by profile fitting. The angular position of the amorphous halo and so the density of the amorphous phase is higher in the presence of the crystalline phase compared to the completely amorphous state. The crystalline structure (α or γ), which is difficult to distinguish at higher temperatures due to the Brill transition, was determined by quenching the samples from elevated temperatures to room temperature after heating. The perfection of the α-crystal, i.e. the crystal perfection index, increases with temperature during continuous heating.
    Zusätzliches Material: 13 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 7
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Acta Polymerica 48 (1997), S. 363-368 
    ISSN: 0323-7648
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The structure of the crystalline hard domains of polyurethane elastomers based on 1,5-naphthalene diisocyanate (NDI) has been investigated by X-ray methods. The specimens were pressed films prepared from NDI and 1,4-butanediol (chain extender), with poly(oxytetramethylene) as the soft segments. Small angle X-ray data show that the hard domains are lamellae oriented preferentially with their planes parallel to the film surface. The corresponding wide angle data show that the hard domains are crystalline, and that the degree of crystallinity can be more than 60%. The hard segment chains are relatively extended and are oriented perpendicular to the film surface: they probably form a staggered array in which they are linked in sheets by hydrogen bonds. Molecular models suggest that the hydrogen bonds are shorter, and hence stronger, than those formed in the hard domains of equivalent elastomers based on diphenylmethane diisocyanate (MDI) or dicyclohexylmethane diisocyanate (HMDI). In addition, the stacking of the naphthylene units is unencumbered by the presence of the bridge methylene groups in the latter systems, and these structural features probably account for the higher melting temperature of the hard domains.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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