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Eingeladener Vortrag
- nein (29)
The technique normally used to measure Cp during isothermal cure is Temperature Modulated - Dynamic Scanning Calorimetry TM-DSC. It is however not standardised, experimentally complicated and quite time intensive. As will be shown, Cp may also be estimated during isothermal cure just from using dynamic heating experiments on a fully cured sample. Such values are often sufficient for isothermal heat transfer models that otherwise employ a constant Cp value obtained from the fully cured epoxy. Secondly, the results from dynamic heating experiments provide a quick means, in comparison to isothermal TMDSC measurements, of estimating Cp variation during cure as well as providing a good estimate value for Cp towards the end of isothermal cure. As will be shown, such values obtained from a standardised measurement procedure are very helpful in setting up TMDSC experiments that are more sensitive to experimental error influenced by factors such as sample weight and geometry.
The DSC results illustrate that the measured heat capacity Cp for a fully cured epoxy over a temperature range are very similar to values for samples partially cured at corresponding isothermal temperatures, under the prerequisite that vitrification takes place. In such cases the primary influence on Cp is specific measurement temperature and not degree of cure. For isothermal cure temperatures investigated between 150 and 200 °C, the total change of Cp during cure is nearly constant and correlates well with values published by authors on other epoxy based systems. Taking Cp variation as constant, it is possible from just dynamic heating experiments on the cured epoxy to estimate Cp for the uncured epoxy system at specific cure temperatures. The next step would be to estimate the full Cp profile during isothermal cure, however, in such cases, the time to vitrification would also be needed as additional information.
Thermoanalytische Charakterisierung von Ethylen-Vinylacetat-Copolymer (EVA) für Photovoltaikmodule
(2011)
Das Ziel der Untersuchungen war mit Hilfe von DSC und DMA EVA-Folien im Anlieferungszustand hinsichtlich der Lage der Glasübergangstemperatur, des Schmelzverhaltens und der Temperaturabhängigkeit der Vernetzungsreaktion zu charakterisieren. Auf dieser Basis sollte die Lieferstabilität im Sinne einer Wareneingangskontrolle auf eine messtechnische Basis gestellt werden. In einem 2. Schritt sollte die vernetzte Folie dahingehend charakterisiert werden, ob infolge der Vernetzung eine Änderung der
The temperature dependences of dielectric permittivity and elastic modulus of poly(vinylidene fluoride - hexafluoropropylene) (P(VDF-HFP)) are compared and explained by use of structural data obtained by differential scanning calorimetry and X-ray analysis. Special emphasis is put on the effect of uniaxial stretching which renders the polymer ferroelectric. It is shown that dielectric and mechanical relaxations at the glass transition (aa relaxation) are closely related and not significantly affected by stretching. It is further confirmed that stretching destroys the non-polar spherulitic crystalline structure and produces relatively small-sized polar crystallites. This manifests in the disappearence of the so-called ac relaxation which is associated to molecular motions within the spherulitic crystalline lamellae. However, there are discrepancies between dielectric and mechanical losses above the glass transition which point towards a still not described structural transition.
Rubber is widely used as sealing material in various applications. In many fields the sealing function at low temperatures is necessary. Therefore the understanding of failure mechanisms is of high importance. Rubbers are normally used above their glass-rubber transition region but the minimum working temperature limit is not defined precisely. Therefore the lower operation temperature limit of rubber seals should be determined in dependence of the material properties. The results of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) are combined with the results of the standardized compression set according to ISO 815 respectively a modified test using the DMA equipment.
Über die in der Technik weit verbreitete typisierte Harnstoffformmasse UF 131.5, ein Aminoplast, wird berichtet, dass sie im Zuge der thermisch aktivierten Vernetzungsreaktion wegen "Überhärtung" mangelhafte Eigenschaften annimmt. Zur Verifizierung dieses Effektes werden mithilfe der Ultraschall-Prozesskontrolle gezielt Proben unterschiedlicher Aushärtegrade hergestellt. Sie werden mit verschiedenen Methoden, wie der "Kochprobe" und der Thermoanalyse, charakterisiert und auf ihre Materialeigenschaften untersucht. Dabei zeigt sich ein deutlicher Einfluss der Härtezeit auf die Glasübergangstemperatur der Formmasse. In den mechanischen Eigenschaften ist eine Veränderung allerdings nur in der Schlagzähigkeit festzustellen, die sich mit steigender Härtezeit sogar wesentlich verbessert.
Epoxy carbon-fibre prepreg, Hexcel Type 6376 HTS, was investigated using Dynamic Mechanical Analysis (DMA). The DMA characteristic parameters are storage modulus E', loss modulus E' and loss factor tanδ. These parameters are ideally suited to observe the vitrification, referred to as glass transition, resulting from the cross-linking reaction. Detection of the cure state may also be achieved by determining the momentary glass transition temperature of partially cured samples. The consequent use of a multi-frequency measuring regime was used to derive the apparent activation energy for the glass transition process. Different temperature programs were also applied to monitor the curing process directly, as well as to investigate the different states of incomplete cure reached in preceding curing steps. The intention was to provide better understanding of the consequences of an interrupted autoclave curing process and to use DMA to detect the cure state achieved. With DMA, the continuation of an incomplete curing process also can be monitored. DMA measurements up to 300 °C showed, furthermore, that the final glass transition temperature was reduced by thermal degradation at high temperatures.
With an extended contact and non-contact mode scanning force microscope samples with different heterogeneous electrical properties can be characterized. The contact mode method allows the determination of local electric conductivities of heterogeneous systems at the sample surfaces. An interpretation of this behaviour can be obtained in combination with other SFM modes such as topography, friction and compliance used simultaneously. The non-contact mode SFM allows to get more information about the local surface charge of heterogeneous samples. In this paper two new SFM approaches will be discussed on examples of carbon-fibre reinforced, organic and ceramic materials
Two different approaches to investigate the local complex conductivity and the surface charge with Scanning Force Microscopy (SFM) techniques are presented. It is shown that the measurement of local electrical properties with SFM leads to interesting information about the composition of electrically heterogeneous surfaces
A stoichiometric amineepoxy formulation was cured in the presence of a thermoplastic, namely poly(vinylpyrrolidone) (PVP). The epoxy system consisted of the resin diglycidyl ether of bisphenol A (DGEBA) and the aromatic curing agent 4,4'-diaminodiphenylsulfone (DDS). As shown for this system in a former study by Oyama et al. [Oyama HT, Lesko JJ, Wightman JP. J Polym Sci B 1997;35:33146. [36]], preferential absorption of amine molecules by PVP can occur. In the present study, the focus is on the variations of local elastic properties within the epoxy interphase adjacent to the PVP layer. The curing was performed close to the glass transition temperature, Tα, of the PVP film, namely at 170 °C. Variations of the local amine concentration were tracked using energy-dispersive analysis of X-rays (EDX), by taking benefit of the sulfur contained in DDS. Using temperature-dependent dynamic mechanical analysis (DMA), a series of epoxy reference samples of different amineepoxy concentration ratios, r, was investigated in order to work out the relationship between r and the epoxy storage modulus at room temperature. In the excess-epoxy regime, r<1, the modulus is observed to increase with departure from the stoichiometric ratio, r=1. Considering the respective suppression of the ß-transition, the observed characteristic can be explained by an antiplasticisation effect. Depth-sensing indentation (DSI) experiments across the epoxy/PVP interphase provided evidence for strong modulus variations. In consistency with the EDX and the DMA data, in the vicinity of the PVP layer the local epoxy modulus is increased. The total change of the epoxy Young's modulus is ~1.1 GPa. However, the total width of the modulus decay of ~175 µm is ~2.5 times larger than the one of the DDS concentration gradient. This finding is discussed in terms of additional spatial variations of the DGEBA concentration as well as long-range diffusion currents of DDS induced by the interdiffusion processes and their effect on the final network of crosslinks.