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Eingeladener Vortrag
- nein (29)
Rubbers are widely used as main sealing materials for Containers for low and intermediate level radioactive waste and as additional component to metal seals in spent fuel and high active waste containers. The save enclosure of the radioactive container inventory has to be guaranteed according to legislation and appropriate guidelines for long term storage periods as well as down to temperatures of -40 °C for transportation. Therefore the understanding of failure mechanisms that lead to leakage at low temperatures is necessary to ensure a proper material choice which is certainly also influenced by additional factors as e.g. the aging behavior.
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
Faserverbundbauteile werden durch Tränkung von Fasergewebe mit flüssigem Harz, in der Regel Epoxidharzen, und anschließender Härtung des Harzes gefertigt. Dabei kann man das Gewebe im Vorfeld mit reaktivem Harz tränken und als so genanntes Prepreg verarbeiten oder man injiziert das frisch mit dem Härter gemischte Harz in ein Werkzeug, in dem das Gewebe bereits liegt - z. B. beim RTM-Prozess. Ausgehend von der Aufgabenstellung, eine Prepregherstellung mit hohem Qualitätsstandard zu realisieren und Möglichkeiten der Fertigungskontrolle für den Prepreg-Verarbeiter aufzuzeigen, wurde an einem für die Prepregherstellung vorgesehenen Harzsystem eine weitgehende Charakterisierung des Aushärtungsverlaufs vorgenommen. Wegen der Schwierigkeit, schnell konstante Aushärtungstemperaturen zu erreichen, wurden bei allen Methoden mit einer Heizrate von 1 K/min von RT bis 200 °C aufgeheizt.
Harnstoff-Formmassen gehören zu den duroplastischen Formmassen, die im Werkzeug chemisch vernetzen und so ihre herausragende Temperaturbeständigkeit erreichen.
Im Wettbewerb mit Thermoplasten weisen Formmassen den Nachteil auf, dass die Vernetzungsreaktion eine kritische Zeit bedingt, damit die Glasübergangstemperatur soweit verschoben werden kann, dass die heißen Teile stabil und blasenfrei entformt werden können. Die Zykluszeiten sind bei Formmassen daher deutlich höher als bei Thermoplasten.
Eine Möglichkeit, die Zykluszeit zu verringern, wäre die Erhöhung der Werkzeugtemperatur, da bekanntlich eine Erhöhung der Reaktionstemperatur um 10 K zu einer Verdoppelung der Reaktionsgeschwindigkeit führt.
Allerdings wird dabei das Zeitfenster für die Entformung optimal gehärteter Teile deutlich kleiner, der Prozess anfälliger gegen Schwankungen im Prozess und in der Formmasse-Zusammensetzung. Mit einer Online-Kontrolle des Vernetzungszustands sollte es aber gelingen, den Prozess auch bei einer höheren Werkzeugtemperatur noch stabil zu beherrschen. In der vorliegenden Arbeit wird die Methode der dielektrischen Prozesskontrolle in der Fertigung von Spritzgieß-Formteilen erprobt und die Möglichkeiten einer Prozesssteuerung werden herausgearbeitet.
Carbon-fibre prepregs have found widespread use in lightweight applications. They are based on a carbon-fibre fabric impregnated with reactive epoxy resin. Prepreg materials are generally pre-cured so that they have a higher molecular weight than typical resins in order to reduce resin flow, which facilitates storage and later processing properties.
The measurements were carried out using commercially available materials and follow the published DMA investigations of the same material. TMDSC was used to find the correlation between curing conditions, the degree of cure and glass transition temperature. TMDSC has the advantage over standard DSC that it enables better determination of the glass transition temperature, which is often accompanied by an exothermic curing reaction, and thus overshadowed. The influence of the amplitude of temperature modulation was tested in preliminary experiments. For non-cured material a glass transition temperature of approximately 0 °C was determined; whereas for the totally cured material it was approximately 230 °C. The changes in degree of cure, temperature of actual glass transition and post-reaction are given as a function of curing time at 180 °C. The correlation between actual glass transition temperature and degree of cure is derived.
Carbon fibre prepregs have found widespread application in lightweight constructions. They are based on a carbon-fibre fabric impregnated with reactive epoxy resin. DMA measurements under temperature conditions similar to an autoclave programme were carried out using commercially available prepreg material with a high glass transition temperature. The characteristic of the temperature programme was a dynamic heating segment at 1.5 K/min followed by a longer isothermal segment at 180 °C. The courses of the storage modulus E', loss modulus E'' and tanδ were recorded. The measuring frequency was varied between 1 Hz and 33.3 Hz. Gelation and vitrification are assigned. The influence of the measuring frequency on the time to vitrification and the correlation with DSC are discussed. The reaction does not end even after 10 h curing at 180 °C, which is interpreted as the slow cessation of the reaction caused by vitrification.
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.
EVA is a widely used material for the encapsulation of photovoltaic modules. It melts at elevated temperatures, and seals the module before it is crosslinked at temperatures above 130 °C by a peroxide-initiated crosslinking reaction. EVA has good optical properties necessary for application in solar modules. For process optimization and quality management, a method for the quick and reliable characterization of EVA crosslinking behaviour is of great value. Here, the practicability of ultrasound for online crosslinking monitoring is demonstrated. A sound velocity increase of about 8 m/s during the crosslinking reaction is found. The ultrasound results are compared with rheometer measurements performed with a curemeter typically used for the investigation of rubber crosslinking.
Two types of commercially applied Ethylene/Vinyl Acetate Copolymers (EVA) for encapsulation of photovoltaic modules were investigated by the thermal analysis methods of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) in the temperature range from -150 °C to 200 °C. Glass transition, crystal melting and cross-linking were analyzed. The aims of the investigations were to gain more information for incoming goods control and to get information about the whole temperature dependent material properties in the investigated temperature range, starting at very low temperatures up to the crosslinking temperature region.
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
Thermosetting moulding compounds are synthetic materials which can be easily formed in the molten state and achieve high temperature stability due to a cross-linking process which takes place during manufacture. To ensure thermal and mechanical properties, post-curing of moulded phenolic resin components is necessary for high quality applications. In the industrial practice, post-curing time-temperature-programs are heuristically acquired. In this paper, dynamical mechanical thermal analysis is employed to determine optimal post-curing conditions for injection moulded parts from phenolic resin.
In processing fibre-reinforced composites, the curing reaction can be significantly retarded if the temperature and reaction time are not optimally set. In such situations, complete curing is sometimes impossible under practically relevant conditions. It is difficult for processors to recognize or detect incomplete curing. The equilibrium glass transition temperature plays an important role in complete curing in the production process.
Vernetzen statt Verglasen
(2000)
Zusammenfassung
In diesem Beitrag wird zunächst die für die on-line Prozesskontrolle an duroplastischen Formmassen entwickelte Ultraschallmesstechnik vorgestellt. Die Methode basiert auf der Durchschallung des vernetzenden Materials mit Hilfe von in das Werkzeug integrierten druck- und temperaturfesten 4 MHz-Ultraschallsensoren. Die Auswertung von Schalllaufzeit und Signalamplitude erfolgt vollautomatisch und dient der Berechnung von Schallgeschwindigkeit und -dämpfung. Beide Größen repräsentieren die änderung der mechanischen Eigenschaften infolge der Vernetzungsreaktion. Durch Anwendung auf vulkanisierende Materialien sollte die Anwendbarkeit der bewährten Methode erweitert werden. Im Ergebnis wird gezeigt, dass die Größe des Messeffekts von der Menge an Vernetzer (Schwefelkonzentration) abhängt. Bei ausreichend hohem Vernetzungsgrad zeigt die Ultraschallgeschwindigkeit signifikante, gut auswertbare Resultate, die den Ablauf der Vulkanisation on-line zu verfolgen gestatten. Ein Vergleich mit Vulkameterkurven zeigt große ähnlichkeiten und berechtigt zu der Hoffnung, dass die Methode industriellen Einsatz finden kann.
Non-destructive evaluation (NDE) of composites: using ultrasound to monitor the curing of composites
(2013)
Typical composite materials for lightweight construction consist of a fibre (glass or carbon) reinforced thermosetting matrix. The impregnation of the fabric is made with liquid resin – usually epoxy resin or unsaturated polyester resin are used. The main processing methods are resin transfer moulding (RTM) and prepreg technology often used in combination with autoclave curing. After shaping, the resin must be cured. The final properties of the produced parts depend on the curing degree and the final glass transition temperature. Analytical methods and the use of ultrasound for online cure monitoring in the manufacturing process are introduced. Examples for the application of ultrasonic cure monitoring for the production of composite parts for traffic systems are also covered.
Post-annealing of thermosets
(2006)
Carbon fibre prepregs have found widespread application in lightweight constructions. They are based on a carbon fibre fabric impregnated with reactive epoxy resin. Measurements were carried out using commercially available prepreg material. For Dynamic Mechanical Analysis (DMA), a single cantilever measuring device was applied. The DMA results were refined by additional DSC measurements. The measurements were carried out with dynamic heating in the temperature range -90 to 280 °C. The heating rates were 1 and 2 K/min, respectively. A glass transition of the uncured material (Tg0) near 1 °C, and crosslinking-induced vitrification and devitrification at the maximal glass transition temperature of the cured material (Tgmax) in the temperature range 220 to 230 °C were found. The activation energies for the glass transitions were determined using an Arrhenius plot. By detailed consideration of the influence of the frequency on the DMA data, indications for gelation were deduced.
Investigation of curing of epoxy resin composite materials by dynamic mechanical analysis (DMA)
(2006)
"Sehende" Nachtemperung: Praktische Anwendung der Methode der Dynamisch Mechanischen Analyse (DMA)
(2005)
The prospects of modern thermoanalytical methods for characterisation
of flow, curing and final mechanical behaviour of
moulding compounds were demonstrated. Using urea resin
moulding compounds from different manufacturers the possibilities
of the various techniques could be shown. With comparatively
low effort, fundamental information can be gained
before production process had been started. On this basis it is
possible to make appropriate material selection at an early
point in the process chain. On the basis of thermoanalytical
data an incoming goods inspection can be established. Also it
is easy to control the compliance with the conditions of delivery.
In some cases it could also be helpful to have stored analysis
data especially when problems appear in manufacturing
process or unexpected part damages occur
With the ultrasound measuring system it is possible to transfer
the findings from the analytical methods directly to the processes
in the mould. The application of ultrasound provides
Dynamic Mechanical Analysis in the mould. Beside quality
assurance ultrasound can also be used for process optimisation,
especially for reduction of cycle time. In an advanced form
ultrasound information can be used as a basis for improved
machine control based on material state. The ultrasound measuring
system developed by ISK Iserlohn and BAM can be
obtained from the ISK.
Commercially available melamine/phenolic (MP) moulding compounds used for manufacturing electro installation parts were investigated by laboratory thermal analysis methods: Dynamic Mechanical Analysis (DMA), Differential Scanning Calorimetry (DSC) and Dielectric Analysis (DEA). The results were compared with on-line measurements in a compression mould using incorporated dielectric and ultrasound sensors. Softening and cross-linking behaviour were analyzed. For on-line process monitoring, only the ultrasound method worked well. The dielectric method was distorted by water formed as a by-product from the poly-condensation reaction.
Dargestellt wird eine Gegenüberstellung der Ergebnisse von Messungen zur Ozonkonzentrationsbestimmung nach zwei Verfahren. International wird in der Kautschukindustrie ein UV-spektroskopisches Verfahren angewandt. Die deutsche Kautschukindustrie verwendet ein nasschemisches Verfahren. Die beiden Verfahren ergeben nicht die gleichen Ergebnisse. Daher wird der Unterschied genauer ermittelt.
Die Auswirkungen der unterschiedlichen Ozonkonzentrationsbestimmungen auf die Prüfung der Ozonbeständigkeit an Elastomeren werden gezeigt.
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
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.
Epoxy composites used for high-end structural applications are typically cured under the influence of temperature and pressure causing a number of complex chemical and physical transformations. On heating a mould, temperature gradients will occur through the component which will depend largely on the thermophysical properties of the specific composite. The crosslinking reaction is exothermic leading to additional heat release, thus complicating heat transportation models. If such effects are not accounted for, it can lead to variations in resin flow, poor fibre wetting causing voiding and inhomogeneous cure, leading to shrinkage and unfavourable variations in moulded part geometry. Limited information is available for thermal models used in the manufacture of reinforced thermosets. Autoclave [1, 2] and laser or infra-red curing processes [3, 4] typically use constant values determined on fully cured parts. In this work, the variation in thermal conductivity (K) (W/(m K)), thermal diffusivity (a) (m(2)/s) and specific heat capacity at constant pressure (c(p)) (J/(g K) is determined for a carbon fibre prepreg during cure. It is the intention to improve understanding of how these parameters are related to chemical or physical transformations occurring during cure, and where estimates or shortcuts may be used for heat transfer models
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.
Einfluss hoher Temperaturen und Drücke auf die Ultraschalleigenschaften eines Komposit-Prüfkopfes
(2004)
Making Cure Visible
(2005)
Angesichts der spezifischen Bedeutung der Aushärtung von Phenolharzen für ihre Eigenschaften als Ingenieurwerkstoffe besteht großes Interesse an deren quantitativer Charakterisierung. Mittels DSC-Messungen unter hohem Druck (HP-DSC) kann die Vernetzungsreaktion der Phenolharzformmassen durch die Unterdrückung der Verdampfung niedermolekularer Substanzen ohne störende Überlagerungen verfolgt werden. Mittels verschiedener Vernetzungsgrade können die Einflussparameter der Aufheizrate und der Nachtemperung optimiert werden. Die Messergebnisse ermöglichen eine Modellierung der Reaktionskinetik mit dem Ziel einer verbesserten Prozessführung und Qualitätskontrolle in der industriellen Praxis.