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Eingeladener Vortrag
- nein (29)
The application of microwave measurements to the characterisation of rubber compounds vulcanisation is considered. The behaviour of mechanical and microwave (20 GHz) dielectric parameters during vulcanisation was investigated for rubber compounds with different concentrations of active and non-active carbon black. An increase of concentration or activity of carbon black results in the increase of both dielectric permittivity ε?(T) and loss ε?(T) and in the increase of torsion modulus as well. The start of the vulcanisation reaction is indicated by an increase of dielectric permittivity and torsion modulus in all investigated unvulcanised compounds with carbon black. While for compounds with non-active carbon black the vulcanisation can be better indicated by the ε?(T) anomaly, for compounds with active carbon black it is more clearly seen by the change of ε?(T) behaviour.
Cure monitoring of epoxy films by heatable in situ FTIR analysis: Correlation to composite parts
(2014)
The curing mechanism of an epoxy film containing dicyandiamide (DICY) and an epoxy formulation based on diglycidyl ether of Bisphenol A (DGEBA) polymer was studied as a function of various temperature programs. The investigation was performed in situ, using a thin film of the epoxy mixture on a silicon wafer substrate in a heatable transmission tool of a FTIR spectrometer. Based on these model-curing experiments, a major curing mechanism was proposed, taking into account the appearance, the decrease, and the development of characteristic bands at various temperatures. The conclusions of the model curing were correlated to FTIR measurements on a real, 50-mm-thick glass fiber reinforced component composite part from a technical process. It could be shown that characteristic bands that develop at curing temperatures above 150°C appear especially in the center of the thick sample. From the chemical or molecular point of view, this demonstrates the established technician's understanding that temperature control inside a large-scale fiber composite of, for example, aircraft, wind-turbine, automotive applications component is of major importance.
Partial discharges may cause damage to electrical insulation of high voltage equipment. They initiate elastic waves in the insulating material, e.g. in the stress cone of an outdoor termination. Localisation of the origin of such elastic waves can help to predict serious damaging processes in the electrical insulation. In order to measure and evaluate the wave propagation effects in typical multilayered elastomeric structures, knowledge of the material properties is required. The propagating velocity and the attenuation of longitudinal waves are important parameters. Values for these quantities found in the literature were not appropriate. Therefore, for cross-linked polyethylene (XLPE) and cured liquid silicone rubber (LSR), the longitudinal wave velocity and the attenuation were evaluated in the temperature interval from -20°C to 50°C and in the frequency range from 200 kHz to 600 kHz using a two-sample ultrasound technique. The loss factor was determined from these measured quantities. Additionally, low frequency Dynamic Mechanical Thermal Analysis (DMTA) was applied to investigate LSR and XLPE in a temperature interval between -100 and 50°C and to check qualitatively the ultrasound data.
The time-dependent sorption of biodiesel in a typical polyethylene for container applications is investigated in comparison to conventional diesel fuel at three different temperatures. In this context, the desorption behavior is also addressed. Subsequently, the effects of both penetrants on mechanical properties are characterized in terms of impact strength and dynamic-mechanical analysis. The discussion of property changes is firstly based on the sorption kinetics of biodiesel and diesel, which is determined by immersion experiments allowing for the calculation of respective diffusion coefficients. Changes in impact strength as determined by the Charpy method are further characterised in more detail by analyzing the fracture surfaces, and correlated with results of dynamic-mechanical analysis.
In a previous paper we investigated the influence of sorbed biodiesel or diesel on mechanical properties of a typical polyethylene grade for tank applications. Besides the basic sorption and desorption behavior of these two fuels, the study addressed the concentration-dependent mechanical properties as revealed by a non-instrumented Charpy impact test and dynamic mechanical analysis (DMA). In the present paper we extend this investigation focusing on the temperature-dependent impact fracture behavior. Therefore, an instrumented Charpy impact test was employed, allowing a more detailed analysis of the fracture behavior. Furthermore, from the load-time-diagrams obtained from the instrumented impact test, corresponding fracture times can be calculated, allowing a clear correlation of the fuel sorption induced changes in fracture toughness with the enhanced ß-relaxation observed by DMA. As in the previous study, the fracture surfaces of the impact tested specimens were analyzed in order to confirm the brittle or ductile character of the fracture indicated by impact strength and the corresponding load-deflection diagrams.
Adhesion of amorphous polymers as a function of temperature probed with AFM force-distance curves
(2005)
Forcedisplacement curves have been obtained with a commercial atomic force microscope at different temperatures and probe rates on a thick film of poly(n-butyl methacrylate) and on two films of polystyrene with different molecular weight. In a previous publication [B. Cappella, S.K. Kaliappan, H. Sturm, Macromolecules 38 (2005)1874] the analysis of forcedisplacement curves has been focused on the stiffness and on the Young's modulus of the samples. In the present publication we consider the temperature dependence of the work of adhesion. We have obtained master curves of the work of adhesion at fixed maximum loads and, by comparing the results of the two analysis, we show that the work of adhesion follows the WilliamsLandelFerry equation with the same coefficients previously found for the Young's modulus. Furthermore, we show that the temperature dependence of the work of adhesion of the polymers is a consequence of the temperature dependence of the tipsample contact area and in the end of the temperature dependence of the stiffness and of the elasticplastic properties of the samples.
Ultrasound waves penetrate solid objects without damaging them. Their fields of application range from the imaging of internal organs in medicine, to interior testing of mechanical and chemical engineering components. However, ultrasonic systems can also be used to visualise the way the mechanical properties of reactive resins change during processing in the mould.
Ultraschallwellen durchdringen Festkörper, ohne sie zu schädigen. Der Einsatzbereich von Ultraschall reicht von der Darstellung der inneren Organe in
der Medizin bis zur Prüfung des Inneren von Bauteilen im Maschinen- und
Anlagenbau. Ultraschall-Systeme können jedoch auch genutzt werden, um
sichtbar zu machen, wie sich mechanische Eigenschaften von Reaktionsharzen
während ihrer Verarbeitung im Werkzeug verändern.
The curing conditions play an important role in the quality assurance of composite products.
Especially as composite materials are widely used in high tech areas so that they are required to fulfil high quality Standards. Some problems which occur during curing, for instance undercuring, can hardly be detected using Standard NDT investigations, mainly because they are manifested only at high temperatures, particularly close to glass-rubber-transition. On-line eure monitoring has the outstanding advantage that it can monitor the material parameters even at the highest temperatures possible.
In recent years eure monitoring with ultrasonic methods has become more populär. In comparison to dielectric methods mechanical parameters are measured directly. The quantities to be measured are the velocity and the attenuation of the sound wave. On this basis the storage and loss modulus can be calculated. Depending on the form of excitation with longitudinal or transversal waves these moduli are referred to as long wave or shear modulus.
Well developed Computer based technology and sensor materials are available in the non-destructive testing (NDT) market. The measuring equipment employed a commercial NDT System, which worked computer-aided. With a special Software the demands of automatic Operation under industrial conditions was accomplished. This measurement equipment was tested on composites. Its structure, performance and some practical results will be presented in the following paper.
In recent years eure monitoring with ultrasonic methods became more important. An on-line measurement System for industrial applications is presented in this paper. It operates in through-transmission and the measured parameters are the sound velocity and the attenuation of the sound wave. An objective of this paper is to establish the ränge of possible applications for an ultrasonic eure monitoring System.
Das Fließ-Härtungs-Verhalten von Duroplastformmassen wird gegenwärtig nur
unvollständig durch empirische Größen beschrieben. Diese ungenauen und
unsicheren Angaben können zu Schwierigkeiten bei der optimalen Einstellung
der Fertigungsmaschinen des Verarbeiters führen. Insbesondere Veränderungen
der Formmasseeigenschaften während des Transportes und der Lagerung stören
die Produktion. Das vorgestellte Messverfahren mit Ultraschall-sensoren ermöglicht
die schnelle und vollständige Erfassung des Fließ-Härtungs-Verhaltens, auch
während des technologischen Prozesses. Experimentelle Ergebnisse zu
Alterungs-erscheinungen dieser Formmassen illustrieren den Nutzen des
Verfahrens für Formmasse-produzenten und -verarbeiter.
Zusammenfassung
Der Ausgangspunkt für diese Arbeiten ist eine in [1] beschriebene Ultraschall-(US)-Sensorik zur Aushärtungskontrolle. Sie wurde für rieselfähige Formmassen entwickelt [2,3]. Darauf aufbauend ist es das Ziel der vorliegenden Arbeit, die Voraussetzungen für den Einsatz dieser Sensorik beim Harzinjektionsverfahren zu schaffen und ihre Kalibrierung durch rheologische und DSC-Messungen zu ermöglichen.
Der erste Teil des Beitrages beschäftigt sich mit dem technologischen Ablauf des Harzinjektionsverfahren und den Einsatzmöglichkeiten der US-Sensorik bei dieser Technologie. Ergebnisse von Schallgeschwindigkeits- und Dämpfungsmessungen für EP-Harze werden vorgestellt.
Im zweiten Teil wird auf das Kalibrieren der US-Sensorik für den Verarbeiter eingegangen. Es kann mittels der bisherigen Prozessführung oder durch Vergleich mit den Ergebnissen anderer Mess-Verfahren wie Rheometer- oder Differential-Scanning-Calerometry-(DSC)-Messungen erfolgen.
Ultrasound on-line NDT methods have been demonstrated as a useful tool for monitoring the curing reaction of thermosets. In order to achieve this ultrasound sensors are incorporated into compression, injection and RTM (resin transfer) mould. For many commercial products imprints or any surface markings upon the moulded product are undesirable. Due to its physical properties ultrasound has a large advantage over other techniques for similar applications. The sound wave can pass through the wall of the mould and direct contact with the moulded part is not required. In this particular case one fundamental problem is a good coupling of the sensors to the mould wall. Several mediums came into question but because of the high technical (e. g. temperature and long time stability) and practical demands, it was decided that dry (non-fluid) coupling would be the most promising candidate. A handful of coupling foils suitable also at high temperatures and for long time application under industrial conditions were tested and are presented in this paper.
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.
Ferroelektrete sind zelluläre polarisierte Polymere, die ferroelektrische und dadurch auch piezoelektrische Eigenschaften aufweisen. Unter anderem werden sie für den Bau von Mikrofonen und Ultraschallwandlern für Materialprüfung eingesetzt. Dabei erweist sich ihre besonders niedrige akustische Impedanz als Vorteil. Ursache dafür ist vor allem ihr außergewöhnlich niedriger Elastizitätsmodul in Dickenrichtung. In diesem Beitrag werden zwei Methoden für die Ermittlung des Elastizitätsmoduls des geladenen zellulären Polypropylens (zPP) dargestellt. Die erste ist eine neuartige modellgestützte Methode mittels Laservibrometrie an dem eigenentwickelten Polypropylen-Wandler, wobei die Resonanzschwingung des Wandlers bei 250 kHz gemessen wird.
Die zweite Methode ist dynamisch-mechanische Analyse (DMA) durchgeführt mit Frequenzen von 0,3 bis 50 Hz, erstmalig für das zPP angewendet.
Viscoelastic properties of cellular polypropylene ferroelectrets (PP FEs) were studied at low
frequencies (0.3–33 Hz) by dynamic mechanical analysis and at high frequencies (250 kHz) by laser Doppler vibrometry. Relaxation behavior of the in-plane Young’s modulus (Y´
11~1500 MPa at room temperature) was observed and attributed to the viscoelastic response of polypropylene matrix.
The out-of-plane Young’s modulus is very small (Y´33≈0.1 MPa) at low frequencies, frequency- and stress-dependent, evidencing nonlinear viscoelastic response of PP FEs. The highfrequency mechanical response of PP FEs is shown to be linear viscoelastic with Y´33≈0.8 MPa. It is described by thickness vibration mode and modeled as a damped harmonic oscillator with one degree of freedom. Frequency dependence of Y*33 in the large dynamic strain regime is described by the broad Cole-Cole relaxation with a mean frequency in kHz range attributed to the Dynamics of the air flow between partially closed air-filled voids in PP FEs. Switching-off the relaxation contribution causes dynamic crossover from the nonlinear viscoelastic regime at low frequencies to the linear viscoelastic regime at high frequencies. In the small strain regime, contribution of the air flow seems to be insignificant and the power-law response, attributed to the mechanics of polypropylene cell walls and closed air voids, dominates in a broad frequency range. Mechanical Relaxation caused by the air flow mechanism takes place in the sound and ultrasound frequency range (10 Hz–1MHz) and, therefore, should be taken into account in ultrasonic applications of the PP FEs deal with strong exciting or receiving signals.
Today rubber is due to its unique property profile one of the most important materials for the production of bearings, dampers or also tires and tubes. In the production of rubber goods a chemical cross-linking reaction (vulcanisation) generates the final material properties. This process takes place during the shape giving of the rubber compound in the mould and can proceed for several minutes. The cross-linking process is influenced by the mixture of the basic polymer, the cross-linking agent, the influence of catalysts and inhibitors and especially the processing conditions. The quality of every ingredient, the reproducibility of the mixing ratio, the homogeneity of the mixture and the accurateness in temperature control can have a direct influence on the cross linking reaction. To control the quality of a rubber compound and verify the processing conditions in industry moving die rheometers, named curemeter, are involved in the production process. Starting from our experience in cure monitoring of thermosetting materials by measuring ultrasound velocity in the mould we extended the measuring principle to rubber vulcanisation monitoring. After first investigations using a compression mould we dealt here with on-line monitoring of vulcanisation in an injection moulding process which is one of the most used techniques in rubber industry.
Aufgrund ihrer einfachen und zuverlässigen Anwendung werden Elastomere für viele Dichtungsaufgaben eingesetzt. In vielen Anwendungsbereichen, wie z.B. Verkehr, Luftfahrt und Verfahrenstechnik, können während des Einsatzes tiefe Temperaturen auftreten, bei denen die Funktionsfähigkeit der Dichtung erhalten bleiben muss. Daher ist die Untersuchung des Verhaltens von Elastomerdichtungen bei tiefen Temperaturen wichtig, um ihren Temperatureinsatzbereich nach unten abzugrenzen und dadurch einen verlässlichen Betrieb zu sichern. Ziel dieser Arbeit ist es, den sicheren Einschluss von gefährlichen Gütern unter verschiedenen Umgebungsbedingungen und über lange Zeiten zu ermöglichen bzw. die Materialauswahl entsprechend zu steuern.
Rubbers are often used for seal applications due to their special material properties and easy use. In many applications the material is exposed to low temperatures during Operation. Therefore it is important to know the material behavior at low temperatures to determine the temperature ränge that allows a Safe Operation of the seal, e.g. in storage and transport Containers for radioactive materials.
The seal function of an elastomer is limited in temperature by the rubber-glass transition during which the material properties change from rubber-like to stiff and glass-like. For a given application this correlation is not trivial and therefore needs an in-depth investigation under consideration of the physical properties and the
application conditions.
In this work different analytical methods are used to characterize the material behavior at low temperature in the ränge of the glass-rubber-transition and are compared with the quality of Operation of a component which is here defined by the detected leakage rate.
In consideration of the influence of the curing reaction on the material properties of elastomers, it is very important to control the vulcanization process properly.
As shown previously [1], the effects of the vulcanization reaction of an elastomer can be monitored by use of ultrasonic sound waves. This technique has to a certain degree a high similarity to the standard curemeter test according to ISO 6502 but can be applied also inside a production tool.
So far, the method was only applied to the vulcanization of one compound at a given temperature and sample thickness. This is now complemented with measurements on another compound system at different temperatures and sample thicknesses.
The expected effects of temperature and thickness on the curing behaviour were found by use of the ultrasound online control.
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.
Monitoring the vulcanization of elastomers: Comparison of curemeter and ultrasonic online control
(2009)
The vulcanization of elastomeric materials has a high impact on the properties of the final product. Therefore, it is important to monitor and control this crosslinking process. A common technique to attain the necessary curing time is the use of a curemeter in accordance with ISO 6502 in order to determine the time for full cure of a sample with a standardized geometry. Based on this result and a lot of practical experience, the required curing time for a given product geometry is estimated. Within the scope of this work, a new analysis technique will be compared with the standard procedure. The ultrasonic online control employs ultrasound waves to measure the changes in material properties caused by vulcanization. For this study, a natural rubber compound with a conventional curing system was investigated by both techniques. It was found that the results of the ultrasonic technique show good agreement with the results of the curemeter.
A new method for the evaluation of the low temperature properties of rubber materials is presented. The method emulates the standardized compression set measurement, which is frequently used for sealing materials, but can be performed within a considerably shorter time. The results are compared with the standard test and found to be qualitatively the same. Slight differences are discussed on the basis of the differences in the measurement procedures. Further data evaluation is done by fitting functions to describe the material behaviour.
Für Elastomenwerkstoffe im Allgemeinen und im Bereich der Dichtungstechnik im Besonderen ist der Druckverformungsrest eine wichtige Kenngröße zur Beurteilung der Eignung eines Werkstoffs bzw. der Funktion eines Bauteils. Er ermöglicht eine Einschätzung des zeitabhängigen Rückstellverhaltens eines Werkstoffs nach Deformation. Dieses ist für Dichtungen von besonderer Bedeutung, da der Test deren Einbauzustand nachstellt.
Oft wird er, bei der Prüfung unter erhöhten Temperaturen, zur Beurteilung des Alterungsverhaltens verwendet und kann anhand eines definierten Versagenskriteriums zur Lebensdauerabschätzung eingesetzt werden. Bei tiefen Temperaturen dient er dazu, die limitierende Einsatztemperatur zu bestimmen. Dabei spielt eine Alterung im eigentlichen Sinne nur eine untergeordnete Rolle, wohl aber physikalische Effekte wie Tieftemperaturkristallisation und Glasübergang. Diese Effekte sind weit weniger durch lange Lagerzeiten beeinflusst als die eigentliche Alterung.
Die Versuchsdurchführung unterscheidet sich je nach angewandter Norm und kann einen deutlichen Einfluss auf den Druckverformungsrest haben. Alle standardisierten Methoden sind aufgrund der langen Lagerzeiten relativ langwierig und erfordern das regelmäßige Eingreifen durch den Prüfer. Zusätzlich sehen einige Methoden nur die Bestimmung eines einzelnen Wertes nach einer definierten Zeit vor.
Um die Messungen zu beschleunigen wurde eine Methode entwickelt, die automatisch die erforderlichen Messungen bei mehreren Temperaturen durchführt.
Dazu wird ein Prüfgerät der Dynamisch Mechanischen Analyse verwendet, das kontinuierlich die Deformation während eines frei programmierbaren Temperaturzyklus misst, wodurch eine sehr große Datenmenge verfügbar ist.
Ein Vergleich der neuen Methode mit den Ergebnissen des nach ISO 815 genormten Messprinzips ergibt eine gute Übereinstimmung. Ergebnisse der neuen Methode werden vorgestellt und die Vorzüge der kontinuierlichen Datenerfassung, z.B. für die Materialauswahl, diskutiert.
Die vorgestellten Ergebnisse beziehen sich zum großen Teil auf die in beschriebenen Untersuchungen und Ergebnisse.
Der Druckverformungsrest (DVR) stellt insbesondere für Dichtungsanwendungen eine wichtige Kenngröße zur Beurteilung der Eignung eines Elastomers dar. Er ermöglicht die Einschätzung des zeitabhängigen Rückstellverhaltens eines Werkstoffs nach Deformation. Neben der Prüfung bei erhöhten Temperaturen, zur Beurteilung des Alterungsverhaltens, lässt sich bei der Durchführung bei tiefen Temperaturen die limitierende Einsatztemperatur bestimmen. Die Versuchsdurchführung unterscheidet sich je nach angewandter Norm und kann einen deutlichen Einfluss auf den DVR-Wert haben. Um bei tiefen Temperaturen eine schnelle Aussage zu gestatten, ist eine im Vergleich zu genormten Methoden deutlich schneller durchzuführende, automatisierte Methode entwickelt und mit Standardmethoden verglichen worden. Durch kontinuierliche Messung des Druckverformungsrests kann die Kinetik der Materialrückstellung betrachtet und dadurch ein effizienter Materialvergleich und eine effiziente Materialauswahl ermöglicht werden. Compression set (CS) is especially for sealing applications an important parameter for material selection. It allows an assessment of the time dependent recovery after deformation.
In addition to testing at elevated temperatures which aims at the evaluation of the ageing behaviour, testing at low temperatures permits the determination of the low working temperature limit. The test procedure varies depending on the applied standard and can show a significant effect on the CS value. In order to allow a quick statement regarding low temperatures an automated procedure being significantly faster realisable in relation to the standardised methods has been developed and compared with standard procedures. Continuous measurement of the compression set allows evaluating the recovery kinetics and therefore an efficient comparison and selection of materials.
The method for the determination of compression set values with a Dynamic Mechanical Analysis (DMA) setup at low temperatures, which was presented previously, allows a much faster and readily automated procedure than the standardized compression set test according to ISO 815-2. This method is applied to a series of different elastomeric materials that are commonly used for sealing applications. The results of the compression set test are compared with results from thermal analysis to allow an in depth comparison of the material behaviour at low temperatures.
Furthermore, a comparison between two EPDM materials is presented. These materials show very similar properties determined by thermo analytical methods such as Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) but differ clearly in their compression set behaviour. This comparison shows the importance and value of information of the compression set test in addition to thermal analysis to judge the behaviour of sealing materials and confirms the relevance of the new compression set test method for the investigation of low temperature properties of elastomers.
The investigation of low temperature properties of elastomeric sealing materials by means of thermo-analytical methods is a sound way to get information about the glass transition process.
The breakdown temperature of the sealing function of O-ring seals was measured in a component test setup depending on material and degree of compression.
An in depth explanation of the observed component tests behaviour is currently in preparation. It requires the results of thermo-analytical methods and measurements as the compression set (not shown here). With that, a model was developed to describe the correlation between physical material parameters and observed component behaviour.
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.
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 encapsulation 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 during transport.
Therefore the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance.
It is known that the material properties of rubbers are strongly temperature dependent. At low temperatures this is caused by the rubber-glass transition (abbr. glass transition). During continuous cooling the material changes from rubber-like entropy-elastic to stiff energy-elastic behaviour, that allows nearly no strain or retraction, due to the glass transition. Hence rubbers are normally used above their glass transition but the minimum working temperature limit is not defined precisely, what can cause problems during application. 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 standardized measurements as the compression set according to ISO 815. To reduce the test time of the standard tests a faster technique was developed.
Additionally, the breakdown temperature of the sealing function of complete O-ring seals is measured in a component test setup to compare it with the results of the other tests. The experimental setup is capable of measuring the leakage rate at low temperatures by the pressure rise method.
A fluorocarbon rubber (FKM) was selected for this investigation as it is often used for radioactive waste containers. Some materials (seals and test sheets) were purchased from a commercial seal producer and some materials were compounded and cured at BAM in form of rubber sheets.
Elastomers are widely used as the main sealing materials for containers for low and intermediate level radioactive waste and as an additional component to metal seals in spent fuel and high active waste containers. The safe encapsulation of the radioactive container inventory has to be guaranteed according to regulation and appropriate guidelines for long term storage periods as well as for temperatures as low as -40°C during transport. Therefore, the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance. It is known that the material properties of elastomers are strongly temperature dependent. At low temperatures, this is caused by the rubber-glass transition (abbreviated: glass transition). During continuous cooling, the material changes from a rubber-like entropy elastic to a stiff energy elastic behaviour, which allows nearly no strain or retraction. Hence, rubbers are normally used above their glass transition, but the minimum working temperature limit is not defined precisely; this can cause problems during the above noted applications. Therefore, the lower operation temperature limit of elastomer seals must be determined in dependence of the material properties. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) are combined with standardised measurements to determine the compression set according to ISO 815. To reduce the test time of the standard tests, a faster technique than normally used was developed. Additionally, the breakdown temperature of the sealing function of complete O ring seals was measured in a component test set-up to compare it with the results of the other tests. The experimental set-up is capable of measuring the leakage rate at low temperatures by the pressure rise method. A fluorocarbon rubber (FKM) was selected for this investigation as it is often used for radioactive waste containers. The materials (seals and test sheets) were purchased from a commercial seal producer.
Die Messung des dynamischen Speichermoduls mit der Dynamisch-Mechanischen-Analyse ermöglicht einen schnellen Überblick über das temperaturabhängige Verhalten von elastomeren Dichtungsmaterialien. Ein direkter Rückschluss von der so ermittelten Glasübergangstemperatur Tg auf die Versagenstemperatur einer Dichtung ist aber ohne zusätzliche Messungen bisher nicht möglich.
Mit den Ergebnissen des Druckverformungsrestes DVR und des DVRDMA ist eine ge-nauere Beschreibung der Tieftemperatureigenschaften und dadurch der Funktion von elastomeren Dichtungsmaterialien möglich. Messungen ergeben beispielsweise, dass sich das EPDM bei einer Temperatur von -40 °C laut der Dynamisch Mechanischen Analyse noch im gummielastischen Bereich befindet. Die DVRDMA-Werte zeigen eine Rückstellung um mehr als 40 % der Ausgangsdeformation in wenigen Minuten.
Mit derart detailliert bestimmten Eigenschaften lassen sich Rückschlüsse auf einsatzspezifische Anforderungen wie z. B. die Dichtwirkung in Abhängigkeit von Betriebstemperatur und mechanischer Belastungsgeschwindigkeit ziehen, so dass je nach Einsatzbedingungen für die Dichtungen eine geeignete Materialauswahl getrof-fen werden kann.
To achieve the required tightness levels of Containers for low and intermediate level radioactive wastes rubbers are widely applied as main sealing materials. The save encapsulation of the radioactive Container contents has to be guaranteed according to legislation and appropriate guidelines for long storage periods as well as down to temperatures of-40 °C during transportation.
Therefore the understanding of failure mechanisms that lead to leakage at low temperatures is of high importance.
It is known that the material properties of rubbers are strongly influenced by temperature. At low temperatures this is caused by the rubber-glass transition (abbr. glass transition). During continuous cooling the material changes from rubber-like entropy-elastic to stiff energy-elastic behaviour, that allows nearly no strain or retraction. Therefore, rubbers are normally used above their glass transition but the minimum working temperature limit is not defrned precisely, what can cause problems during application. The temperature ränge where full functionality is possible is strongly dependent on the application conditions and the material.
For this investigation mainly ethylene propylene diene (EPDM) and fluorocarbon rubbers (FKM) were selected as they are often used for radioactive waste Containers.
Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) are typically used for the determination of the temperature ränge of the glass transition process. The standardized compression set measurement according to ISO 815 is common for investigation of rubber sealing materials as the test simulates the seal behaviour after release. To reduce the test time of the Standard tests a faster technique giving the same information was developed.
Additionally, the breakdown temperature of the sealing function of complete O-ring seals is measured in a component test Setup to compare it with the results of the other tests. The experimental Setup is capable of measuring the leakage rate at low temperatures by the pressure rise method.
A model was developed that allows calculating the minimum working temperature limit of a seal by combining the results of the applied methods.
Rubbers are widely used as sealing material in various applications. In many fieldsthefunction of seal materials at lowtemperatures is required. Therefore the understanding of faiiure mechanisms that lead to leakage at low temperatures is of high importance. 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 results of standardized measurements as the compression set according to ISO 815. To reduce the test time of the Standard tests a faster and more efficient technique was developed and applied. In addition the breakdown temperature of the sealing function of O-ring seals at lowtemperatures is measured in a component test Setup in dependence of the material and the degree of compression.
Elastomere werden vielfach als Dichtungsmaterial für verschiedene Anwendungen eingesetzt.
In vielen Bereichen ist die Funktion der Dichtung auch bei tiefen Temperaturen erforderlich. Daher ist das Verständnis des Versagensmechanismus von großer Bedeutung.
Normalerweise werden Elastomere oberhalb ihres Glass-Gummi Umwandlungsbereiches eingesetzt, wobei die minimale Einsatztemperatur nicht exakt definiert ist. Daher ist es sinnvoll, diese untere Temperatureinsatzgrenze in Abhängigkeit von den Materialeigenschaften zu bestimmen. Hierfür werden die Ergebnisse der thermischen Analyse mit den Resultaten des Druckverformungsrests aus einer abgewandelten Messung mit der Dynamisch Mechanischen Analyse (DMA) kombiniert.
Weiterhin werden Ergebnisse von Bauteilversuchen vorgestellt und diskutiert.
Die vorgestellten Untersuchungen wurden zum großen Teil auf Untersuchungen im Rahmen der Dissertation von M. Jaunich durchgeführt.