TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - Mc Hugh, Jarlath T1 - Dynamic mechanical analysis (DMA) of epoxy carbon-fibre prepregs partially cured in a discontinued autoclave analogue process N2 - 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. KW - Composites KW - Epoxy KW - Cross-linking KW - Prepreg KW - Degree of cure KW - Glass transition PY - 2015 DO - https://doi.org/10.1016/j.polymertesting.2014.11.004 SN - 0142-9418 VL - 41 SP - 140 EP - 148 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-32325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Investigation of Elastomer Seal Behaviour for Transport and Storage Packages T2 - Ramtrans 2015, 10th International Conference on Radioactive Materials Transport and Storage CY - Oxford, United Kingdom DA - 2015-05-19 PY - 2015 AN - OPUS4-33454 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Alterung von Elastomerdichtungen für Lagerbehälter N2 - Unsere Aufgabe im Fachbereich 3.4 der Bundesanstalt für Materialforschung und prüfung (BAM) ist die sicherheitstechnische Begutachtung von Transport- und Lagerbehältern für radioaktiven Abfall, die für langfristige Zwischenlagerung ausgelegt sind. Ein Arbeitsschwerpunkt ist die Bewertung der Lebensdauer von Metall- und Elastomerdichtungen in den Behältern im Hinblick auf die Anforderungen für langfristige Behältersicherheit (min. 40 Jahre in Deutschland). Um die Eigenschaftsänderungen der Elastomerdichtungen während einer beschleunigten Alterung über lange Zeiträume (bis zu fünf Jahre) untersuchen zu können, wurde ein Alterungsprogramm an ausgewählten Elastomeren (HNBR, EPDM, FKM) begonnen. Im Gegensatz zu Normalterungsverfahren altern wir keine Normteile, sondern O-Ringe im unverpressten sowie verpressten Zustand. Diese Vorgehensweise ermöglicht die Bewertung des Einflusses der Verpressung auf die Alterung sowie die Untersuchung des Bauteilversagens mittels Leckageratenmessungen unter anwendungsnahen Bedingungen. Weitere Charakterisierungsmethoden sind Härtemessung, dynamisch-mechanische Analyse (DMA), Thermogravimetrie (TGA), Druckspannungsrelaxation, Druckverformungsrest (DVR), Dichtebestimmung und Zugversuch. Das Ziel ist, die Leckagerate mit anderen Eigenschaften bzw. Methoden zu korrelieren, um so ein aussagekräftiges und leichter zu bestimmendes Lebensdauerkriterium für elastomere O-Ringe abzuleiten. Während der Alterung können in Abhängigkeit von Material sowie Alterungsdauer und –temperatur Inhomogenitäten aufgrund von diffusionsbegrenzter Oxidation auftreten, durch die sich unterschiedliche Eigenschaften an der Oberfläche und im Volumen der Dichtung ergeben, was zu falschen Lebensdauerabschätzungen führen kann. Mittels Mikrohärtemessung über den Querschnitt werden diese Effekte charakterisiert und bei der Extrapolation mittels Zeit-Temperatur-Verschiebung und Arrheniusgraph berücksichtigt. Bisher liegen Daten von bis zu einem Jahr bei vier verschiedenen Temperaturen (75 °C, 100 °C, 125 °C und 150 °C) gealterten Proben vor. Nach 100 Tagen bei 150 °C weisen HNBR und EPDM schon einen DVR von über 80 % auf, aber noch keinen signifikanten Anstieg der Leckagerate. Diese sinkt zunächst während der Alterung, da die Permeabilität aufgrund von Vernetzungsreaktionen sinkt. Bei HNBR ist dies aufgrund der dominanteren Vernetzungsreaktionen während der Alterung noch stärker ausgeprägt als bei EPDM. T2 - Technomer 2015 - 24. Fachtagung über Verarbeitung und Anwendung von Polymeren CY - Chemnitz, Germany DA - 12.11.2015 KW - Aging KW - Elastomer KW - Seal KW - Leakage KW - Compression PY - 2015 SN - 978-3-939382-12-6 SP - 43 CY - Chemnitz AN - OPUS4-35050 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Mike A1 - Zencker, Uwe A1 - Wolff, Dietmar A1 - Jaunich, Matthias A1 - Kömmling, Anja A1 - Völzke, Holger A1 - Schulze, Dietmar T1 - Numerical simulation of the behaviour of elastomer seals under consideration of time dependent effects N2 - Due to delays in the site-selection procedure to establish a deep geological repository for spent nuclear fuel and high level waste and in construction of the already licensed Konrad-repository for low and intermediate level waste without heat generation, extended periods of interim storage become more relevant in Germany. BAM is involved in most of the cask licensing procedures and especially responsible for the evaluation of cask-related long-term safety issues. The long-term performance of elastomer seals for lid Systems of transport and storage casks whether used as auxiliary seals in spent fuel caslcs or as primary seals for low and intermediate level waste packages is an important issue in this context (Jaunich, 2013; Jaunich, 2014; Kömmling, 2015). The polymeric structure of these seals causes a complex mechanical behaviour with time-dependent elasticity reduction and loss of elastic recovery. The paper presents first results of a comprehensive test Programme consisting of several static and dynamic mechanical short- and long-term tests which have been carried out at BAM on specimens made of representative types of elastomers, fluorocarbon rubber (FKM) and ethylene propylene diene rubber (EPDM). The investigation of the test results used to identify material models and their Parameters as well as the development of two finite element models for the numerical Simulation of tension and compression tests using the finite element code ABAQUS® are described. The calculation results are presented in comparison to the test results. The influence of important material and test parameters was investigated and discussed in sensitivity analyses. T2 - RAMTRANSPORT 2015 - International conference on the radioactive materials transport and storage CY - Oxford, UK DA - 19.05.2015 KW - Numerical analysis KW - Extended interim storage KW - Elastomer seals PY - 2015 SP - Session 4, Paper 28, 1 EP - 9 AN - OPUS4-33832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grelle, Tobias A1 - Wolff, Dietmar A1 - Jaunich, Matthias T1 - Temperature-dependent leak tightness of elastomer seals after partial and rapid release of compression N2 - A device has been designed, built and tested that allows the investigation of effects of dynamic loads on the leak tightness of elastomer seals at low temperatures. With the test setup, the compression of the tested seal can be reduced by a defined degree in a time period of less than 1 s. For the evaluation of the leak tightness, leakage rates can be determined. It was shown that the rapid partial release of an elastomer seal leads to its failure already at the beginning of the rubber–glass transition and, therefore, at significantly higher temperatures than the loss of leak tightness observed under static conditions. KW - Sealing material KW - Elastomer KW - Dynamic loading KW - Low temperature behaviour KW - Leakage rate PY - 2015 DO - https://doi.org/10.1016/j.polymertesting.2015.09.009 SN - 0142-9418 VL - 48 SP - 44 EP - 49 PB - Elsevier Ltd. CY - Amsterdam [u.a.] AN - OPUS4-34445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias A1 - Grelle, Tobias A1 - Wolff, Dietmar T1 - Influence of partial release on sealing performance of elastomer O-rings at low temperatures N2 - For many sealing applications rubbers are applied due to their special material properties and easy use. In many applications as e.g. in aviation, traffic or process technology the material can be exposed to low temperatures during operation. Therefore it is important to know the material behaviour at those low temperatures to determine the temperature range that allows a safe operation of the seal. As rubbers are 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 acitve waste containers, a comprehensive elastomer investigation program is run at BAM. This program comprises investigations of elastomer overall performance, durability, influence of gamma irradiation and low temperature behaviour. In this paper we focus on the behaviour of elastomer seals below ambient temperatures after a fast partial release. Despite the primarily static application conditions of many seals their behaviour after partial compression release is of interest with regard to potential decrease of leak-tightness. For this investigation a special setup was designed which allows the partial release of compressed seal systems at different temperatures accompanied by leakage rate measurements. The results for FKM seals are presented and discussed. T2 - Technomer 2015 - 24. Fachtagung über Verarbeitung und Anwendung von Polymeren CY - Chemnitz, Germany DA - 12.11.2015 KW - O-ring KW - Glass-rubber transition KW - Compression set KW - Partial release PY - 2015 SN - 978-3-939382-12-6 SP - P 3.7, 1 EP - 6 CY - Chemnitz AN - OPUS4-35130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Influence of gamma irradiation on low temperature properties of rubber seal materials N2 - In many fields the function of seal materials is required at low temperatures. Therefore the understanding of failure mechanisms at low temperatures is of high importance. In some applications elastomeric seals are used in environments with increased irradiation backgrounds, as e.g. in containers for radioactive waste. This paper reports on the influence of gamma irradiation on the low temperature properties of different fluorocarbon rubber (FKM) materials. The samples were irradiated with gamma doses of up to 600 kGy and the induced changes of material properties were tested by methods sensitive to the rubber-glass transition, like DSC and DMA. Additionally, compression set measurements were performed to give information about recovery behaviour at low temperatures. KW - Seal KW - O-ring KW - Low temperature KW - Gamma irradiation KW - Compression set KW - Dichtungen KW - O-Ringe KW - Tiefe Temperatur KW - Gamma-Bestrahlung KW - Druckverformungsrest PY - 2015 SN - 0948-3276 SN - 0022-9520 VL - 68 IS - 6 SP - 85 EP - 89 PB - Hüthig CY - Heidelberg AN - OPUS4-33552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Influence of partial release on sealing performance of elastomer O-Rings at low temperatures T2 - Technomer 2015 CY - Chemnitz DA - 2015-11-12 PY - 2015 AN - OPUS4-34935 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Ageing of elastomeric seals for storage containers N2 - At BAM Federal Institute for Materials Research and Testing in Germany, it is our responsibility to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes the investigation of elastomeric seals applied in the containers. Besides examining the low-temperature behavior of elastomeric seals, it is our goal to evaluate the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. Furthermore, we deem it necessary to exceed the requirements given in the ageing standard DIN 53508 and take into account diffusion-limited oxidation (DLO) effects and non-Arrhenius behavior when making lifetime predictions. Therefore, we started an ageing programme with selected rubbers (HNBR, FKM and EPDM) which are oven-aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) in order to extrapolate the data to service temperature using different models and check which one is appropriate. Samples are examined at different times up to 5 years. In order to be able to compare between compressed and relaxed rubber, they are aged in two conditions: the undeformed O-ring state as well as compressed between plates with a compression of 25 % corresponding to the actual compression during service. Additionally, we are ageing samples in flanges that allow leakage rate measurements which is the central performance criterion. Analysis methods include hardness as a quick indicator, compression set and compression stress relaxation as measures reflecting the actual properties of a compressed seal. Additionally, we are applying classical polymer analysis methods like dynamic mechanic analysis and thermogravimetric analysis which show changes in the polymeric structure due to chain scission and crosslinking. Furthermore, we are testing the leakage rate of the O-rings in order to correlate the changes in physical properties to the actual performance of the seal. First results of samples aged up to 100 days show a strong increase in hardness for HNBR, a moderate increase for EPDM and hardly a change for FKM. A similar result is seen in the compression set of samples aged 100 d at 100 °C in compression as HNBR has reached 60 %, EPDM 25 % and FKM 15 % compression set. However, after ageing at 150 °C, EPDM shows a worse performance with 95 % compression set compared to HNBR with only 80 %. This is probably due to DLO effects in HNBR that appear because of the fast ageing and low oxygen permeability in HNBR. This leads to a deficit of oxygen in the center of the sample which is thus protected from ageing and can retain elastic properties. The full paper shall discuss the changes in material properties observed to date and the impact on the performance of elastomeric seals. T2 - IRC 2015 - International rubber conference CY - Nürnberg, Germany DA - 29.06.2015 KW - Elastomer KW - Rubber KW - Aging KW - Lifetime KW - Seal KW - Cask KW - Compression PY - 2015 SP - 1 EP - 10 AN - OPUS4-34939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Influences on the low temperature sealability of elastomer O-rings T2 - International Rubber Conference 2015 CY - Nuremberg, Germany DA - 2015-06-29 PY - 2015 AN - OPUS4-33752 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -