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 - 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 - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - A new method to evaluate the low temperature function of rubber sealing materials N2 - 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. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2010 DO - https://doi.org/10.1016/j.polymertesting.2010.07.006 SN - 0142-9418 VL - 29 IS - 7 SP - 815 EP - 823 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-21914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias A1 - Wolff, Dietmar ED - Van Breugel, K. ED - Koenders, E.A.B. T1 - Approach for the investigation of long-term behaviour of elastomeric seals for transport and storage packages N2 - Elastomers are widely used as main sealing materials for Containers for low and intermediate Ievel radioactive waste and as additional component to metal seals in spent fuel and high active waste Containers. According to appropriate guidelines and regulations safe enclosure of the radioactive Container contents has to be guaranteed for long storage periods as well as down to temperatures of -40 °C for transportation. Therefore the understanding of seal behaviour in general is of high importance and ageing of elastomeric seals has to be considered with regard to possible dynamic events taking possibly place during transport after storage. T2 - 1st Ageing of materials & structures 2014 conference CY - Delft, The Netherlands DA - 26.05.2014 KW - O-Ring KW - Seal KW - Ageing KW - Elastomer KW - Compression set PY - 2014 SN - 978-94-6186-313-3 SP - 87 EP - 93 AN - OPUS4-30820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jaunich, Matthias A1 - Probst, Ulrich A1 - Schulz, Sebastian A1 - Wolff, Dietmar A1 - Stark, Wolfgang ED - Berger, K.-F. ED - Kiefer, S. T1 - Elastomere - Untersuchung des Tieftemperaturverhaltens im Dichtungseinsatz N2 - 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. KW - Dichtung KW - Druckverformungsrest KW - Elastomer KW - Glasübergang PY - 2013 SN - 978-3-9811509-7-1 SP - 82 EP - 91 CY - Mannheim AN - OPUS4-29661 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 - JOUR A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Goral, Milan A1 - Wolff, Dietmar T1 - Insights for lifetime predictions of O-ring seals from five-year long-term aging tests N2 - O-rings made of HNBR, EPDM and FKM were aged in the compressed and uncompressed state at 150 °C, 125 °C, 100 °C, 75 °C, 60 °C and 23 °C for aging times of up to five years. Hardness was measured and increased with aging time and temperature for HNBR and EPDM, but it remained practically constant for FKM. Indenter modulus measurements were performed on the lateral O-ring surface (that was free of DLO effects) to assess an influence of the compression during aging, but none was detected. The equilibrium compression set (CS) exhibited faster and stronger degradation than hardness and was used for lifetime predictions using the time-temperature superposition (TTS) principle. With an end-of-lifetime criterion of 70 % CS, lifetimes of 4.5 years, 50 years and 526 years at 75 °C were estimated for HNBR, EPDM and FKM, respectively. The activation energies derived from an Arrhenius plot of the shift factors from the TTS were 85 kJ/mol, 99 kJ/mol and 78 kJ/mol for HNBR, EPDM and FKM, respectively, revealing that a higher activation energy does not necessarily mean that the material has a higher lifetime at lower temperatures. Furthermore, the measured lifetime of EPDM O-rings at 100 °C (5 years) was compared to that predicted on the basis of the lifetime at 150 °C as well as 125 °C using the corresponding shift factors. The error of the prediction was only ± 4 %. However, this precise prediction could only be achieved using the five-year long-term aging data. When using only data from aging times up to 0.5 years and 2 years, the lifetime of EPDM O-rings at 100 °C was underestimated by 31 % and 22 %, respectively. KW - HNBR KW - EPDM KW - FKM KW - DLO KW - Hardness KW - Compression set KW - Rubber KW - Elastomer KW - Degradation PY - 2020 DO - https://doi.org/10.1016/j.polymdegradstab.2020.109278 VL - 179 SP - 109278 PB - Elsevier Ltd. AN - OPUS4-51060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang T1 - Monitoring the vulcanization of rubber with ultrasound: Influence of material thickness and temperature N2 - 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. KW - Vulcanization KW - Cure process KW - Ultrasound KW - Curemeter KW - Elastomer KW - Natural rubber PY - 2009 DO - https://doi.org/10.1016/j.polymertesting.2009.08.006 SN - 0142-9418 VL - 28 IS - 8 SP - 901 EP - 906 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-19959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Subramani Bhagavatheswaran, E. A1 - Wießner, S. A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Einfluss der Alterung auf dichtungsrelevante Eigenschaften von FKM-, VMQ- und EPDM-Elastomeren N2 - Da Elastomere in vielfältigen Dichtungsanwendungen eingesetzt werden und dabei teilweise großen Einfluss auf die Funktionsfähigkeit und Sicherheit haben, ist der Einfluss der Alterung auf dichtungsrelevante Eigenschaften relevant. Eine strukturierte Untersuchung des Einflusses von verschiedenen Mischungsrezepturen auf die Bauteileigenschaften, das Alterungsverhalten und die Funktion wird vorgestellt. T2 - Technomer 2017 CY - Chemnitz, Germany DA - 09.11.2017 KW - Dichtung KW - Alterung KW - Struktur-Eigenschaftsbeziehung KW - Elastomer PY - 2017 SN - 978-3-939382-13-3 VL - 2017 SP - 41 EP - 41 AN - OPUS4-42844 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Hoster, B. T1 - Monitoring the vulcanization of elastomers: Comparison of curemeter and ultrasonic online control N2 - 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. KW - Cure process KW - Ultrasound KW - Curemeter KW - Elastomer KW - Vulcanization KW - Online control PY - 2009 DO - https://doi.org/10.1016/j.polymertesting.2008.11.005 SN - 0142-9418 VL - 28 IS - 1 SP - 84 EP - 88 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-18674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -