TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - Comparison of low temperature properties of different elastomer materials investigated by a new method for compression set measurement N2 - 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. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2012 U6 - https://doi.org/10.1016/j.polymertesting.2012.07.016 SN - 0142-9418 VL - 31 IS - 8 SP - 987 EP - 992 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-26538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Wolff, Dietmar A1 - Stark, Wolfgang T1 - Low temperature properties of rubber seals - Results of component tests - N2 - 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. KW - Seal KW - O-ring KW - Low temperature KW - Component test KW - Compression set KW - Dichtungen KW - O-Ringe KW - Tiefe Temperatur KW - Bauteilversuche KW - Druckverformungsrest PY - 2013 SN - 0948-3276 SN - 0022-9520 VL - 66 IS - 7-8 SP - 26 EP - 30 PB - Hüthig CY - Heidelberg AN - OPUS4-28894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Oxidative ageing of elastomers: Experiment and modelling N2 - During an extensive test programme at the Bundesanstalt für Materialforschung und prüfung, material property changes of EPDM O-rings were investigated at different ageing times and two ageing temperatures of 125∘C and 150∘C. To exclude possible diffusion-limited oxidation (DLO) effects that can distort the data, IRHD microhardness measurements were taken over the cross section of compressed O-rings. Continuous stress relaxation measurements were taken on samples free of DLO effects. The additional effect of physical processes to irreversible chemical ones during a long-term thermal exposure is quantified by the analysis of compression set measurements under various test conditions. By combining the different experimental methods, characteristic times relative to the degradation processes were determined. On the basis of experimental data, a microphysically motivated model that takes into account reversible and irreversible processes was developed. The parameter identification strategy of the material model is based on our experimental investigations on homogeneously aged elastomer O-rings. The simulated results are in good agreement with the experiments. KW - Compression stress relaxation KW - Compression set KW - IRHD microhardness KW - Modelling PY - 2022 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-545910 SN - 1432-0959 SP - 1 EP - 9 PB - Springer CY - Berlin AN - OPUS4-54591 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 U6 - 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 - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - Low temperature properties of rubber seals N2 - 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. N2 - Tiefentemperaturverhalten von Elastomerdichtungen 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 Übergangsbereiches eingesetzt aber die minimale Einsatztemperatur ist nicht exakt definiert. Daher ist es sinnvoll diese untere Temperatureinsatzgrenze in Abhängigkeit von den Materialeigenschaften zu bestimmen. Die Ergebnisse der DSC und der DMA werden mit den Ergebnissen des standardisierten Druckverformungsrestes nach ISO 815 und einer abgewandelten Messung mit der DMA kombiniert. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2011 SN - 0948-3276 SN - 0022-9520 IS - 03 SP - 52 EP - 55 PB - Hüthig CY - Heidelberg AN - OPUS4-23422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Revealing effects of chain scission during ageing of EPDM rubber using relaxation and recovery experiment N2 - Both chain scission and crosslinking reactions occur during ageing of EPDM rubber. However, with many conventional polymer analysis methods such as hardness and DMA, it is hardly possible to obtain information about the contribution of each reaction type to the measured data. For example, hardness and Tg both increase during ageing of EPDM, indicating crosslinking during ageing, but it is not clear whether this is partly counterbalanced by chain scission reactions which would lower hardness and Tg. An indication that chain scission reactions probably counteract the hardness or Tg increase by crosslinking is given by Compression Set (CS) measurements. CS exhibits a higher change than hardness or Tg, as CS increases additively through both chain scission and crosslinking reactions. In order to elucidate the share of chain scission reactions in the total degradation, a method testing relaxation and recovery behaviour using DMA equipment was applied. The method revealed the strong influence of chain scissions, leading to more pronounced relaxation and higher residual strain after compression. KW - Compression set KW - DMA KW - Nnetwork KW - Crosslinking PY - 2016 U6 - https://doi.org/10.1016/j.polymertesting.2016.10.026 SN - 0142-9418 SN - 1873-2348 IS - 56 SP - 261 EP - 268 PB - Elsevier Ltd. AN - OPUS4-38012 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 U6 - 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 - 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 - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Scission, cross-linking, and physical relaxation during thermal degradation of elastomers N2 - Elastomers are susceptible to chemical ageing, i.e., scission and cross-linking, at high temperatures. This thermally driven ageing process affects their mechanical properties and leads to limited operating time. Continuous and intermittent stress Relaxation measurements were conducted on ethylene propylene diene rubber (EPDM) and hydrogenated nitrile butadiene rubber (HNBR) samples for different ageing times and an ageing temperature of 125 °C. The contributions of chain scission and cross-linking were analysed for both materials at different ageing states, elucidating the respective ageing mechanisms. Furthermore, compression set experiments were performed under various test conditions. Adopting the two-network model, compression set values were calculated and compared to the measured data. The additional effect of physical processes to scission and cross-linking during a long-term thermal exposure is quantified through the compression set analysis. The characteristic times relative to the degradation processes are also determined. KW - Ageing KW - Scission KW - Cross-linking KW - Compression set KW - Physical relaxation PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-486091 SN - 2073-4360 VL - 11 IS - 8 SP - 1280, 1 EP - 12 PB - MDPI AN - OPUS4-48609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Understanding the recovery behaviour and the degradative processes of EPDM during ageing N2 - Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement. KW - Compression set KW - Ageing KW - Recovery KW - Degradative processes KW - Leakage rate PY - 2023 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-573699 SN - 0142-9418 VL - 121 SP - 107987 PB - Elsevier Ltd. AN - OPUS4-57369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - von der Ehe, Kerstin A1 - Wolff, Dietmar A1 - Völzke, Holger A1 - Stark, Wolfgang T1 - Understanding low temperature properties of elastomer seals N2 - 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. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2011 U6 - https://doi.org/10.1179/1746510911Y.0000000004 SN - 1746-5095 SN - 1746-5109 SN - 0957-476X VL - 22 IS - 2 SP - 83 EP - 88 PB - Ramtrans Publ. CY - Ashford AN - OPUS4-24015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -