TY - CONF A1 - Wolff, Dietmar A1 - Jaunich, Matthias A1 - Stark, Wolfgang T1 - Investigating the performance of rubber seals at low temperatures T2 - IHLRWM 2013 - 14th International high-level radioactive waste management conference (Proceedings) N2 - 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. T2 - 14th International high-level radioactive waste management conference CY - Albuquerque, New Mexico, USA DA - 28.04.2013 KW - Rubber seals KW - Elastomers KW - Compression set KW - Low temperature KW - Leakage rate PY - 2013 SN - 978-1-62748-644-6 SP - 1 EP - 7(Paper # 6888) PB - Omnipress AN - OPUS4-28530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - McHugh, J. T1 - Cure state detection for pre-cured carbon-fibre epoxy prepreg (CFC) using temperature-modulated differential scanning calorimetry (TMDSC) JF - Polymer Testing N2 - 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. KW - Prepreg KW - Carbon fibre KW - Glass transition KW - Degree of curing KW - DSC KW - TMDSC PY - 2013 DO - https://doi.org/10.1016/j.polymertesting.2013.07.007 SN - 0142-9418 VL - 32 IS - 7 SP - 1261 EP - 1272 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-29067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - McHugh, J. T1 - Carbon-fibre epoxy prepreg (CFC) curing in an autoclave analogue process controlled by dynamic mechanical analysis (DMA) JF - Polymer Testing N2 - 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. KW - Prepreg KW - CFC KW - Curing KW - DMA KW - DSC KW - Autoclave KW - Gelation KW - Vitrification KW - Glass transition PY - 2013 DO - https://doi.org/10.1016/j.polymertesting.2013.09.014 SN - 0142-9418 VL - 32 IS - 8 SP - 1487 EP - 1494 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-29479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 JF - Polymer testing 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 - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias A1 - Bohmeyer, W. A1 - Lange, K. T1 - Investigation of the crosslinking behaviour of ehtylene vinyl acetate (EVA) for solar cell encapsulation by rheology and ultrasound JF - Polymer testing N2 - 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. KW - Ethylene vinyl acetate KW - EVA KW - Crosslinking KW - Ultrasound KW - Rheology KW - Curemeter KW - DSC PY - 2012 DO - https://doi.org/10.1016/j.polymertesting.2012.07.004 SN - 0142-9418 VL - 31 IS - 7 SP - 904 EP - 908 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-26291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stark, Wolfgang A1 - Jaunich, Matthias T1 - Investigation of ethylene/vinyl acetate copolymer (EVA) by thermal analysis DSC and DMA JF - Polymer testing N2 - 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. KW - EVA KW - Thermal analysis KW - DSC KW - DMA KW - Glass transition KW - Crystal melting KW - Cross-linking PY - 2011 DO - https://doi.org/10.1016/j.polymertesting.2010.12.003 SN - 0142-9418 VL - 30 IS - 2 SP - 236 EP - 242 PB - Elsevier Ltd. CY - Amsterdam [u.a.] AN - OPUS4-23206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias A1 - Wolff, Dietmar A1 - Stark, Wolfgang A1 - Völzke, Holger T1 - Investigation of elastomer seal behavior for transport and storage packages T2 - PATRAM 2013 - 17th International symposium on the packaging and transportation of radioactive materials (Proceedings) N2 - 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. 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 behavior is of high importance. In this paper we focus on the behavior of elastomer seals at low temperatures with regard to poten-tial decrease of leak-tightness. In addition, changes in material properties due to aging effects over long periods of time and their influence on the seal performance is investigated. It is known that material properties of rubbers are strongly temperature dependent. At low tempera-tures this is caused by the rubber-glass transition (abbr. glass transition). During continuous cool-ing, the material changes from rubber-like entropy-elastic to stiff energy-elastic behavior, that al-lows 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. Aging of elastomer seals is important, as possible dynamic loads may have to be considered during the whole interim storage period (so far approved in Germany for up to 40 years) and for transporta-tion after storage. For the investigations, fluorocarbon (FKM) and ethylene-propylene-diene (EPDM) rubbers were selected as they are often used in radioactive waste containers. Some materials were purchased from a commercial seal producer and some materials were compounded and cured at BAM. The elastom-ers where studied by several thermo-analytical methods and compression set to characterize the material behavior at low temperatures. Additionally component tests were performed to determine the breakdown temperature of the sealing function of complete elastomer O-rings. T2 - PATRAM 2013 - 17th International symposium on the packaging and transportation of radioactive materials CY - San Francisco, CA, USA DA - 18.08.2013 PY - 2013 SP - Paper 227, 1 EP - 8 PB - Omnipress AN - OPUS4-30377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias A1 - Wolff, Dietmar A1 - Stark, Wolfgang T1 - Low temperature properties of rubber seals - results of component tests T2 - 10th Fall rubber colloquium (Proceedings) T2 - 10th Fall rubber colloquium CY - Hannover, Germany DA - 2012-11-07 PY - 2012 SN - 978-3-9814076-1-7 IS - khk2012_jaunich.pdf SP - 1 EP - 8 AN - OPUS4-26995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias A1 - Wolff, Dietmar A1 - Stark, Wolfgang T1 - Investigating low temperature properties of rubber seals T2 - WM2013 Conference (Proceedings) N2 - 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. T2 - WM2013 Conference CY - Phoenix, Arizona, USA DA - 24.02.2013 PY - 2013 SN - 978-0-9836186-2-1 SP - 1 EP - 12 CY - Phoenix, Arizona, USA AN - OPUS4-28853 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 - JF - Kautschuk, Gummi, Kunststoffe (KGK) 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 -