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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.
In Germany, the search for a final repository for highly radioactive material is currently based on the assumption that interim storage will take considerably longer than was anticipated. At that time, authorization procedures assumed that interim storage would be brief, until the containment systems could be placed in a final repository. For today's new approvals and extensions, the IAEA (International Atomic Energy Agency) regulations for the transport of radioactive material require an assessment of all components and component groups with regard to ageing. To assess the safety requirements not only over the previously envisaged periods but also over long durations, numerous individual parts and component groups must be examined and evaluated for ageing and interactions between materials. The metal seals of a double lid sealing system, for example, are critical components that must be studied with respect to ageing. In a containment system for radioactive material, metal seals must not only undergo classic ageing, but also withstand mechanical influences and radiation over extended periods. In addition to assessments by the applicants, BAM must also independently analyze and evaluate these ageing mechanisms as part of its sovereign mandate.
Another challenge in both new approvals and extensions is the assessment of transport regarding changes in the state of the art, which are not synchronously assessed in the regulations. In transporting radioactive material, a classic oil fire has been assumed in a hypothetical accident scenario from the development of the regulations to the present day. Due to the rapid development of propulsion technologies in recent years, such as battery or hydrogen-powered vehicles, investigations must be conducted in the revision process of the IAEA regulations to assess the impact of these new technologies on safety assessments. It is important for the member states of the IAEA to know whether new technologies are covered by the regulations or if changes are necessary to continue issuing international licenses. By focusing on batteries from the material to the cell to the module and the application, BAM contributes to the evaluation of batteries at every step of the chain. In addition to the safety of current and new battery technologies, BAM also endeavors to address issues of compositional trace and sustainable energy materials.
The investigation of the long-term performance of sealing systems employed in containers for radioactive waste and spent nuclear fuel is one research focus area for division 3.4 “Safety of Storage Containers” at the Bundesanstalt für Materialforschung und -prüfung. Metallic seals are in use in interim storage casks for used fuel and high active waste. Their change in performance over time is of high importance for maintaining safe enclosure. Therefore, investigations on these systems were started at BAM to get a general understanding of the relevant processes. Our investigations comprise investigations on different parameters which influence the seal performance and the main part is focussed on the time and temperature dependent behaviour.
In this contribution an update on the performed tests and their respective results will be given in respect to the overview presented in 2020.
The understanding of the long-term behaviour of the sealing systems and the performance evaluation during interim storage and subsequent transportation are our goals.
It is an essential requirement for all building products to ensure durability of their fire safety. Throughout the working life of products, intumescent coatings are aged by certain climatic factors. To predict a lifetime of several years, generally the behaviour of the intumescent coating is extrapolated based on accelerated artificial ageing. The established German and European procedures to assess the durability assume a working life of at least 10 years. For a longer period, additional evidence is required; yet the procedure and the specifications to justify this are not described. In addition to addressing this formal lack, from a scientific point of view it is necessary to investigate the degradation of intumescent coatings in detail and to propose a reliable test concept to assess durability for more than 10 years. This paper summarises the existing knowledge about the ageing of intumescent coatings. The results of various demanding weathering approaches are presented for two intumescent coatings tested in a joint research project. Moreover, formulations with a reduced amount of functionally relevant components were analysed to gain insight into the associated effects. Derived from these research results and knowledge, recommendations are proposed to assess the durability of intumescent coatings for more than 10 years based on a combination of verifications.
Acceptable limits for activity release from transport casks for high-level radioactive material specified in the IAEA regulations must be kept by the integrity of cask body and the cask sealing system. BAM as the German competent authority for mechanical, thermal and containment assessment of packages liable for approval verifies the activity release compliance with the regulatory limits. The specification of conservative package design leakage rates is one of the most important aspects in assessment.
Metal seals of the Helicoflex® Type are usually used to ensure the required package tightness for both, storage, and transport of the cask before and after storage. Due to the long-term use the seal behavior is influenced by temperature and time. The mechanical and thermal loadings associated with the routine, normal and accident conditions of transport specified in the regulations can have a significant effect on the leak tightness of the sealing system. Whereas the safety for application of new, non- aged Helicoflex® seals is verified sufficiently, there are still technical data gaps concerning the efficiency of aged Helicoflex® seals.
BAM performed experiments to learn more about the sealing efficiency of aged Helicoflex® seals with Aluminum and Silver outer jackets. The seals were compressed in test-flanges and for artificial ageing the complete flange systems were stored in an oven for several month at a high temperature. After this ageing procedure the flanges were opened completely, the seals were moved a little to vary the contact area, and the flanges were compressed again. During the compression and decompression tests after the aging, load-deformation characteristics of the seals, and leakage rates were measured.
With these tests a load situation was simulated, which can occur in the regulatory drop test of the cask: Under high impact loads the bolted lid can lift a little for a short moment, allowing a little movement of the seal, so that the contact area can change before compressing again.
Details about test conditions and first results will be presented in the poster.
Abstract Hydrogenated nitrile butadiene rubber (HNBR) elastomer was thermo-oxidatively aged at different temperatures up to 150 °C. Fourier transform infrared spectroscopy (FTIR), compression stress relaxation (CSR) and international rubber hardness degree (IRHD) microhardness were used to characterise the chemo-mechanical changes of HNBR O-rings during thermo-oxidative ageing. FTIR shows the development of carbonyl, methyl and ester groups but the nitrile content was not affected by ageing. The effect of sample geometry during CSR was investigated. CSR data were converted through integrated kinetic laws. The conversion has proven its sensibility to detect heterogeneous ageing. This was confirmed by the IRHD measure-ments across the section of O-rings. The influence of compression during ageing was assessed through IRHD measurements across the section of compressed and uncom-pressed aged O-rings. The DLO effect was more pronounced in compressed O-rings. By applying the model of Wise et al., theoretical IRHD and oxidation profiles were determined on the basis of IRHD experimental data of compressed O-rings. Good agreements between the experimental and the theoretical IRHD profiles in the core region were obtained. However, near the edge, the theoretical IRHD values were overestimated.
Deconvoluting the impact of early-life abuse conditions on the degradation of lithium-ion cells
(2023)
The successful repurposing of degraded lithium-ion (Li-ion) batteries in second-life applications is a vital step towards achieving a circular economy. While reusing aged Li-cells is a promising way of mitigating their overall environmental footprint, it is crucial to anticipate their future safety and performance characteristics . Unfortunately, predicting these properties is a cumbersome task, essentially caused by limited knowledge of the interference of different degradation modes in the cells’ first life.
To still enable estimating of these parameters from a current state, the present study systematically investigates the impacts of abusive conditions in an early phase of the cells’ life on their subsequent degradation behavior. For this purpose, individual Li-cells are initially stressed by different measures such as overcharging, deep-discharging, plating, and deliberate combinations of the aforementioned methods. Electrochemical performance indicators are monitored during subsequent cycling of the cells which provides insights into the interdependencies of different degradation modes induced by specific stress conditions. In this manner, it is clarified whether or not the total degradation can be determined by a convolution or a superposition of individual deterioration effects and, thus, be described as a multidimensional state function.
This knowledge will finally contribute to a better understanding of the performance and safety behavior of degraded Li-ion batteries which can help to successfully implement them into second-life applications.
Asphalt is one of the most common materials used in road construction. It is subject to both chemical and structural aging processes during use. At least to our knowledge, it is not currently known whether these aging processes also lead to a measurable change in the thermal properties of asphalt. If so, these changes could be exploited for non-destructive testing of the aging condition in situ. Photothermal analysis of a component surface involves looking at the time course of the surface temperature during and after pulse-like heating with an expanded laser beam. In the case of concrete surfaces, this method works well under laboratory conditions. It allowed the determination of the thermal effusivity. Now it should be investigated whether the photothermal signal allows conclusions to be made regarding the aging state of the asphalt. Within the scope of this paper, 2 asphalt specimens were investigated: a closed asphalt with 3% void content (SMA 11S) and an open-pore asphalt with 25% void content (PA 8). Both samples were artificially degraded according to a standardized procedure, leaving a portion of the surface unaffected. Subsections from both areas were then separated for photothermal testing. It was found, that the photothermal method is apparently not sensitive enough to detect aging on asphalt in general. However, it is noteworthy that both asphalt types heat up significantly faster than would be expected from the theory of heat conduction, which might be explained by the specific microstructure.
In this work we present results for three typical sealing materials (EPDM, HNBR, FKM) after up to 100 days ageing at high temperature under hydrogen. To allow for a better evaluation of the occurring changes the results are compared with effects of ageing in air on the material properties. Despite the common assumption that ageing under hydrogen atmosphere is expected to be less severe for the material in com-parison to air ageing, this is not seen for every material.
The storage of spent fuel and high level radioactive waste in Germany is performed in interim storage containers with double lid systems. The lids are bolted and equipped with metal seals (e.g. Helicoflex®) to ensure the safe enclosure of the inventory. The used metal seals have a layered structure consisting of three components as can be seen schematically in the cross-sectional view in Fig. 1.
In the center a helical spring is positioned that is surrounded by two C-shaped jackets and is mainly responsible for generation of the required restoring force. The inner jacket is made of stainless steel and homogenizes the restoring force of the helical spring. The outer jacket is made of silver or aluminium which both are soft metals in comparison to the contact partners (lid and container body). During bolting of the lid to the container body the seal is compressed. The generated restoring force of the helical spring causes a plastic deformation of the outer jacket and adapts to the surfaces of the lid and the container body. Hence, leakage paths are closed and the sealing function is generated.
Typical durations for existing interim storage licenses in Germany are 40 years, but it can be expected that they have to be extended to longer periods as a final repository will not be available before the end of the running licence periods. This extension of license periods requires a solid understanding of the long-term behaviour of the seals under storage conditions. To meet this challenge long-term investigations have been started at Bundesanstalt für Materialforschung und –prüfung (BAM) in 2009. These tests focus on seals assembled in test flanges which are stored at temperatures ranging from room temperature to 150 °C for accelerated ageing. The aged seals are tested repeatedly after certain ageing steps and the leakage rate as indicator for sealing performance, the remaining seal force, and the useable resilience upon decompression are determined.
In the poster an update on the performed investigations in respect to earlier publications (Grelle et al. 2019, Goral et al. 2023) will be given and the implications of the results for resilient long term safety will be presented. Additionally, a focus will be laid on the currently planned further investigations and the question “What is additionally needed for evaluation of an interim storage period extension in regard to the used metal seals?” will be addressed.