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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.
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.
BAM-GGR 023 was published in June 2022
BAM-GGR 023 gives guidance to applicants regarding ageing management for competent authority approved package designs
Ageing management with evaluation of ageing mechanisms according to para 613A of IAEA SSR-6 (Rev. 1) and their effects are part of the general management system.
Essential items are: AMS (systemic-related), AMP (package design-related) and AMD (package-related)
There are different requirements for organization and extent of ageing management depending on type of use
There are also different requirements for ageing evaluation depending on type of use for packaging/package, classification of components and their accessibility and replaceability
Overview of ongoing research and future prospects on polyethylene neutron shielding materials at BAM
(2023)
The extension of the interim storage period of radioactive waste before disposal will cause additional challenges for the nuclear waste management in Germany, so that an extensive knowledge of the long-term performance of casks, including their components and inventories, will be required for future extended storage licenses.
Ultra-high and high molecular weight polyethylenes ((U)HMW-PE) are used for neutron shielding purposes in casks for storage and transport of spent fuel and high-level waste due to their extremely high hydrogen content. During their service life of several decades as cask components, the PE materials are exposed to neutron and gamma radiation from the radioactive inventory of the casks, mechanical assembling stresses and temperature. All these combined effects affect the material properties of such components which in turn may be crucial for some possible accident scenarios.
At the Bundesanstalt für Materialforschung und -prüfung (BAM), the effects of high temperature exposure in combination with subsequent or previous irradiation were investigated with a comprehensive aging program including thermal aging at 125 °C for different aging periods up to 5 years and irradiation with doses ranging from 50 to 600 kGy.
This contribution provides an overview of the ongoing research related to the structural changes of (U)HMW-PE induced by gamma irradiation and high temperature exposure and focuses on current research perspectives at BAM with regard to the prediction of the dynamic behavior of the material during extended interim storage in case of an accident scenario. First results of the coupled effect of temperature, radiation and mechanical loading will be presented. The effect of microstructural changes induced by gamma irradiation and high temperature on the mechanical behavior of (U)HMW-PE will be assessed.
With our experiments we want to simulate a load situation which can result from a cask vertical drop test. The lid can lift a little for a very short moment and that can perhaps result in a little movement of the seal, a little rotation or a little lateral movement, so that the contact section can change. The aim of the project is to learn more about the sealing efficiency after the seal is compressed again. What we know from former component tests with non-aged seals is, that the leakage rate measured after one or more decompression /compression cycles with seal movement becomes significant higher. And this result is considered for specification of design leakage rates for release calculation in safety cases.
In the recent years we all have learned more about the significant influence of temperature and time on seal behavior and so the plan was to do similar experiments with aged seals, just to get an idea about seal behavior and achievable leakage rates.
What we did in detail is:
We compressed Helicoflex-seals of both design types, with Aluminum and Silver outer jackets, in testflanges and aged them in an oven at a temperature of 125°C for 3 months to produce seal properties comparable with properties after several years use at more typical operating temperatures between 90 and 100°C.
After this ageing procedure we opened the flanges completely, moved the seal a little to vary the contact area and compressed the flanges again. What we measured during all compression and decompression cycles was the load, the deformation and -as long as possible- the leakage rates.
With integration of the new para 613A into SSR-6 [1] the consideration of ageing mechanisms is now obligatory for the design of packages and their approval. In addition, para 809(f) of SSR-6 [1] requires consideration of the effects of storage on ageing mechanisms, safety analyses and operation and maintenance instructions.
German competent authorities Bundesanstalt für Materialforschung und -prüfung (BAM) and Bundesamt für die Sicherheit der nuklearen Entsorgung (BASE) are considering the aspect of ageing in approval procedures. Ageing assessment is mainly focused on dual purpose casks (DPC) package designs which are long-term stored in interim storage facilities.
With integration of the new para 613A into SSR-6 [1] the consideration of ageing mechanisms is now obligatory for the design of packages and their approval. In addition, para 809(f) of SSR-6 [1] requires consideration of the effects of storage on ageing mechanisms, safety analyses and operation and maintenance instructions.
German competent authorities Bundesanstalt für Materialforschung und -prüfung (BAM) and Bundesamt für die Sicherheit der nuklearen Entsorgung (BASE) are considering the aspect of ageing in approval procedures. Ageing assessment is mainly focused on dual purpose casks (DPC) package designs which are long-term stored in interim storage facilities. For these package designs, the evaluation of ageing management is now mandatory for the maintenance of the package design approvals with a validity period of 5 years and beyond. The ageing management includes amongst others a gap analysis, the assessment of ageing effects and operational experiences during operation and interim storage.
BAM works on the compilation of a guideline for implementation of paras 613A, 809(f) and 809(k) for packages requiring competent authority approval at the application procedure in Germany. The paper describes essential items of ageing mechanisms and will give a foresight to the ageing management evaluation by BAM.
Based on the preliminary presentations in this task force it is repeated how a basic population scatters and its degradation influences properties statistically. There is a remainder on the issue of accepting borderline populations due to the minimum burst ratio requirement.
Then it is explained in detail how the analysis of minimum requirements by a Monte-Carlo-simulation works. The result with respect to the further reduced minimum burst ratio of 2.0 is summarised and means a two-step approach of two scatter levels requiring two different minimum burst ratios.
The methods for evaluating batch tests are analysed. A proposal for integration a statistical analysis is described in detail.
Finally, the positive effect of proof testing is shown and its dependence from the real ageing is shown.
This ends in the recommendation to have a stronger and quantitative look on real ageing and to follow the 2 proposed sets of criteria for a safe usage of hydrogen storage systems.
Elastomer seals are used in many industrial applications due to their excellent mechanical properties at a wide range of temperatures. Their high versatility and recovery potential under several load conditions make them well suitable for the application in containers designed for transport, storage and/or disposal of radioactive materials. In containers for low and intermediate level radioactive waste, elastomer seals are used as barrier seals, and as auxiliary seals in storage and transportation casks (dual purpose casks) for heat generating radioactive waste, such as spent fuel and high-level waste. While a seal exchange at defined intervals is typical in many conventional applications, it is impossible or at least hard to perform when principles of minimization of radiation exposure have to be considered and prohibit an unnecessary cask handling. An extensive knowledge of the change of the elastomer’s properties during aging and the availability of reliable end-of-lifetime criteria to guarantee the permanent safe enclosure of the radioactive material is mandatory. As BAM is involved in most of the national cask licensing procedures and in the evaluation of cask-related long-term safety issues, great efforts have been already made and are still planned to scientifically support this task.
Compression stress relaxation and compression set were identified as key indicators of elastomer long-term performance and quantitatively investigated in comprehensive test programs. Among other representative types of elastomers, specimens made from ethylene propylene diene rubber (EPDM) were tested before, during and after aging to capture the most important of their complex mechanical properties.
In the presented study, exemplary results were used to simulate the compression stress relaxation and the compression set of elastomer O-rings during aging. Regarding the influence of temperature, the time temperature superposition principle is applied in the relaxation analysis of elastomer O-rings. The proposed model is implemented in the commercial finite element software ABAQUS/Standard® [1] with a sequential temperature displacement coupling. Numerical results match the experimental compression stress relaxation measurements well. The prediction of compression set values after long-term aging shows a relatively good agreement with the experimental results. Nevertheless, all input parameters derived from the specimen tests, additional assumptions concerning boundary conditions and modeling strategy are discussed with regard to the identified slight discrepancies.
The possibility to extend the finite element model to represent the O-ring seal’s ability to recover after a (fast) partial release is taken into account
In Germany, spent nuclear fuel and vitrified high active waste is stored in dual purpose casks (DPC) at interim storage facilities. In order to ensure the transportability of the DPC to a final repository in future, the maintenance of the package design approval is realized. Therefore, the assessment of possible ageing effects during interim storage is necessary to ensure an evaluation of the transportability. The lecture presents BAM's current ageing evaluation concept in the field of trasnport law.
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 (BAM). Our investigations comprise investigations on metallic and elastomeric seals and covers experimental investigations to get a database on the component/material behaviour, work on analytical descriptions and numerical analysis. Our aim is to understand the long-term behaviour of the sealing systems for evaluation of their performance during possible extended interim storage and subsequent transportation.
Packages for the transport and storage of radioactive materials are often sealed with elastomer or metal seals. These seals are basic components to meet the leak tightness criteria for these kind of packages. An overview over ongoing research and development concerning metal and elastomer seals is given in the presentation. Introductions in the fundamental functionality of elastomer and metal seals are presented. Ageing processes are shown for both components regarding to different ageing effects.
Elastomer seals are widely used as barrier seals in containers for low and intermediate level radioactive waste. In addition, they are also used in waste fuel storage and transportation casks as auxiliary seals. Depending on the area of use, the rubber materials have to demonstrate proper sealing performance with respect to mechanical, thermal and environmental conditions as well as irradiation during the entire operation period. A fundamental understanding of the structure property relationship and their changes during aging can help to evaluate the long-term sealing performance.
In the present study, specific materials are investigated to study the structure-property and seal performance-correlation. Fluoro-elastomer (FKM), silicone rubber (VMQ) and ethylene propylene diene rubber (EPDM) were chosen as base rubbers. Comparable mechanical properties for these seals, especially in terms of a comparable compression behavior were achieved by careful control of base rubber formulation, i.e., by opting for the right filler and its concentration, amount of crosslinking chemicals, and with the assistance of process oils. Moreover, with the same rubber, similar mechanical properties were achieved by varying the filler concentration and crosslinking degree, which shall enable to correlate the particular influence on the structure property dependency of the seals in detail. The materials are investigated under pristine and aged conditions to evaluate the influence of aging, e.g. on the stress relaxation or recovery behavior. These values appear to be suitable parameters to judge the expected sealing performance.
Due to the electrically conducting nature of some fillers used to reinforce rubbers (such as carbon blacks, carbon nanotubes (CNTs), Graphene, etc.) it is possible to obtain current information about mechanical and visco-elastic properties by monitoring the electrical conductivity or resistivity. A simple relation that relates electrical resistance with mechanical stress was derived and the stress values were theoretically predicted from the electrical resistance values, which showed good correlation with experimental results.
Elastomer seals are widely used as barrier seals in containers for low and intermediate level radioactive waste. In addition, they are also used in waste fuel storage and transportation as auxiliary seals. Depending on the area of use, the rubber materials have to demonstrate proper sealing performance with regard to mechanical, thermal and environmental conditions as well as irradiation during the entire operation period. A fundamental understanding of the structure property relationship can help to understand the performance of rubber seals in aged conditions. The present study focuses on the investigation of specific materials to study the structure-property and seal performance-correlation. Fluoro-elastomer (FKM), silicone rubber (VMQ) and ethylene propylene diene rubber (EPDM) were chosen as the prime candidates. Mechanical properties for these seals were achieved by careful control of base rubber formulation, i.e., by opting for the right filler and its concentration, amount of crosslinking chemicals, and with the assistance of process oils. Moreover, with the same rubber, similar mechanical properties were achieved by varying the filler concentration and crosslinking degree, which enables us to understand the structure property dependency of the seals in detail. The materials are investigated in the pristine and under aged conditions to evaluate the influence of ageing on e.g. the stress relaxation or recovery behavior. These values appear to be suitable parameters to judge the expected seal performance. Due to the electrically conducting nature of fillers used to reinforce rubbers (such as carbon blacks, carbon nanotubes (CNTs), Graphene, etc.) it is possible to obtain current information about mechanical and visco-elastic properties by monitoring the electrical conductivity or resistivity. A simple relation that bridges electrical resistance and the mechanical stress was derived and the stress values were theoretically predicted from the electrical resistance values, which showed good correlation with experimental results.
Characterisation of degradation and determination of end-of-lifetime criterion for O-ring seals
(2017)
The ageing of polymers, including elastomers, is an undesirable but inevitable process leading to a limited lifetime of rubber products such as seals. Independent of the application, as e.g. automotive, piping or container applications, a long lifetime or at least a timely exchange of a seal before occurence of critical failure is desired.
In order to investigate the degradation of material properties and to determine the lifetime of elastomers used as seals, an ageing programme was started with hydrogenated acrylonitrile butadiene rubber (HNBR), ethylene propylene diene rubber (EPDM) and fluorocarbon rubber (FKM) [1-3]. Both O-ring seals (uncompressed and compressed by 25 %) with a cord diameter of 10 mm as well as sheets with a thickness of 2 mm were aged at 75 °C, 100 °C, 125 °C and 150 °C for up to two years. The changes of material properties during ageing were characterised for each material using the sheets by means of e.g. dynamic-mechanical analysis and tensile tests, while sealing properties such as compression stress relaxation (CSR), compression set (CS) and leakage rate were determined on O-rings. The experimental results indicate that while material properties, CSR and CS show considerable degradation effects, the static leakage rate stays constant or even decreases before failure occurs quite suddenly at advanced degradation levels. This reveals that static leakage rate has only limited sensitivity for the degradation of the seal material.
Our approach to determine a suitable end of lifetime criterion, which involves a partial decompression of the seal during the leakage test, is presented and discussed.
Elastomer seals are widely used as barrier seals in containers for low and intermediate level radioactive waste and in some countries for spent fuel transportation casks. Depending on the area of use, the rubber materials have to demonstrate proper sealing performance with regard to mechanical, thermal and environmental conditions as well as irradiation during the entire operation period.
In Germany the low and intermediate level radioactive waste is planned to be disposed in the Konrad repository in standardized containers. Many of these containers use an elastomer seal between lid and container body. Depending on the radiactive inventory and a possible containment of the waste in inner barrels and/or concrete structures, such containers may require a specific leak tightness. In such cases, specified leakage rates are shall not be exceeded by the the seals to keep potential activity releases from the inventories well below defined limits.
Generally, all waste containers have to fulfill the waste acceptance criteria for the Konrad repository as defined by the reports BfS SE-IB-29/08 and SE-IB-30/08. From these criteria several requirements for seal performance are derived. The seals have to:
- ensure full functionality until final container disposal,
- maintain its function in case of a thermal or mechanical accident,
- ensure encapsulation also at -20 °C.
This combination of requirements is challenging especially as a seal exchange, which is typical for many other applications, is hardly possible and thus a sound understanding of how to perform safety evaluation of containers is required. Therefore BAM has initiated investigations on elastomer seal behaviour. This work focuses on low temperature behaviour and sealing performance concerning static conditions as well as partial loss of compression and ageing of elastomer seals. Concerning ageing, property changes caused by long-term thermooxidative conditions as well as gamma irradiation are investigated.
This contribution presents an overview and explanation of the aims of the ongoing research and gives an update of the most relevant results.
BAM is the federal institute for materials research and testing in Germany. One of our tasks is to evaluate the safety of casks designed for transport and/or storage of radioactive waste. As elastomeric seals are used in the containers as safety-relevant parts, it is our goal to be able to evaluate the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. For this reason, an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) was started. Ageing was performed at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to 2 years. For assessing properties related to the sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates. For comparison, uncompressed O-rings were aged as well. The aged materials were characterized with conventional polymer analysis methods such as hardness and tensile tests, but also with more seal-specific methods such as compression stress relaxation (CSR, reflecting the loss of sealing force of a compressed seal over time), and compression set (CS, representing the recovery behaviour of a seal after release from compression). CS is chosen as the property for lifetime prediction as it is both sensitive to degradation and related to the seal performance. CS data is extrapolated to 60 °C, which yields lifetimes of approximately 5 years for HNBR and 64 years for EPDM for a criterion of 85 % CS respectively, and approx. 40 years for FKM for a criterion of 65 % CS (the highest value measured so far).
BAM is the federal institute for materials research and testing in Germany. One of our tasks is to evaluate the safety of casks designed for transport and/or storage of radioactive waste. As elastomeric seals are used in the containers as safety-relevant parts, it is our goal to be able to evaluate the service lifetime of the seals with regard to the requirements for long-term safety (40 years and more) of the containers. For this reason, an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) was started. Ageing was performed at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for up to 2 years. For assessing properties related to the sealability, O-rings were aged in compression by 25 % (corresponding to the compression during service) between plates. For comparison, uncompressed O-rings were aged as well. The aged materials were characterized with conventional polymer analysis methods such as hardness and tensile tests, but also with more seal-specific methods such as compression stress relaxation (CSR, reflecting the loss of sealing force of a compressed seal over time), and compression set (CS, representing the recovery behaviour of a seal after release from compression). CS is chosen as the property for lifetime prediction as it is both sensitive to degradation and related to the seal performance. CS data is extrapolated to 60 °C, which yields lifetimes of approximately 5 years for HNBR and 64 years for EPDM for a criterion of 85 % CS respectively, and approx. 40 years for FKM for a criterion of 65 % CS (the highest value measured so far).
The ageing of polymers, including elastomers, is an undesirable but inevitable process leading to a limited lifetime of rubber products such as seals. In order to investigate the degradation of material properties of elastomers used as seals, an ageing programme was started with hydrogenated acrylonitrile butadiene rubber (HNBR), ethylene propylene diene rubber (EPDM) and fluorocarbon rubber (FKM) [1-3]. Sheets of 2 mm thickness were aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) for time periods of 1 day up to 1 year. The aged samples were examined using standard analytical methods such as hardness, dynamic-mechanical analysis (DMA), thermogravimetric analysis (TGA), mass loss, density and tensile tests. Additionally, DMA equipment was used to investigate relaxation and recovery behaviour which is more sensitive to degradation effects and can help to correctly interpret data from hardness and DMA measurements. The results show e.g. an increase in hardness and glass transition temperature for HNBR and, less pronounced, for EPDM. This confirms ageing mechanisms described in the literature, e.g. dominant crosslinking reactions in HNBR and both chain scissions and crosslinking for EPDM. FKM, which is very heat resistant, exhibits only minor degradation. Where possible, shift factors for time-temperature data sets were determined. The values obtained from different methods are compared and discussed.
The Bundesanstalt für Materialforschung und –prüfung (BAM) and Sandia National Laboratories (SNL) entered into a Memorandum of Understanding (MOU) in September 2012 to foster technical collaborations in the areas associated with the backend of the commercial nuclear fuel cycle. Specifically, the focus is on packaging, transportation, and storage of commercial spent nuclear fuel. The institutes meet about twice each year, alternating between institutes. This provides the opportunity for staff members from the host organization more exposure to technical issues that are of concern internationally and to collaborate with technical experts working on similar problems.
Since 2012, the focus of the meetings has been on technical issues associated with extended dry storage and subsequent transportation of commercial spent fuel. Topics range from hydride effects on cladding integrity, spent fuel response during Normal Conditions of Transport (NCT), finite element analyses of fuel and cask response to accident conditions, bolt and seal behavior over extended periods of time, and corrosion associated with bolts, metallic seals, and stainless steel canisters.
This MOU has provided an effective leverage for technical collaboration. For example, SNL is funding (through DOE), Savannah River National Laboratories (SRNL) to look at bolt and seal degradation issues. SRNL has an MOU with BAM to collaborate on bolt and seal degradation during extended storage. Likewise, Sandia and BAM are collaborating with the EC Joint Research Center on an International Nuclear Energy Research Initiative (I-NERI) to investigate spent fuel behavior when subjected to mechanical loadings. This important work will provide insight into failure mechanisms, as well as spent fuel release fractions, given a breach of the cladding wall.
This presentation provides an overview of high ranked technical issues associated with extended storage and subsequent transportation, as well as the work underway at BAM and SNL that are addressing these issues.
As a Federal institute for materials research and testing it is part of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes the investigation of elastomeric seals and polymeric neutron shielding materials used in the containers.
In this contribution we would like to present our research focused on the long term performance and associated changes of material properties of elastomeric seals (e.g. EPDM, FKM) and neutron shielding materials ((Ultra) High Molecular Weight Polyethylene) employed in storage casks. Our approach comprises accelerated ageing investigations at elevated temperatures and to some extent investigations of irradiated materials.
As the requirements for the extended use of cables in nuclear power plants and for the long term use of cask components are to a certain extent similar, our work might be of interest for the workshop on “Cables ageing in nuclear power plants; R&D current status and forecast”.