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For many sealing applications rubber O-rings are applied due to their special properties and easy use. In many applications as e.g. in aviation, traffic or process technology the material can be exposed to a variety of conditions during operation as e.g. low temperatures, elevated temperatures and different media. Therefore, it is important to know the material behaviour and the seal performance under those conditions. Additionally ageing of seals is an important factor which has an influence on the long term reliability.
In this contribution we would like to discuss different aspects affecting the seal performance, lifetime estimation and address open questions which should be addressed to come to a deeper understanding of these seals commonly understood as typical machine elements.
Results of running investigations at the Bundesanstalt für Materialforschung und -prüfung (BAM), Division 3.4 “Safety of Storage Containers” are presented and discussed.
The excellent mechanical properties of elastomer seals at a wide range of temperatures as well as their high versatility and recovery potential under several load conditions make these materials well suitable for the application in containers designed for transport and disposal of negligible heat generating radioactive 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 which prohibit an avoidable cask handling. An extensive knowledge of the change of the elastomer properties during aging and the availability of reliable end-of-lifetime criteria to guarantee the safe enclosure of the radioactive material for the required time are 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 already been made and are still ongoing to scientifically support this task.
Among other representative types of elastomers, specimen made from ethylene propylene diene rubber (EPDM) were tested before, during and after aging to capture the with respect to application most important of their complex mechanical properties.
Exemplary results of these investigations were used to calibrate material models implemented in the commercial finite element software ABAQUS/Standard®. The finite element model already presented in previous works uses a sequential temperature displacement coupling. The calculated compression stress relaxation (CSR) and compression set (CS) values do satisfactorily match the experimental results.
In many investigations performed at BAM both values (CSR and CS) were identified as key indicators of elastomer’s long-term performance.
However, the possibility to correlate these equivalent indicators with performance values such as tightness and leakage rate, measurable in the mounted state, is an important goal of our future work. In the presented study the ABAQUS® feature of “pressure penetration” is introduced in the suggested finite element model for this purpose. It provides the possibility to simulate the penetration of a gas into a possible gap between flange and O-ring causing an opening of a leakage path. Three dimensional and axis-symmetric finite element models were generated to represent flat and grooved flanges of different dimensions.
The sensitivity of the feature to several input parameters is investigated and the observed behavior of the O-ring is correlated with the results of performed leakage tests.
EPDM, HNBR and FKM materials were exposed at 150 ◦C to air under atmospheric pressure and to hydrogen at 50 bar for different ageing times. All measurements after hydrogen exposure were conducted on samples in degassed condition to assess irreversible effects resulting from that exposure and to compare them to those after ageing in air. Density, hardness, tensile properties, compression set, and hydrogen permeability of all samples were analysed. In both ageing environments, HNBR exhibited the most significant changes of material properties.
However, for both EPDM and HNBR, considerably less severe ageing effects were observed under hydrogen in comparison to ageing in air. On the other hand, FKM showed about the same low level of deterioration in both ageing environments but exhibited poor resistance against damage due to rapid gas decompression in hydrogen environment that can lead to seal failure. The obtained results may serve as a guidance toward a better understanding for design and utilisation of elastomeric materials in future hydrogen infrastructure components.
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.
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.
Determining a suitable and reliable end-of-lifetime criterion for O-ring seals is an important issue for long-term seal applications. Therefore, seal failure of ethylene propylene diene rubber (EPDM) and hydrogenated nitrile butadiene rubber (HNBR) O-rings aged in the compressed state at 125 °C and at 150 °C for up to 1.5 years was analyzed and investigated under static conditions, using both non-lubricated and lubricated seals. Changes of the material properties were analyzed with dynamic-mechanical analysis and permeability experiments. Indenter modulus measurements were used to investigate DLO effects. It became clear that O-rings can remain leak-tight under static conditions even when material properties have already degraded considerably, especially when adhesion effects are encountered. As a feasible and reliable end-of-lifetime criterion for O-ring seals under static conditions should include a safety margin for slight dimensional changes, a modified leakage test involving a small and rapid partial decompression of the seal was introduced that enabled determining a more realistic but still conservative end-of-lifetime criterion for an EPDM seal.
Elastomer seals are mounted as barrier seals in lid systems of containers designed for transport and disposal of negligible heat generating radioactive waste and as auxiliary seals in spent fuel storage and transportation casks (dual purpose casks (DPC)). When the behavior of mounted seals under normal and hypothetical accident conditions of disposal and transport is to be simulated, a comprehensive knowledge of their complex mechanical properties at every state of aging is necessary. In previous works, BAM’s efforts in experimental investigations on specimen artificially aged at different temperatures and times and the implementation of the found results in finite element material models were presented. Additionally, our approaches to reproduce the aging process itself and to extrapolate the results of artificially accelerated aging to longer times were presented. Numerical simulations have shown that the behavior of the seal during mounting and one-sided pressurizing and the resulting performance values such as leakage rate strongly depend on the coefficient of friction (COF) between flange and seal. The friction coefficient, in turn, depends on the aging state of the elastomer material as several publications suggest (see below).
Dynamic COF between an exemplary ethylene propylene diene rubber (EPDM) material and a stainless steel ball were determined by using a self-designed linear oscillation tribometer. Unaged and artificially aged EPDM specimen stored for 30 days and 100 days at a temperature of 150 °C were tested. A stainless steel ball (d=10 mm) is brought in contact with the specimen’s surface und loaded by normal forces of 2.5 N, 5 N, 10 N and 20 N. During a reciprocating movement of the EPDM sheet, the horizontal force/friction force is continuously measured, and the COF can be derived.
It is well known that friction is a complex phenomenon especially in soft materials. It cannot be excluded that the measured friction force is influenced by additional force components, resulting from the ball’s grooving through the elastomer’s surface. This force depends on the penetration depth of the ball and on the resistance of the elastomer in its different states of aging. The latter results from microstructural changes i.e., chain scission and additional crosslinking that occur during aging which in turn influence the softening or hardening of the material.
A finite element (FE) ABAQUS® model was developed to reproduce the measurement process. It should help to better understand the physical mechanisms and to quantify the percentage of measured forces resulting from real friction on the one hand and forces resulting from unintended side effects that could falsify the result on the other hand. The behavior of the elastomer in its different states of aging is reproduced by a FE material model already presented in previous works of BAM.
Elastomeric seals are essential components in the infrastructure which prevent leakage of gas and proper function of technical devices and are therefore highly safety relevant. For proper function a remaining resilience and tolerance to pressure changes is required.
The ageing of 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 occurrence of critical failure is desired.
Hydrogen is a key element for the energy turnaround and therefore the compatibility of seals with hydrogen is essential. In addition to the effect of hydrogen uptake and release, which might also cause destructive effects such as rapid gas decompression, ageing at high temperature under hydrogen atmosphere is of interest too. Most of the existing work is addressing the performance of new materials and comprises only very limited investigations concerning long-term use and the behaviour of aged materials in contact with hydrogen. As ageing can lead to substantial changes of material properties, it must be evaluated whether these changes are beneficial or deteriorating for the component function.
In this work we present and compare results of the characterisation of three sealing materials (EPDM, HNBR, FKM) after ageing at high temperature under hydrogen and air. Despite the common assumption that ageing under hydrogen atmosphere should be less severe for the material in comparison to air ageing, this is not the case for every material.
Component and material investigations on metal seals for high level radioactive waste containers
(2018)
Long-term investigations performed at BAM look to extend the state of knowledge on safety-related components of interim storage containers. Metal seals act as the primary sealing barrier in the bolted double lid closure system of the containers. The behaviour of metal seals has been investigated for ageing times up to 8.5 years and for various temperatures. The main cause for reduction in useable resilience overtime was due to creep deformation of the outer jacket of the seal.
Component and material investigations on metal seals for high level radioactive waste containers
(2018)
In Germany casks for interim storage of spent nuclear fuel and high level radioactive waste are equipped with Helicoflex® metal seals as main sealing barrier of the double lid system. The long-term behaviour of those seals is investigated at Bundesanstalt für Materialforschung und –prüfung (BAM) in order to evaluate the safety function of the containment at different temperatures over storage periods of 40 years or more in case extended interim storage becomes necessary.
Long-term investigations have been done for ageing times of up to 8.5 years at temperatures ranging from room temperature to 150 °C. It was found that the seal force and useable resilience decrease over time, which is mainly caused by creep deformation of the aluminium (or silver) outer jacket of the seals. This effect becomes stronger with increasing temperature.
The ageing processes of the seal material and the overall seal behaviour is under investigation in order to derive analytical descriptions for the long-term seal performance. Thus, standardized tests on the basic seal materials, with focus on aluminium, and additional investigations on the seals as a component are conducted. The current investigations include compression and tension creep measurements as well as tensile testing. Furthermore, ageing of seal segments provides information on the development of the contact area width, jacket thickness and microstructural changes in dependence of time and temperature. The obtained data are used for the development of material models and an analytical approach to describe and predict the time and temperature dependent sealing behaviour in the long-term.
A Memorandum of Understanding (MOU) between Argonne National Laboratory (Argonne) and the German Bundesanstalt für Materialforschung und -prüfung (BAM) was signed in October 2014. Its objectives are to promote cooperation among scientists and specialists at Argonne and BAM and establish a framework for collaboration in advanced technologies associated with the back end of the nuclear fuel cycle. Collaborative activities involving Argonne and BAM may be implemented through the promotion of joint research activities and scientific workshops and conferences; exchange of technical information; and visits by scientists, specialists, and graduate, postgraduate, and Ph.D. students. The MOU was renewed in January 2020 for another five years. Highlights of the progress and achievements are provided in identified topical areas for collaboration on ageing management guidance, storage, transportation and disposal R&D, joint conference activities, and conclude with the benefits of the MOU in fostering Argonne and BAM collaboration.
In Germany spent nuclear fuel and high level radioactive waste is stored in interim storage containers with double lid systems. Those lids are equipped with metal seals (e.g. Helicoflex®) that ensure the safe enclosure of the inventory. The used metal seals consist of three components as can be seen in the cross-sectional view in Figure 1. The innermost part is a helical spring that is surrounded by an inner jacket made of stainless steel. The outer jacket that is made of a softer material which in case of assembly in the aforementioned storage containers is silver or aluminum (i.e. Al 99.5). During application the seal is compressed and due to the restoring force of the helical spring, the outer jacket is plastically deformed and adapts to the sealing surface. Hence, leakage paths are closed and the sealing function is generated. In Germany the above-mentioned containers are licensed for up to 40 years of interim storage, which in case extended storage becomes necessary before a final repository is available will have to be extended to even longer periods. Therefore, the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads as well.
At Bundesanstalt für Materialforschung und –prüfung (BAM) long-term investigations are being conducted in which seals are assembled in test flanges and aged at temperatures ranging from room temperature to 150°C for accelerated aging. The aged seals are tested semi-annually (after the first 6 months in which the seals are tested more frequently) regarding the sealing performance, the remaining seal force, and the useable resilience upon decompression. Results of these investigations have been published over the past years (e.g. Grelle, Wolff, Probst, Jaunich, & Völzke, 2017; Völzke, Wolff, Probst, Nagelschmidt, & Schulz, 2014). It was found that the seal force and the useable resilience decrease with time and temperature, which is in agreement with the result of other studies (Sassoulas et al., 2006; Wataru et al., 2016) as well. Geometry change of the outer jacket has been identified as the main reason for this seal behavior. At the prevailing operating temperatures and stresses the aluminum is subjected to creep deformation leading to a thinning of the outer jacket. Since the seal groove depth remains unchanged the helical spring expands, which in turn leads to a decrease of the generated spring and seal force.
Although the main reason for the change of seal parameters over time and temperature is known, a detailed characterization of the seal behavior and a reliable prediction of the parameter development for aging times that exceed the experimental time frame have not been possible, yet.
For deeper understanding of the aging processes, an Investigation program, which is covered in this contribution, is conducted at Bundesanstalt für Materialforschung und –prüfung (BAM) that focusses on the behavior of the aluminum jacket and its influence on the long-term sealing performance. The program investigates properties of material samples as well as the behavior of the seal as a component.
Original sheet material of the same aluminum that is used for manufacturing of the seals is investigated in compression creep tests. For this, a DMA (dynamic mechanical analysis) machine is employed (here used for static tests) that allows for a measurement of the specimens deformation under forces of up to 500 N. The advantage of this method is that the original material can be tested in the same shape as used for the seals which is 0.5 mm thick sheet material. For investigation of tensile creep standard specimens are used, that were machined from surrogate material of the same composition and annealing condition.
Furthermore, aluminum seals that are cut into smaller segments are assembled in flanges and placed in heating chambers at temperatures ranging from 23°C to 150°C. After different periods of time from 3 days to 300 days the segments are taken out of the flanges and are investigated, thus giving information on different states of aging. Measurements of the development of the seal contact width and the aluminum jacket thickness are done with an optical microscope. Further investigations on the segments will include metallography and hardness measurements.
From the detailed material and component behavior including the results of the long-term seal force and useable resilience investigations a better understanding of the overall seal behavior can be gained. The aim is to contribute to the development of material models and analytical approaches for the prediction of the sealing behavior in dependence of time and temperature.
Elastomere werden vielfach in Produkten eingesetzt, die bei verschiedenen Temperaturen verwendet werden. O-Ringe sind kostengünstige Dichtelemente, die allerdings für die Funktionsfähigkeit und Sicherheit eines Produkts entscheidend sein können. Die untere Temperatur-einsatzgrenze ist dabei relevant und aus wissenschaftlicher Sicht nicht allgemein gültig zu definieren, da diese einerseits durch die Änderungen der Materialeigenschaften im Zuge des Gummi-Glas-Übergangs definiert werden, die Temperaturlage dieses Übergangs jedoch sehr stark von den jeweiligen Einsatzbedingungen (z.B. Frequenz) abhängt. Dadurch ergeben sich große Unterschiede zwischen statischen und dynamischen Anwendungen.
Verschieden Untersuchungen sollen vorgestellt und interpretiert werden, um das Auditorium auf verschiedene Herausforderungen aufmerksam zu machen und Lösungsansätze vorzustellen.
Dichtungsverhalten bei niedrigen Temperaturen - Untersuchung der unteren Temperatureinsatzgrenze
(2018)
Elastomere werden vielfach in Produkten eingesetzt, die bei verschiedenen Temperaturen verwendet werden. Dabei sind O-Ringe kostengünstige Dichtelemente, die allerdings für die Funktionsfähigkeit und Sicherheit eines Produkts entscheidend sind. Die untere Temperatureinsatzgrenze ist dabei durchaus relevant und aus wissenschaftlicher Sicht nicht allgemeingültig zu definieren, da diese einerseits durch die Änderungen der Materialeigenschaften im Zuge des Gummi-Glas-Übergangs definiert werden, die Temperaturlage dieses Übergangs jedoch sehr stark von den jeweiligen Einsatzbedingungen (z.B. Frequenz) abhängt. Dadurch ergeben sich große Unterschiede zwischen statischen und dynamischen Anwendungen. Verschiedene Untersuchungen sollen vorgestellt und interpretiert werden, um das Auditorium auf verschiedene Herausforderungen aufmerksam zu machen und Lösungsansätze vorzustellen...
Editorial
(2019)
Dear Readers, a new year started for all of us (as I write these lines, possibly it was already some time ago when these lines are finally available) and this is the time for the so-called New Year’s resolutions. Setting goals and changing our behavior as well in a private as in a professional context.
For Scientists the resolutions may comprise tasks like finalizing a longago started publication, picking up the loose ends of an application for funding or just bringing the running projects in a greater structure.
High and ultra-high molecular weight polyethylenes were gamma-irradiated with doses up to 600 kGy. The changes in the material properties were analysed using DSC, DMA, IR spectroscopy, as well as measurements of density and insoluble content. The irradiation led to an increase of the degree of crystallinity because of chain scissions during irradiation, leading to shorter and thus more mobile chains. Both the plateau value of the shear modulus G′ and the insoluble content increased with Irradiation dose, indicating the formation of additional crosslinks. Furthermore, IR spectroscopy revealed irradiation induced oxidation and the formation of double bonds, indicating that some of the hydrogen atoms responsible for the neutron shielding capability have been released.
To improve the predictive capability of long-term stress relaxation of elastomers during thermo-oxidative ageing, a method to separate reversible and irreversible processes was adopted.
The separation is performed through the analysis of compression set after tempering. On the Basis of this separation, a numerical model for long-term stress relaxation during homogeneous ageing is proposed. The model consists of an additive contribution of physical and chemical relaxation.
Computer simulations of compression stress relaxation were performed for long ageing times and the results were validated with the Arrhenius treatment, the kinetic study and the time-temperature superposition technique based on experimental data. For chemical relaxation, two decay functions are introduced each with an activation energy and a degradative process. The first process with the lower activation energy dominates at lower ageing times, while the second one with the higher activation energy at longer ageing times. A degradation-rate based model for the evolution of each process and ist contribution to the total system during homogeneous ageing is proposed. The main advantage of the model is the possibility to quickly validate the interpolation at lower temperatures within the range of slower chemical processes without forcing a straight-line extrapolation.
The indication-oriented Dental Bone Graft Substitutes (DBGS) selection, the correct bone defects classification, and appropriate treatment planning are very crucial for obtaining successful clinical results. However, hydrophilic, viscoelastic, and physicochemical properties’ influence on the DBGS regenerative potential has poorly been studied. For that reason, we investigated the dimensional changes and molecular mobility by Dynamic Mechanical Analysis (DMA) of xenograft (cerabone®), synthetic (maxresorb®), and allograft (maxgraft®, Puros®) blocks in a wet and dry state. While no significant differences could be seen in dry state, cerabone® and maxresorb® blocks showed a slight height decrease in wet state, whereas both maxgraft® and Puros® had an almost identical height increase. In addition, cerabone® and maxresorb® blocks remained highly rigid and their damping behaviour was not influenced by the water. On the other hand, both maxgraft® and Puros® had a strong increase in their molecular mobility with different damping behaviour profiles during the wet state. A high-speed microscopical imaging system was used to analyze the hydrophilicity in several naturally derived (cerabone®, Bio-Oss®, NuOss®, SIC® nature graft) and synthetic DBGS granules (maxresorb®, BoneCeramic®, NanoBone®, Ceros®). The highest level of hydrophilicity was detected in cerabone® and maxresorb®, while Bio-Oss® and BoneCeramic® had the lowest level of hydrophilicity among both naturally derived and synthetic DBGS groups. Deviations among the DBGS were also addressed via physicochemical differences recorded by Micro Computed Tomography, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, X-ray powder Diffractometry, and Thermogravimetric Analysis. Such DBGS variations could influence the volume stability at the grafting site, handling as well as the speed of vascularization and bone regeneration. Therefore, this study initiates a new insight into the DBGS differences and their importance for successful clinical results.