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Biofuels including ethanol and biodiesel (FAME) represent a renewable fuel alternative to petroleum-derived transport fuels. The aim of this work was to study the interaction between high density polyethylene (HDPE) with permeation barriers in form of polyamide (PA) and fluorination, and biofuels such as E85 (fuel with 85 % ethanol), biodiesel and B10 (heating oil with 10 % biodiesel). 10 l jerrycans made of polyethylene with permeation barrier of PA were filled with E85 and biodiesel and exposed to temperatures of 20 °C and 40 °C for 5 years. Half of the 20 l jerrycans of HDPE for filling with B10 were fluorinated at the inner layer to prevent permeation before the exposure. Tensile properties were determined once a year, and FTIR-spectroscopy was used to evaluate possible changes.
The tensile properties tensile strength and breaking elongation of HDPE jerrycan cuttings with permeation barrier decreased, but not significantly, after immersion in E85, biodiesel and B10. The elasticity modulus of the polyethylene grades was especially reduced during exposure to E85.
The FTIR spectra of HDPE jerrycan cuttings with permeation barrier showed that immersion tests for five years with the test fuels at 20 °C and 40 °C did not lead to a decomposition of the permeation barriers.
THz and mid IR spectroscopy of high-molecular PE (HMW) and ultra high-molecular PE (UHMW) reveals modifications of the molecular structure. Characteristic absorption bands are changed if the two materials are exposed by γ-Co60 radiation up to 600 kGy and subsequently stored at an annealing temperature of 398 K until for 729 days.
Fibre-reinforced plastics (FRP) especially carbon-fibre-reinforced polymer (CFRP) and glass-fibre-reinforced polymer (GFRP) are commonly used materials in high pressure vessels and storage units for automotive and aerospace purposes. Optical fibres are suitable to be integrated or directly applied to the surface of FRP components. Using optical fibres it is possible to monitor the distributed strain profiles and changes within the fatigue life of a pressure vessel to ensure the operational safety. Within artificial ageing experiments we used swept wavelength interferometry (SWI) based distributed strain sensing for the monitoring of commercial high-pressure composite cylinder. This artificial ageing was performed using test conditions of 503bar pressure load (service pressure 300 bar) and 89 °C for 100 h. The polyimide coated optical fibres were glued to the surface externally in circumferential and axial direction. Using distributed strain sensing (DSS) material expansion of over 0.5% were monitored with sub-centimetre spatial resolution. Within the circumferential direction we observed up to 10 % local fluctuation compared to the median strain caused by inhomogeneous material expansion, which could cause local material fatigue. In addition, we determined material degradation manifested itself as localized remaining material expansion and/or contraction. Results have been validated by other non-destructive methods like digital strip projection.
Within a current research project at the Federal Institute for Materials Testing and Research (BAM), the degradation process of composite pressure vessels is studied to be able to give more accurate lifetime predictions in future. The presented research is based on type III pressure vessels consisting of an aluminium tank which is fully wrapped with carbon fibre reinforced plastics. Focus is set on the analysis of residual stresses which are induced into the pressure vessel during manufacturing process in order to increase high cycle fatigue. However, with increasing lifetime residual stress conditions do change. To be able to measure and monitor stress conditions, the application of a non-destructive measurement method is aspired.
In this paper, potential of an experimental modal analysis is worked out to capture and monitor aging and degradation effects in pressure vessels. With the presented method, information about changes in residual stress can be obtained via an analysis of the modal parameters. To realize an application, first, a finite element simulation is used to prove and evaluate potential capability and validity. In the following, a test bench is set up and successively optimized in its accuracy and efficiency. Sensitivity of the applied measurement technique is experimentally ascertained trough the measurement of several prestress modified pressure vessels. Finally, experimental results are interpreted and evaluated with the help of numerically gained findings.
Elastomers show a high versatility which makes them ideal materials for sealing applications in various fields. Especially under changing application conditions the high recovery potential of this class of material is beneficial to compensate temperature or pressure fluctuation, and geometrical changes resulting from mechanical loads in e.g. accident conditions. Out of these reasons elastomers are also used in containers for low and intermediate level radioactive waste and for spent fuel transportation casks. In casks designed for low and intermediate level waste elastomer seals can act as primary seal responsible for the containment function whereas in spent fuel storage and transportation casks (dual purpose casks (DPC)) elastomer seals are used as auxiliary seals to allow leakage rate measurements of metal barrier seals. An inherent prerequisite for this kind of application is the Long time-scale of operation without or with limited possibility of seal replacement. In Germany an interim storage license for DPC`s is typically issued for 40 years, a timeframe which might increase in the future due to challenges of the final repository siting procedure. For low and intermediate level waste, also long time periods are required before final disposal can be achieved. Therefore, the performance of elastomer seals over extended time periods is, as for other applications, of high importance.
A typical approach to ensure long-term functionality is to perform accelerated aging tests to calculate an estimated lifetime by assuming e.g. Arrhenius like equations for the timetemperature relationship. This approach requires a suitable end of life criterion considering the application of interest. This often can represent a challenge on its own.
As BAM is involved in most of the cask licensing procedures and especially responsible for the evaluation of cask-related long-term safety issues we initiated several test programs for investigating the behavior of elastomer seals. Experiments concerning the low temperature performance down to -40 °C and the influence of gamma irradiation have been started first.
Currently the thermal aging behavior of elastomer seals, which is the topic of this contribution, is examined. For our aging investigations we use a broad approach to first determine the property changes in different elastomer materials due to thermo-oxidative aging at elevated temperatures and secondly, we test how the typical methods of lifetime extrapolation can be applied to these results. This Approach enables us to detect and exclude undesired side effects which very often influence lifetime estimations. In this contribution, our recent results are extended. The results show that lifetime estimation based on single material properties can be misleading and therefore a combination of several methods is recommended.
Weathering reference materials (WRMs) are used to characterize the harshness of an exposure, aiming on either reproducibility of a specific exposure or on the comparability between various kinds of natural or artificial weathering exposure.
The materials that are used as weathering reference materials differ in their sensitivities (as well as in interactions and interferences of the latter), conditioned by the different processes which lead to the respective property change. It is also essential to take into account the necessary measurement equipment for the respective property change, in order to allow timely intervention.
What are the key issues on choosing a weathering reference material?
What can be learned from the weathering reference materials, investigated so far?
Possibilities and limitations are discussed on the basis of existing weathering reference materials. Conclusions are drawn, for establishing new weathering reference 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 (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.
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.
Biodiesel (FAME) from rapeseed is an environmentally friendly alternative to common fossil fuels. It is also suitable to serve as blending component to fuels like heating oil. If the fuel composition is changed, materials compatibility must be guaranteed. Adding polar biodiesel to nonpolar heating oil, changes the blend’s solvency and might cause swelling, extraction and solvation of polymers. The objective of this research was to investigate the compatibility of polymeric materials, which are commonly used for components in middle distillate facilities, along with blends of heating oil and 20 % biodiesel (B20). For this propose, ACM, HNBR, FKM, PE, PA 6, POM, PUR and PVC were exposed to heating oil and B20 for 42 and 84 days at 40 °C. In addition, the polymers HNBR, FKM, PA, POM and PVC were also exposed at 70 °C. Furthermore, the resistance of polymers in eight-year aged B10 at 40 °C was evaluated. Ageing of biodiesel increases acidity which might propagate polymer corrosion. The materials were evaluated as resistant, if the loss in tensile properties (tensile strength and elongation at break) and Shore hardness remained under 15 % compared to the initial unexposed material values. For investigations under compressed conditions, the compression set was determined for specimens of ACM, FKM and HNBR after exposure in heating oil B0 and B20 for 3,7,14, 28, 56 and 90 days at 40 °C according to ISO 815-1. It was found that the resistance in B20 at 40 °C was given for all tested polymers except PUR. In the 8 years aged B10, PUR and POM were not compatible and ACM just conditionally compatible. At 70 °C, FKM and PVC were resistant in B20, whereas HNBR and PA 6 were not compatible. Swelling occurred for the elastomers ACM, HNBR and PUR.
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.