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Paper des Monats
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Eingeladener Vortrag
- nein (19)
Rubber is widely used as sealing material in various applications. In many fields the function of seal materials at low temperatures is necessary. 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 temperature dependent. At low temperatures this is caused by the rubber-glass transition (abbr. glass transition). During continuous cooling, due to the glass transition the material changes from rubber-like entropy-elastic behaviour to stiff energy-elastic behaviour, that allows nearly no strain or retraction. Hence, rubbers are normally used above their glass transition. But as the minimum working temperature limit of elastomers cannot be defined globally and precisely, the lower operation temperature limit of rubber seals should be determined in dependence of the application conditions and the most relevant material properties.
In this paper, wesummarize results of our temperature dependent investigation of seal material properties by classical thermal analysis as Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA), combined with measurements of standardized tests as compression set and the seal performance determined in component tests. To reduce the test time of compression set tests a faster technique was developed and applied.
To study the influence of dynamic events on the seal performance and to enhance the understanding of occurring seal failure, a setup for a fast partial seal release was designed.
Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement.
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 encapsulation 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 during transport.
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 temperature dependent. 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, due to the glass transition. Hence rubbers are normally used above their glass transition but the minimum working temperature limit is not defined precisely, what can cause problems during application. 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 the results of standardized measurements as the compression set according to ISO 815. To reduce the test time of the standard tests a faster technique 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 fluorocarbon rubber (FKM) was selected for this investigation as it is often used for radioactive waste containers. Some materials (seals and test sheets) were purchased from a commercial seal producer and some materials were compounded and cured at BAM in form of rubber sheets.
In Germany, the concept of dry interim storage in dual purpose metal casks before disposal is being pursued for spent nuclear fuel (SF) and high active waste (HAW) management. However, since there is no repository available today, the initially planned and established dry interim storage license duration of up to 40 years will be too short and its extension will become necessary. For such a storage license extension it is required to assess the long-term performance of SF and all safety related storage system components in order to confirm the viability of extended storage.
The main safety relevant components are the thick-walled dual purpose metal casks. These casks consist of a monolithic cask body with integrated neutron shielding components (polymers, e.g. polyethylene) and a monitored double lid barrier system with metal and elastomeric seals. The metal seals of this bolted closure system guarantee the required leak-tightness whereas the elastomeric seals allow for leakage rate measurement of the metal seals.
This paper presents an update on running long-term tests on metal seals at different temperatures under static conditions over longer periods of time. In addition, first results of our approach to understand the aging behavior of different elastomeric seals and neutron radiation shielding material polyethylene are discussed.
Elastomers are widely used as the main sealing materials for containers for low and intermediate level radioactive waste and as an additional component to metal seals in spent fuel and high active waste containers. The safe encapsulation of the radioactive container inventory has to be guaranteed according to regulation and appropriate guidelines for long term storage periods as well as for temperatures as low as -40°C during transport. 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 elastomers are strongly temperature dependent. At low temperatures, this is caused by the rubber-glass transition (abbreviated: glass transition). During continuous cooling, the material changes from a rubber-like entropy elastic to a stiff energy elastic behaviour, which allows nearly no strain or retraction. Hence, rubbers are normally used above their glass transition, but the minimum working temperature limit is not defined precisely; this can cause problems during the above noted applications. Therefore, the lower operation temperature limit of elastomer seals must be determined in dependence of the material properties. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) are combined with standardised measurements to determine the compression set according to ISO 815. To reduce the test time of the standard tests, a faster technique than normally used was developed. Additionally, the breakdown temperature of the sealing function of complete O ring seals was measured in a component test set-up to compare it with the results of the other tests. The experimental set-up is capable of measuring the leakage rate at low temperatures by the pressure rise method. A fluorocarbon rubber (FKM) was selected for this investigation as it is often used for radioactive waste containers. The materials (seals and test sheets) were purchased from a commercial seal producer.
Ultra high molecular weight polyethylene (UHMW-PE) - due to its high hydrogen content - is used as neutron shielding material in casks for storage and transport of radioactive materials. Besides this, UHMW-PE - as a high-performance polymer - has been used for several years in medical technology due to its excellent slip and wear properties. Due to the special properties of UHMW-PE which result basically from its extreme chain lengths and its high degree of crystallinity, it is predestinated for the aforementioned applications.
In both cases, irradiation and its impact on the molecular structure of polyethylene play an important role. In the first case, irradiation exists as a by-product of inserting the radioactive material in the cask. Hence PE has to withstand any type of degradation affecting safety relevant aspects to be applicable for long term radiation shielding purposes for instance over a period of 40 years. In the second case irradiation is applied deliberately for purposes such as sterilization and crosslinking, leading to partial improvement of the mechanical properties (e.g. fracture toughness, crack propagation resistance, wear resistance) and better Chemical stability.
Specifically concerning their use in the field of medical technology, different types of UHMW-PE have been objects of numerous publications. It is generally accepted that two parallel and competitive processes, based on chain scission and reactions of Ccentered radicals and molecular fragments, occur in PE as a consequence of radiation: radical recombination accounts for crosslinking, together with some disproportionation, formation of low molecular weight fragments, and recrystallization. Furthermore, formation of oxygenated structures in the presence of traces of oxygen is an antagonist of the C-centered radicals. Radiation induced scission preferentially takes place in the amorphous phase and noncrystalline surface of the crystals. It is followed by folding of molecular fragments, crystallinity growth and increased perfection in the crystal lamellae [4, 5]. Chain scission results in shorter polymer molecules, fewer entanglements, and consequently, increased molecular mobility.
The scope of our investigation comprises an estimation of the radiation and thermal impact on the molecular and supra molecular structure of the two types of PE used for neutron shielding cask components. A further point which is worth to explore is to what extent these changes are detectable by thermo-analytical (TA) methods, such as Differential Scanning Calorimetry (DSC), Thermo Mechanical Analysis (TMA), Dynamic Mechanical Analysis (DMA) and Thermogravimetry (TG). Additionally FT-IR and solubility measurements have been performed.
In our studies we focused on the UHMW-PE material GUR 4120 which was y irradiated at RT and compared to the untreated material.
THz and Mid IR Fourier transform spectroscopy on polyethylene irradiated with Gamma- Co60 radiation
(2014)
THz and mid IR spectroscopy of high molecular PE (HMW) and ultra high molecular PE (UHMW) reveals modifications of the molecular structure induced by γ-Co60 radiation. UHMW-PE and HMW-PE can be distinguished. The integral absorption in the B1u THz-region can quantitatively describe the amorphization of crystallinity. The formation of trans vinylene unsaturations and the decay of vinyl can be followed by mid IR spectroscopy
The thermal expansion of polymeric parts can be an issue in many applications where the available space is limited, or exact dimensions of the part are required. For this study, a device was designed and built that allowed measuring the thermal expansion simultaneously in all three spatial directions on cubic samples with real-scale dimensions (78 mm edge length). The results are shown between 25 °C and 125 °C for two PE materials, one HMWPE and one tempered UHMWPE, for non-irradiated samples as well as cubes that have been irradiated with 100 and 400 kGy. The results measured with the new device were very similar to those measured with conventional thermo-mechanical analysis equipment and to literature data of UHMWPE. The HMWPE material shows a much larger thermal expansion coefficient in one direction compared to the other two directions during the first heating due to frozen stresses from the pressing step during material manufacturing. These stresses are mostly released by the expansion during the first heating, so that the expansion during the second heating is more uniform. The overall volumetric expansion is the same for both heating runs. By contrast, the tempered UHMWPE material shows no significant difference between first and second heating run, as the stresses from processing could already relax in the tempering step. The irradiation treatment does not affect the values significantly for the given test set-up.
Due to delays in the siting procedure to establish a deep geological repository for spent nuclear fuel and high level radioactive waste as well as in construction of the already licensed Konrad repository for low and intermediate level radioactive waste, extended periods of interim storage become more relevant in Germany. BAM is involved in most of the cask licensing procedures and especially responsible for the evaluation of cask-related long-term safety issues.
The long-term performance of elastomer seals for lid systems of transport and storage casks, whether used as auxiliary seals in spent fuel casks or as primary seals for low and intermediate level waste packages, is an important issue in this context. The polymeric structure of these seals causes a complex mechanical behavior with time-dependent sealing force reduction.
The results of a comprehensive purpose-designed test program consisting of basic compression and tension tests as well as relaxation tests on unaged specimens of representative types of elastomers (fluorocarbon rubber (FKM) and ethylene propylene diene rubber (EPDM)) at different temperatures and strain rates are presented. They were used to identify the constitutive behavior and to obtain parameters for finite element material models provided by the computer code ABAQUS®. After estimating the influence of uncertainties such as Poisson’s ratio and friction coefficient by sensitivity analyses, the chosen parameters had to prove their suitability for the finite element simulation of the specimen tests themselves.
Based on this preliminary work the simulation of a specific laboratory test configuration containing a typical elastomer seal with circular cross section is presented. The chosen finite element material model and the implemented parameters had to show that they are able to represent not only the specimen behavior under predominantly uniaxial load but also the more complex stress states in real components. Deviations between the measured and calculated results are pointed out and discussed.
For the consideration of long-term effects in the simulation of elastomer behavior, test results of aged specimens are needed. First information about a new test program, started recently and planned to provide these data, are given.