Degradation von Werkstoffen
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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.
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.
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 an ageing temperature of 125 °C. To exclude possible diffusion limited oxidation (DLO) effects that can distort the data, IRHD micro hardness measurements were performed over the cross-section of compressed O-rings. Continuous stress relaxation measurements were conducted 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.
The main task of the division "Safety of Storage Containers" at BAM is the safety assessment of storage containers for radioactive waste. A sufficient sealing of bolted lid systems for the safe containment of the waste for transport, storage and disposal is very important. Extensive knowledge of the change of the elastomer’s properties during ageing and the availability of reliable end-of-lifetime criteria is mandatory to guarantee long term safe enclosure.
In a long-term test programme over 5 years we have studied the degradation and the change of sealing properties of several elastomers, including EPDM, at four different ageing temperatures (75 °C, 100 °C, 125 °C and 150 °C). Compression stress relaxation (CSR) and compression set (CS) experiments were carried out. It has been found that when the data does not cover a sufficient time frame necessary for the evolution of the degradation of a chosen property, a curvature in the Arrhenius relationship is observed. For CSR, the curvature was observed for samples aged up to 186 days. As for CS experiments, the curvature was detected for sample aged up to 2 years. To cover the possible lack of experimental long-term data at low temperatures, a numerical model for CSR was developed and longer ageing times for the simulation were adopted. A degradation-rate based model for the evolution of degradative processes 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 an Arrhenius straight-line extrapolation. The model was also applied to CS experiments and validated by the 5 years experimental results where the curvature was gone, and the degradation property has followed an Arrhenius relationship. In the figure the contribution of the two degradative processes are shown over CS and CSR respectively.
Microbiologically influenced corrosion (MIC) is a highly unpredictable process involving a complex group of microorganisms, including sulfate-reducing bacteria and methanogens. Standard laboratory MIC testing using static serum bottle enrichments is an easy but limited method, offering poor resolution on the biomineralization process of corrosion products. An example of this is the presumed corrosion product siderite by corrosive methanogens (Mi-MIC). Previous publications reported siderite was the sole corrosion product of M. maripaludis using metal coupons incubated under stationary conditions.
However, the formation of siderite is closely related to the surrounding environmental conditions, i.e. pH, CO2 concentration, flow and temperature. Thus, siderite as the sole corrosion product of Mi-MIC remain inconclusive and questionable. To study Mi-MIC effectively, a novel versatile multiport flow-column corrosion monitoring system (MFC) was developed. MFC allows sectional corrosion rate determination under flow conditions using different types of material, inoculum and packing material. MFC offers great flexibility, ease of operation and accurate corrosion measurements that can be combined with many other techniques. Using MFC, we studied multiple strains of methanogens and compared it with sulfate-reducing bacteria under neutral and low pH conditions. It was revealed by MFC that corrosive methanogens have equally high corrosion potential as sulfate-reducing bacteria. Additionally, siderite is not the dominant nor sole corrosion product of Mi-MIC. Thus, effective corrosion monitoring and establishing standard laboratory practices, i.e. incorporating MFC as part of regular testing process, will provide deeper understanding of MIC. This will allow further microbial electrophysiology understandings, contributing to effective mitigation strategy development.