TY - JOUR A1 - Spitzer, Stefan A1 - Pandal, Adrián A1 - Rodríguez, Manuel Velasco A1 - Schmidt, Martin A1 - Danzi, Enrico A1 - Dufaud, Olivier A1 - Janovsky, Bretislav T1 - Investigations on different distribution systems for dusts inside the 20L-sphere N2 - The determination of several safety characteristics for dusts requires the dispersion of it in air. This is normally conducted using two vessels, one with an overpressure holding the dust and dispersing it into the second one, where the explosion takes place, through a nozzle. This procedure has the disadvantage that some dusts cannot be conveyed through the nozzle properly. Another disadvantage is that the pressure balancing between the two vessels depends on the dust loading and especially for heavy dusts and high loadings the initial pressure inside the explosion vessel might be reduced. Flocky dusts or dusts that might be dangerous to convey through a thin nozzle with an overpressure (nano powders, zirconium) are also difficult to test according to the existing standards and may not be tested with the standard nozzles, that are so far used for the determination of safety characteristics. One very recent example, testing nitrocellulose, raised the question, whether some dusts even pose a risk being distributed and pressed through a nozzle for the testing device and, in worst case, for the operator. Previous researchers have developed alternative types of nozzles for specific types of dust, but provide limited evaluation of their performance relative to standard nozzles. Additionally, researchers have not provided sufficient geometry so that they can be reproduced by others. One alternative nozzle for the dispersion of flocky or coarse dusts is stated in the ISO standard but not described there either. This article investigates four types of nozzles: The two standard ones that are widely used already, an alternative type, that got introduced into the international standard in 2016 but is still seldomly used and one that was constructed to overcome some of the observed disadvantages. The injection curves are compared with and without dust loadings as well as the explosion characteristics. Eventually, a suggestion is given for different types of dusts. KW - Dust explosions KW - Safety characteristics PY - 2024 DO - https://doi.org/10.1016/j.jlp.2024.105492 SN - 0950-4230 VL - 92 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-61697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Stoian, R. A1 - Bonse, Jörn T1 - Ultrafast Laser Nanostructuring — The Pursuit of Extreme Scales N2 - Long seen as “a solution seeking a problem,” laser pulses are nowadays – more than 60 years after their first practical demonstration – paramount in shaping and structuring matter. Harnessing their capabilities to direct intense beams of light, the number of scientific and technological developments and daily-life applications is continuously increasing. Today, the presence of lasers is ubiquitous in all sites of scientific and technological interest, from the most advanced research laboratories to industrial factories and medical hospitals. The directionality of the laser beam determines equally a local character on lightmatter interaction and as such a local modification to a material target. Furthermore, the coherence of laser radiation enables near-field or far-field scattering and interference effects that widen significantly the capabilities of controlling and tracking laser-matter interactions in space and time. Already with the advent of lasers, powerful beams of light have been directed at solid materials for a variety of purposes, making this application as old as the laser itself. The roots of the major applications for laser structuring were developed already in the 1960s, setting the base of both theoretical and experimental studies on laser ablation, with the number of publications expanding explosively during the next decades. Within this dynamic context, laser processing of materials experienced an impressive development over the years. Laser processing means specifically the capability to structure and tailor a material on its surface or even within its volume, rendering new functions and properties that are impacting the mechanical, electrical, or optical characteristics of the material. These properties are scaledependent, generating thus over the years an equally impressive quest for spatial or temporal resolution. Therefore, the developments in laser engineering with major breakthroughs, notably in pulse duration and power, always closely accompanied the efforts in material structuring with two milestones in sight: (1) yield and (2) resolution. Every step in shrinking the laser pulse duration led to a subsequent strong-impact development in process precision – particularly when the ultrashort pulse durations surpassed the fundamental electron-phonon relaxation times. Thus, minimizing heat diffusion, the advent of pulses with duration smaller than molecular or lattice vibration times has managed to confine the spatial resolution to the optical diffraction limit and sometimes even beyond. The nanoscale was already in sight at the turn of the millennium. An important question may be raised now; is there any fundamental limit in the processing resolution, a barrier defined by the intrinsic properties of light and matter? The answer has an inherently multidisciplinary nature, following the conversion of free-propagating electromagnetic radiation into material-confined energy potentially usable to drive or transform matter, and will be the focus of the present book. Relying on the experience and expertise of the leading researchers in the field, the present book intends to explore the current efforts in achieving laser processing resolution beyond the diffraction limit, laying down a perspective towards extreme laser nanostructuring. Following the most recent advances and developments, it puts forward a concept of extreme processing scales enabled by optical pulses that are able to bypass diffraction limits and achieve structuring characteristic scales beyond 100 nm. This objective can be achieved by a comprehensive understanding on how light can change matter and how, in turn, matter can change light, allowing jointly for actively controlling light and material processes. In order to give an extended perspective on the current state-of-the-art in the field of precision laser structuring, the book is divided into three main parts. The first part of the book (Part I: Fundamental Processes) offers a perspective into the fundamentals of laser-matter interaction on extreme spatial scales, with a description of the most advanced modeling efforts in understanding energy deposition in matter, a plethora of material-relaxation pathways, as well as advanced concepts for probing and observing matter in motion. Roadmaps for energy localization will be developed, and the atomistic perspective of laser ablation visualized. Theoretical modelling enables in-depth insights on ultrafast quantum processes at the nanoscale. Laser-driven self-organization at surfaces will be dissected regarding the question of how light drives material periodic patterns down to the nanoscale, explored and transmitted to its ultimate limits of an atomic printer, and immediately complemented by the unprecedented capabilities of ultrafast in-situ observation approaches for tracking the laser-induced material response with extreme spatial and temporal resolution. In the second part of the book (Part II: Concepts of Extreme Nanostructuring), distinct concepts will be developed and explored that allow confinement of light and harnessing of a material response restricted to nano- or mesoscopic scales at surfaces or in the volume of irradiated materials. A special focus will be on optical near-field related approaches for localizing light on scales even below the optical diffraction limit and plasmonic printing. Spatial and temporal beam-shaping and tailored interference techniques are discussed in the context of ultrashort laser pulses, and insights into some extreme states of matter realized by the tight confinement of laser energy are presented. The ultimate limits of writing waveguides in the bulk of dielectrics and for manifesting 3D-nanolithography are elucidated. Plasma-based surface treatments can significantly enhance the vertical precision of surface processing through etching processes. Finally, the third part of the book (Part III: Applications) leads us to a number of resuming applications, unveiling the tremendous capabilities of surface functionalization through laser micro- and nanostructuring, assessing the 3D-writing of waveguides in the bulk of dielectrics or semiconductors for enabling new branches of integrated photonics, and summarizing related applications ranging from nanophotonics to nanofluidics and from optical sensing to biomedical applications, including the latest capabilities of refractive eye surgery. This part will analyze the applications’ compatibility in yield and reproducibility with current industrial requirements, costs, and intellectual property aspects. It expands the involved spatial scales by more than eight orders of magnitude, when extending extremely small structures featuring sizes of few tens of nanometers to larger dimensions in the meter range. Thus, from surfaces to the bulk, from subtractive to additive manufacturing approaches, from advanced theoretical frames to practical technological processes – we invite the readers here to an exciting journey into the varicolored landscape of extreme laser nanostructuring. The idea of this book project was seeded in early 2020. We were delighted about the numerous and extremely positive responses from the laser-processing community, quickly receiving commitments for more than 30 individual book chapters. About 2500 communications later, the book is published. We would like to thank all authors of this book project for their insightful and detailed chapters, reviewing and reporting on this fascinating topic of the pursuit of extreme scales in ultrafast laser nanostructuring. Moreover, we would like to acknowledge the professional help and guidance of the staff of Springer Nature. Finally, we hope you will enjoy reading this book as much as we have enjoyed putting it together. Saint Etienne, France Razvan Stoian Berlin, Germany Jörn Bonse December 2022 KW - Laser nanostructuring KW - Surface engineering KW - Nonlinear lithography KW - Self-organization KW - Laser-induced periodic surface structures, LIPSS PY - 2023 SN - 978-3-031-14752-4 SN - 978-3-031-14751-7 DO - https://doi.org/10.1007/978-3-031-14752-4 SN - 0342-4111 VL - 239 SP - 1 EP - 1245 PB - Springer Nature Switzerland AG CY - Cham ET - 1 AN - OPUS4-57294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zaghdoudi, Maha T1 - Numerical modelling of compression stress relaxation and compression set of elastomer O-rings during aging N2 - 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 T2 - ASME 2020 Pressure Vessels & Piping Conference (PVP2020) CY - Online meeting DA - 03.08.2020 KW - Stress relaxation KW - Ageing KW - Compression Set KW - O-ring KW - Sequential analysis KW - Simulation PY - 2020 AN - OPUS4-52135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Elastomer seals - overview and development N2 - The talk summarizes the current and future investigations of elastomer seal materials in division 3.4. T2 - IRSN-BAM Symposium Safety of Transport and Storage Packages CY - Online meeting DA - 19.11.2020 KW - Seal KW - Degradation KW - Ageing PY - 2020 AN - OPUS4-51751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sagradov, Ilja T1 - Long-term tests and numerical simulations on metal seals based on continuous force measurement in compressed state N2 - In Germany, the search for a disposal site for heat-generating radioactive waste will take decades longer than originally assumed. Transport and storage casks must therefore ensure safe containment for extended interim storage periods, possibly over 100 years. In order to maintain the required leak tightness, spring core metal seals with aluminum or silver cladding are used. As sealing force decreases over time, BAM has been conducting tests for over 15 years to prove their long-term reliability. This work - a joint project of BASE and BAM - aims to obtain additional material data using a new device for continuous measurement of compression force over time and temperature for lifetime prediction models and is supported by FEM simulations. Initial tests on aluminum and silver seals have been completed, and first results are presented. T2 - safeND 2025 CY - Berlin, Germany DA - 17.09.2025 KW - Interim storage KW - Metal seal KW - Restoring force PY - 2025 AN - OPUS4-64991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grelle, Tobias T1 - Creep Investigations on Aluminum Seals for Application in Radioactive Waste Containers N2 - In Germany spent nuclear fuel (SNF) and high level radioactive waste (HLW) are 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. Being licensed for up to 40 years of interim storage the evaluation of the long-term behavior of the seals is necessary, taking into account storage conditions, decay heat and possible mechanical loads. T2 - International Conference on Aluminum Alloys CY - Montreal, Canada DA - 17.06.2018 KW - Metal seal KW - Creep KW - Long-term behavior PY - 2018 AN - OPUS4-45843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zaghdoudi, Maha A1 - Weber, Mike A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Simulation of compression set of epdm o-rings during aging N2 - It is common practice in the application of finite element analysis to model compression set (CS) of elastomers during aging with two different material models according to the two-network theory of Tobolsky. The theory relies on the existence of two networks. The first one represents the original network after vulcanization and is sensitive to chain scission. The second network accounts for the formation of additional crosslinking during aging. Besides the use of user subroutines to describe the two-network model, an element overlay technique is also needed as the full set of both material behaviors did not exist for assignment to a single element. This element overlay technique is valuable for research and developmental purposes but makes extension to industrial usage quite challenging. Our goal is to simulate the CS of elastomers after long-term aging in a commercial finite element software with no need for extra subroutine codes or mesh superposition. Ethylene propylene diene (EPDM) O-rings were aged in a compressed state at 75 °C, 100 °C, 125 °C and 150 °C for up to 183 days. Investigations of the experimental test results were used to identify material models and their parameters to develop a finite element model to simulate CS. The model was implemented in the finite element software ABAQUS/Standard® with a sequential temperature-displacement coupling. Regarding the influence of temperature, the Arrhenius equation is adopted for the time-temperature relationship. The activation energy value that is required for the simulation is firstly determined from shifting the experimental CS results with the time-temperature superposition technique and plotting the shift factors in an Arrhenius diagram. The experiments were compared with the simulation results. Afterwards different activation energies were used in the simulation and discussed. A suitable choice of the activation energy value with regard to the reference temperature and the test temperature is presented. With the chosen activation energies, the match between numerical CS values after long-term aging and the experimental results was improved. T2 - ASME 2022 Pressure Vessels & Piping Conference CY - Las Vegas, USA DA - 17.07.2022 KW - Simulation KW - Compression set KW - EPDM KW - Aging PY - 2022 SP - 1 EP - 9 AN - OPUS4-57370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn T1 - Chemical and structural changes at the surface of titanium materials upon irradiation with near-infrared ultrashort laser pulses N2 - Due to its large strength-to-weight ratio and excellent biocompatibility, titanium materials are of paramount importance for medical applications, e.g. as implant material for protheses. In this work, the evolution of various types of laser-induced micro- and nanostructures emerging on titanium or titanium alloys upon irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment is studied for various laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz). The morphologies of the processed surfaces were systematically characterized by optical and scanning electron microscopy (OM, SEM). Complementary white-light interference microscopy (WLIM) revealed the corresponding surface topographies. Chemical and structural changes were analysed through depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS) and X-ray diffraction (XRD) analyses. The results point towards a remarkable influence of the laser processing parameters on the surface topography, while simultaneously altering the near-surface chemistry via laser-induced oxidation effects. Consequences for medical applications are outlined. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Laser-induced periodic surface structures (LIPSS) KW - Surface functionalization KW - ToF-SIMS KW - Chemical analysis KW - Titanium PY - 2022 AN - OPUS4-54931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Dichtungsverhalten bei niedrigen Temperaturen - Untersuchung der unteren Temperatureinsatzgrenze von Elastomerdichtungen - N2 - 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. T2 - ISGATEC Forum Werkstoffe 2019 CY - Mannheim, Germany DA - 03.12.2019 KW - Dichtung KW - O-Ring KW - Tiefe Temperaturen KW - Versagenstemperatur PY - 2019 AN - OPUS4-49983 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sagradov, Ilja T1 - Long-term tests on metal seals using continuous force measurement in compressed state N2 - In Germany, spent fuel and heat generating radioactive waste is stored in casks for transport and storage (DPCs). The storage licenses were granted for up to 40 years. Due to the delay in identifying a final repository site for such radioactive waste, the storage periods are to be extended significantly. The objective of our research work is to collect additional material data for metal seals in order to be able to better assess the long-term safety of the sealing system of the casks for a period of up to 100 years. A principal safety consideration for the DPCs is the long-term performance of bolted lid sealing systems utilizing metal seals to ensure the safe enclosure of the radioactive inventory during interim storage. To assess the sealing behavior, it is necessary to examine the aging-dependent residual restoring force for the metal seals and the usable resilience. By investigating the change in these values as a function of time and temperature, further insight can be gained into the assessment of long-term safety for extended interim storage. In the present study, the restoring force of metal seals with an outer aluminum jacket and a torus diameter of 9.9 mm was measured continuously. For this purpose, a specially designed device equipped with a load cell was used under isothermal conditions. As part of the investigation, the level and rate of decrease of the restoring seal force were recorded over test periods of one and two months. The seal temperature was set to 35 °C, 75 °C, 100 °C, 125 °C, and 150 °C, respectively. A direct correlation was observed between the temperature of the seal, the level of the restoring force after compressing and heating the seal, and the drop-off characteristics of the restoring force. It was found that in our test device the force level immediately after reaching the respective temperature is lower for higher seal temperatures, while the drop rate of the restoring force is higher. This paper describes the experimental setting and discusses first results in comparison with our long-term discontinuous measurements. T2 - 21st International Symposium on the Packaging and Transportation of Radioactive Materials - PATRAM 2025 CY - San Antonio, TX, USA DA - 27.07.2025 KW - Temperature-Dependent Performance KW - Extended Interim Storage KW - Long-Term Safety Assessment KW - Metal Seal Aging KW - Restoring Force Degradation PY - 2025 AN - OPUS4-63891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Kotil, Leyla A1 - Matjacic, Lidija A1 - McMahon, Greg A1 - Bernicke, Michael A1 - Bernsmeier, Denis A1 - Kraehnert, Ralph A1 - Hertwig, Andreas A1 - Hodoroaba, Vasile-Dan T1 - Morphological and Chemical Nanoscale Analysis of Mesoporous Mixed IrOx-TiOy Thin Films as Electrode Materials N2 - orous films play an important role particularly in energy applications like photovoltaics, electrolysis or batteries. Thin film properties such as thickness, chemical composition, crystallinity of the framework, and porosity define the activity of the porous films. The accurate morpho-chemical characterisation of mesoporous thin films is a challenging analytical task which requires the consideration of new analytical approaches based on the combination of data of different methods able to address the structure and chemical composition at the nanoscale. In this contribution we characterise thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with Energy-Dispersive X-ray Spectroscopy (EDS) at an SEM applied in a dedicated “thin film analysis” approach (1). Thus, the film mass deposition, film thickness and the film density can be determined. Further, by dividing the measured film density to an assumed (theoretical) metal oxide framework (skeletal) density, the thin film porosity can be extracted, too. In order to assess the homogeneity of the thin film properties like the chemical composition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Auger Electron Spectrometry are applied in the depth profiling mode, so that possible in-depth gradients are detected. Lateral inhomogeneities in the chemical composition and structure of the thin mesoporous films are also identified by applying the same methods in the line-scan or mapping mode, which can be further combined with in-depth sputtering for 3D information. The role of the spatial resolution of the analytical methods considered, which can go down well below 100 nm, will be highlighted. KW - Mesoporous thin films KW - Imaging KW - TiO2 KW - Ir oxid KW - Auger electron spectroscopy KW - ToF-SIMS KW - SEM/EDX PY - 2024 DO - https://doi.org/10.1093/mam/ozae044.252 VL - 30 IS - Supplement 1 SP - 541 EP - 542 PB - Oxford University Press (OUP) AN - OPUS4-61185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbricht, Jürgen T1 - Cyclic loading and creep-fatigue performance of P92 N2 - 9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in power plants due to their excellent creep and oxidation resistance. The growing share of renewable energy sources in power generation forces many of these plants into more flexible operation with frequent load shifts or shutdowns. These cyclic operation profiles constitute a major lifetime issue. The present contribution reports on current findings obtained in a multidisciplinary project which combines cyclic mechanical and cyclic oxidation testing of different 9-12% Cr grades with detailed microstructural analyses. Mechanical analyses are carried out on P92 and P91 steel grades to give an overview of softening phenomena and lifetimes obtained in isothermal cyclic loading (low cycle fatigue, LCF), non-isothermal cyclic loading (thermo-mechanical fatigue, TMF), and service-like combinations of creep and fatigue periods. Complementary microstructural investigations by scanning and transmission electron microscopy plus EBSD are used for phase identification, substrate/oxide interface characterization and quantification of the microstructure evolution under cyclic conditions. T2 - 44th MPA-Seminar CY - Leinfelden/Stuttgart, Germany DA - 17.10.2018 KW - Ferritic-martensitic steels KW - Fatigue KW - Creep-fatigue PY - 2018 AN - OPUS4-47116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zaghdoudi, Maha T1 - Overview of ongoing long-term ageing investigations on elastomer seals N2 - At the Bundesanstalt für Materialforschung und -prüfung (BAM) in Division 3.4 Safety of Storage Containers, one of our tasks is to evaluate the safety of containers designed for disposal of low and intermediate radioactive waste. As such containers might be transported before and stored until disposal, safe enclosure of the radioactive inventory is important for this time span. Elastomer O-rings are widely used as barrier seals in these containers. Thus, as for many other applications, an understanding of the practical effects of ageing degradation on elastomer seals during long-term exposure is mandatory for predicting the lifetime of such components. According to a long-term test programme on three kinds of rubbers (EPDM and FKM (relevant for application), HNBR (for comparison)), over several years we have studied the degradation and the change of mechanical properties (e.g. hardness, strain at break) at four different ageing temperatures (75 °C, 100 °C, 125 °C and 150 °C) as well as the change of sealing properties. Continuous and intermittent compression stress relaxation (CSR) measurements were performed in order to investigate the respective contribution of crosslinking and chain scission to the observed degradation effects. Thus, the degradation kinetics and mechanisms could be resolved more clearly. For assessing the seal performance, compression set (CS) and leakage rate measurements were conducted. The experimental results showed that the O-rings remained leak-tight under purely static conditions even when CSR, CS and mechanical properties already indicated far advanced degradation. For this reason, a modified leakage test involving a small and rapid partial decompression of the seal was developed that enabled determining an end-of-lifetime criterion for O-rings with a safety margin for thermal shrinkage and vibrations. T2 - IRC CY - London, UK DA - 03.09.2019 KW - Compression set KW - Continuous compression stress relaxation KW - Intermittent compression stress relaxation KW - Leakage rate PY - 2019 AN - OPUS4-49073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grelle, Tobias A1 - Wolff, Dietmar A1 - Probst, Ulrich A1 - Jaunich, Matthias A1 - Völzke, Holger T1 - Investigation of the time and temperature dependent behavior of metal seals in radioactive waste containers N2 - The Bundesanstalt für Materialforschung und –Prüfung (BAM) runs an investigation program on the long-term behavior of multi-component metal seals. Such seals are used in a wide area of applications including transport and storage casks for spent nuclear fuel and high level radioactive waste. The seal function is mainly based on the compression of the inner helical spring, which generates the necessary seal force to keep the sealing surfaces in close contact. This in turn leads to a plastic deformation of the outer jacket of the seal, comprised of highly ductile aluminum or silver that adapts to the sealing surfaces of cask body and bolted lid, thus providing high Level leak tightness. In Germany, those casks are licensed for Interim storage periods of up to 40 years or more if extended Interim storage would become necessary before a final repository is available. Thus, the sealing performance has to be evaluated, including factors like elevated temperature due to decay heat or mechanical loads due to transport under normal as well as accident conditions. Long-term investigations at BAM have been running over the last nine years to identify and evaluate the seal performance by measuring the remaining seal force, the useable resilience and the leakage rate after various time intervals at temperatures ranging from room temperature up to 150 °C. It was found that the seal force and useable resilience decrease with time and temperature, caused by creep deformation of the outer jacket. In order to obtain an analytical description for the seal behavior and to achieve more information on the material behavior under application conditions a comprehensive investigation program with Focus on aluminum as outer jacket material was launched. The program includes material investigations such as compression and tension creep tests with representative basic materials. An additional test setup allows for the continuous measurement of the remaining seal force at temperatures of up to 150 °C. Furthermore, seal segments are compressed and stored in heating chambers, thus producing segments at different stages of the aging process. The segments are investigated regarding the development of the contact area width, jacket thickness and microstructural changes. This data will be used to develop material models and an analytical description of the time and temperature dependent long-term sealing behavior. This paper explains the current status of gained test results and modelling approaches and closes with an outlook to the future Project plans. T2 - ASME 2018 Pressure Vessels and Piping Conference CY - Prague, Czech Republic DA - 15.07.2018 KW - Metal seal KW - Creep KW - Long-term behavior PY - 2018 SP - PVP2018-84584, 1 EP - 6 AN - OPUS4-46110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zaghdoudi, Maha T1 - Analysis of heterogeneous ageing of hnbr o rings N2 - 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 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 measurements across the section of O-rings. Oxidation profiles were determined by applying the model of Wise et al. to the IRHD experimental results. T2 - The 2023 Postgraduate Seminar - Advanced Structured Materials CY - Barcelona, Spain DA - 20.02.2023 KW - HNBR KW - Heterogeneous ageing KW - IRHD KW - FTIR KW - CSR PY - 2023 AN - OPUS4-57057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Aging investigations of metal seals used in containers for interim storage of spent fuel N2 - In Germany dual purpose containers with double lid systems are used for the transport and storage of spent fuel and high level radioactive waste. The bolted lids are equipped with metal seals (e.g. Helicoflex®) to ensure the safe enclosure of the inventory for the required time period. The used metal seals have a layered structure consisting of three components. In the center a helical spring is positioned that is surrounded by two C-shaped jackets. The helical spring is mainly responsible for generation of the required restoring force. The inner jacket is made of stainless steel and homogenizes the restoring force generated by the helical spring. The outer jacket is made of silver or aluminum. Both metals are soft in comparison to the contact partners (lid and container body). During bolting of the lid the seal is compressed between lid and container body. The generated restoring force of the helical spring causes a plastic deformation of the outer jacket which adapts to the surfaces of the lid and the container body. Hence, leakage paths are closed and the sealing function is caused. Typical durations for existing interim storage licenses in Germany are 40 years, but due to the challenges in selection and construction of a final repository it can be expected that they have to be extended to longer periods. An extension of license periods requires knowledge of the long-term behavior of the seals. To meet this challenge long-term investigations have been started at Bundesanstalt für Materialforschung und –prüfung (BAM) in 2009. These tests focus on seals assembled in test flanges which are stored at temperatures ranging from room temperature to 150 °C for accelerated aging. The aged seals are tested repeatedly after certain aging steps and the performance is evaluated in respect to the leakage rate, the remaining seal force, and the useable resilience upon decompression. In this contribution an update on the running investigations in respect to earlier publications (Grelle et al. 2019, Goral et al. 2023) will be given and the implications of the results for resilient long-term safety will be presented. New activities will be addressed and their expected outcome be discussed. T2 - PVP2024, Pressure Vessels & Piping Conference CY - Bellevue, WA, USA DA - 29.07.2024 KW - Metal seal KW - Aging KW - Interim storage PY - 2024 AN - OPUS4-61355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jürgens, Maria A1 - Fedelich, Bernard A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - Thermo-mechanical fatigue behavior of P91/P92 N2 - 9-12% Cr ferritic-martensitic stainless steels are widely used as high temperature construction materials in power plants due to their excellent creep resistance and good oxidation resistance. Creep resistance is considered as the primary parameter in material selection for base-load power plants, but the growing share of renewable energy sources in power generation forces many installations into more "flexible" operation with frequent load reductions and shutdowns. Under cyclic operation of power plants, temperature gradients occur especially in thick-walled components. Locally, these gradients lead to complex time- and temperature-dependent loading scenarios which may result in superimposed creep deformation/damage, creep-fatigue and thermo-mechanical fatigue. The combination of different damage processes may seriously reduce the lifetimes of respective components. A fundamental understanding of the damage evolution in ferritic-martensitic steels under combined static and cyclic loading is therefore required. In the present contribution, the thermo-mechanical fatigue and creep-fatigue behavior of two different 9% Cr steel grades (P91 and P92) was investigated. Standard LCF/TMF-tests as well as near-service loading tests with different hold times have been carried out to study the material behavior of the new loading scenarios. Microstructural investigations help to identify the observed deformation characteristics (like e.g. pronounced softening) and the dominating damage mechanisms under different loads. The test programme is complemented by selected tests on service-aged material which demonstrate possible reactions of older components in existing plants to changes in operation profiles. In a next step, the experimental results will be used for parameter identification of a deformation and lifetime model to predict the material behavior. T2 - LCF08 CY - Dresden, Germany DA - 27.06.2017 KW - Near-service testing KW - Power plant KW - Ferritic-martensitic steels KW - P91 KW - P92 KW - Thermo-Mechanical Fatigue PY - 2017 SN - 978-3-9814516-5-8 VL - 2017 SP - 101 EP - 105 PB - DVM CY - Berlin AN - OPUS4-42268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Low temperature properties of rubber seals N2 - Understanding the failure mechanisms that lead to leakage of rubber seals at low temperatures is important. Rubber properties are highly temperature dependent. Changes in behaviour at low temperatures can result from the rubber-glass transition and for some rubbers by partial crystallisation. Experimental results on the low temperature behaviour of different rubber seals were discussed to help understand seal failure processes. T2 - Rubber in Engineering Group (RIEG) webinar an Elastomers at Low Temperatures CY - Online meeting DA - 11.09.2020 KW - Low temperature KW - Rubber seal KW - Compression set KW - Glass transition PY - 2020 UR - https://www.iom3.org/rubber-engineering-group/event/elastomers-low-temperatures AN - OPUS4-51306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sagradov, Ilja T1 - Long-term tests on metal seals using continuous force measurement in compressed state N2 - In Germany, spent fuel and heat generating radioactive waste is stored in casks for transport and storage (DPCs). The storage licenses were granted for up to 40 years. Due to the delay in identifying a final repository site for such radioactive waste, the storage periods are to be extended significantly. The objective of our research work is to collect additional material data for metal seals in order to be able to better assess the long-term safety of the sealing system of the casks for a period of up to 100 years. A principal safety consideration for the DPCs is the long-term performance of bolted lid sealing systems utilizing metal seals to ensure the safe enclosure of the radioactive inventory during interim storage. To assess the sealing behavior, it is necessary to examine the aging-dependent residual restoring force for the metal seals and the usable resilience. By investigating the change in these values as a function of time and temperature, further insight can be gained into the assessment of long-term safety for extended interim storage. In the present study, the restoring force of metal seals with an outer aluminum jacket and a torus diameter of 9.9 mm was measured continuously. For this purpose, a specially designed device equipped with a load cell was used under isothermal conditions. As part of the investigation, the level and rate of decrease of the restoring seal force were recorded over test periods of one and two months. The seal temperature was set to 35 °C, 75 °C, 100 °C, 125 °C, and 150 °C, respectively. A direct correlation was observed between the temperature of the seal, the level of the restoring force after compressing and heating the seal, and the drop-off characteristics of the restoring force. It was found that in our test device the force level immediately after reaching the respective temperature is lower for higher seal temperatures, while the drop rate of the restoring force is higher. This paper describes the experimental setting and discusses first results in comparison with our long-term discontinuous measurements. T2 - 21st International Symposium on the Packaging and Transportation of Radioactive Materials - PATRAM 2025 CY - San Antonio, TX, USA DA - 27.07.2025 KW - Long-Term Safety Assessment KW - Extended Interim Storage KW - Metal Seal Aging KW - Restoring Force Degradation KW - Temperature-Dependent Performance PY - 2025 VL - 2025 SP - 1 EP - 10 CY - Indianapolis, IN, USA AN - OPUS4-63881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Operando electrochemical spectroscopic ellipsometry: Material properties of highly active mesoporous IrO IrOxfilms revealed under realistic OER conditions N2 - Rising energy demand and the impending climate change require the development of a sustainable, fossil-free fuel and chemical production on a global scale. Hydrogen production via water electrolysis will be a fundamental cornerstone in this endeavor. The activity and stability of respective electrode coatings strongly depends on the coating's properties, i.e. phase composition, crystallinity, electrical conductivity, accessible surface, wettability and many other factors. The key to the development of improved catalysts is a better understanding of the relations between their performance, stability and physicochemical properties. However, those relations can be complex, and are strongly influenced also by the reaction environment. Hence, operando analysis of the catalyst material during catalysis at realistic potentials and current densities is highly desirable. Yet, many analytical techniques cannot be applied in liquid environments at realistic potentials and current densities. We propose environmental ellipsometric analysis in a dedicated electrochemical flow cell as a new method to evaluate gas evolution reactions operando under realistic working conditions. Figure 1 illustrates schematically the developed technique. Key factors to success are highly active model-type catalysts with template-controlled porosity, a suitable sample environment, a deep understanding of the spectroscopic method and respective model development, as well as concise cross validation with numerous other analytical techniques. The method was developed and validated by analyzing a calcination series (300 - 600°C) of mesoporous templated IrOx films ex-situ and operando under oxygen evolution reaction (OER) conditions. The employed environmental electrochemical spectroscopic ellipsometric analysis (ECSE) revealed during OER the change of optical and electronic properties, i.e. the dielectric functions (real ε1 and imaginary part ε2), electrical and electronic properties such as resistivity (ρ) and band-to-band transitions (p-d band transitions). Film thickness and porosity were validated by means of scanning electron microscopy (SEM), X-ray reflectometry (XRR) or ellipsometric porosimetry (EP), electrical and electronic properties by means of conductivity measurements, X-ray photoelectron spectroscopy (XPS) or UV-Vis-NIR absorption spectroscopy. The electronic structures of the catalysts from valence electron energy loss spectra (VEELS) derived from the real (ε1) and imaginary part (ε2) of the dielectric function from SE measurements reveal a direct correlation with electrochemical activities in OER. In the presentation reversible and irreversible potential-dependent changes of the catalyst properties during operation will be discussed along with the dynamics of gas formation, transport and dissolution T2 - E MRS 2021 SPRING MEETING CY - Online meeting DA - 31.05.2021 KW - Spectroscopic ellipsometry KW - Ectrocatalysis KW - Oxygen evolution reaction KW - Mesoporous iridium oxide films KW - Non-destructive operando analysis PY - 2021 AN - OPUS4-52929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaunich, Matthias T1 - Long-Term Performance of Elastomer seals - From Aging Tests to Lifetime Estimations N2 - 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 cask 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 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 time-temperature 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 discussed. T2 - ASME Pressure Vessels and Piping Conference 2018 CY - Prague, Czech Republic DA - 15.07.2018 KW - Seal KW - Rubber KW - Degradation PY - 2018 AN - OPUS4-45923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -