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The development of a robust hydrogen infrastructure poses challenges to materials exposed to high pressurized hydrogen environments. Polymeric materials, which are expected to perform as seals, gaskets, O-rings, hoses among other applications face high risk of damage due to rapid gas decompression (RGD) which might cause operational safety issues. In this study, we intend to assess the effects of a high pressurized hydrogen environment on carbon black filled (CB) elastomers. The materials were exposed to 100 MPa hydrogen atmosphere at room temperature and at 85°C. Ex-situ characterization was performed during the first 30 minutes after decompression and repeated two days after the exposure when total gas desorption has taken place. The physical and mechanical characteristics of the materials were determined by means of density and volume change, hardness and tensile tests, and dynamic mechanical analysis.
Intermittent microplasticity via dislocation avalanches indicates scale-invariance, which is a paradigm shift away from traditional bulk deformation. Recently, we have developed an experimental method to trace the spatiotemporal dynamics of correlated dislocation activity (dislocation avalanches) in microcrystals (Phys. Rev. Mat. 2 (2018) 120601; Phys. Rev. Mat. 3 (2019) 080601). Here we exploit the temperature sensitive deformation of bcc metals. A marked change of the slip-size distribution is observed in the studied microcrystals, with increasingly small event-sizes dominating with decreasing temperature. This shows how a reduction in thermal energy increasingly suppresses the length-scale of dislocation avalanches, indicating how long-range correlations become gradually limited to the scale of the lattice. Our results further show that the stress-strain response is composed of strain-increments that are either thermally activated or essentially athermal. Temperature-dependent small-scale testing in combination with state-of-the-art discrete dislocation dynamics (DDD) simulations of Nb microcrystals are used to reveal these insights.
Quenching a metallic liquid sufficiently fast can give rise to an amorphous solid, typically referred to as a metallic glass. This out-of-equilibrium material has a long suite of remarkable mechanical and physical properties but suffers from property deterioration via structural relaxation. As a function of time, relaxation may indeed constitute significant threads to safe applications. Consequently, relaxation of glasses has a long history across different amorphous materials and typical characterization methods promote a picture of gradually evolving and smooth relaxation, as for example obtained from mechanical spectroscopy. However, the true structural dynamics and underlying mechanisms remain far from understood and have hampered a physically informed atomic-scale picture of transport and physical aging of glasses.
Here we exploit the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS) and resolve an unprecedented spectrum of short- and long-term relaxation time scales in metallic glasses. Conducted across temperatures and under the application of stress, the results reveal anything else than smooth aging and gradual energy minimization. In fact, temporal fluctuations persist throughout isothermal conditions over several hundred thousand of seconds, demonstrating heterogeneous dynamics at the atomic scale. In concert with microsecond molecular dynamic simulations, we identify possible mechanisms of correlated atomic-scale dynamics that can underly the temporal fluctuations and structural decorrelations. Despite temporally heterogeneous, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law emerges. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the structural fast and slow relaxation modes as well as a true microstructure in metallic glasses.
Inspired by the ability to track atomic-scale dynamics with x-ray photon correlation spectroscopy (XPCS)1 and recent results of long-term atomistic simulations on material transport2, we reveal here an unprecedented spectrum of short- and long-term relaxation dynamics. Tracked along a 300 000 s long isotherm at 0.98Tg, a Zr-based bulk metallic glass exhibits temporal fluctuations that persist throughout the entire isotherm, demonstrating a continuous heterogeneous dynamics at the probed length scale. In concert with microsecond molecular dynamic simulations, we identify intermittent cluster dynamics as the origin for temporal signatures in the corresponding intensity cross-correlations. Despite temporally heterogeneous aging, the Kohlrausch-Williams-Watts functions is well suited to capture the average intermediate relaxation time regime, but at very long time scales an asymptotic power-law better describes the data. This indicates anomalous diffusion and gives overall strong evidence for temporal fractional diffusion in metallic glasses. We discuss these results in terms of the underlying structural fast and slow relaxation modes and their manifestation in the temporal form of the structural decorrelations.
Metallic glasses (MGs) are disordered solids that exhibit a range of outstanding mechanical, thermomechanical, and functional properties. Whilst being a promising class of structural materials, well-defined and exploitable structure-property relationships are still lacking. This offsets them strongly from the crystalline counterparts, for which length-scale based property determination has been key for decades.
In recent years, both atomistic simulations and experiments have nurtured the view of heterogeneities that manifest themselves either as a structural partitioning into well-relaxed percolated network components and more frustrated domains in atomistic simulations, or as spatially-resolved property fluctuations revealed with atomic force microscopy. These signatures depend sensitively on the processing history and likely reflect emerging medium-range order fluctuations at the scale of 1-10 nanometers.
Here we demonstrate and discuss the emergence of spatially resolved property fluctuations at length scales that are one to two orders of magnitude larger. Such long-range decorrelation length scales are hard to reconcile in a monolithic glass but may offer the perspective of experimentally easy-to-access length-scale based structure-property relationships. Whilst long-range property fluctuations can be seen in both the plastic and elastic response, we focus here on high-throughput elastic nanoindentation mapping across the surface of a Zr-based model glass. After a deconvolution of surface topography and curvature effects, the spatially-resolved elastic response reveals an elastic microstructure with a correlation length of ca. 150-170 nm. Analytical scanning-transmission electron microscopy (STEM) is used to link the elastic property fluctuations to the chemistry and structure of the MG. In concert, nano-elastic mapping and STEM suggests that structural variations in the glass are responsible for the unexpectedly large length scales. We discuss these findings in terms of the materials processing history and the perspective of exploiting nanoindentation-based spatial mapping to uncover structural length scales in atomically disordered solids.
Compatibility of welded austenitic stainless steel (316L) tube for green hydrogen applications
(2024)
The increase in the energy demand and the need to comply to net zero carbon regulations, as per the Paris 2015 climate agreement by 2050, has necessitated the urgency to consider hydrogen as alternative energy carrier. Moreover, hydrogen interaction with metals tend to cause degradation of the mechanical properties in terms of the ductility of the materials. More concern is on the weldment and repair of tubes or pipelines of hydrogen transportation and storage systems. In this study, the heat inducted weld tubes of the cold drawn and annealed austenitic stainless steel (316L) were investigated by slow strain rate test. To achieve the most realistic component-related testing, hollow tube specimens have been fabricated from 1/2-inch Swagelok pipes filled with internal gaseous hydrogen or inert air for reference. The hydrogen concentration measurement is undertaken before and after the autoclave high-pressure pre-charging of the specimens using carrier gas hot extraction. SEM analysis was used to carry out fractographic analysis to determine the crack initiation sites, crack size and was compared for the base material and heat affected zone influence in the gaseous hydrogen. The effect of hydrogen on the material compatibility of the welded austenitic stainless steel is assessed and compared to none-welded tubes tested in defined testing parameters that contribute to Hydrogen Assisted Cracking. A better understanding on the impact of weldment on the structural integrity for stainless steel is elucidated for green hydrogen application.
Early detection of fatigue cracks and accurate measurements of the crack growth play an important role in the maintenance and repair strategies of steel and composite structures exposed to cyclic loads during their service life. Commonly used non-destructive techniques such as strain gauges, clip gauges, ultrasound, etc. used for detection and monitoring of fatigue damage are contact-based and perform local measurements. In addition, complex full-field techniques are commonly investigated, such as digital image correlation (DIC) and infrared thermography (IRT). In this work, a specific implementation of IRT, called lock-in IRT, is implemented for fatigue damage detection. This technique evaluates the thermal stress response of test specimens, specifically focusing or “locking-in” on the frequency of applied cyclic loads. Three different test scenarios are presented.
First, a section of a wind turbine rotor blade made of a glass fibre reinforced plastic (GFRP) shell structure under cyclic load was examined with Lock-In IRT along with DIC. The primary advantage of Lock-In IRT in this test setup was that it required no sample preparation, as compared to the painting and speckle pattern required for DIC. In the frequency domain, specifically the frequency of applied cyclic load, it was possible to extract local directional inhomogeneous loading within the shell structure due to progressive damage, confirmed with the deformation obtained from DIC results.
Second, thick welded specimens made of structural steel S355 were subjected to multiple NDT methods such as strain gauges, crack luminescence penetration (developed specifically at BAM), ultrasound, and IRT, with the aim of investigating the ability of each technique to detect fatigue damage initiation as early as possible in the total fatigue life of the specimen. Amongst the range of implemented techniques, Lock-In IRT provided the first indication of fatigue crack initiation at the weld toe of the specimens. This was validated with the other techniques as well as fractography.
Third, steel S355 specimens used to manufacture offshore wind turbine monopiles were tested. The specimens were extracted from a plate that was submerged in a marine environment, resulting in a corroded surface with corrosion pits. These specimens were subjected to cyclic tensile loads without removing the corrosion pits. The fatigue tests were monitored using IRT in a special full-field capturing setup that enables both sides of the specimen to be examined with one IRT camera. This allowed the entire pitted surface to be monitored for fatigue damage initiation at the same time. With the implementation of Lock In IRT, the surface stress distribution could be captured (the stress concentration at the pits), and fatigue crack initiation could be detected and linked with specific corrosion pits.
Passive infrared thermography as an inspection tool for operational wind turbine rotor blades
(2024)
The growing wind energy infrastructure presents a significant challenge in the maintenance and operation of wind turbines (WT) and their intricate components. An important aspect of WT maintenance is the inspection of wind turbine rotor blades (WTB) to ensure the overall health and safety of the turbine. This inspection process involves both visual and mechanical examinations of the blades to identify any indicators of damage or wear that could compromise their performance and, consequently, the structural integrity of the entire WT system. The complexity of WTBs is compounded by their ever-expanding dimensions, exceeding 100 meters in length for 16 MW WT systems, and their multi-material composition. Within this context, passive infrared thermography emerges as a potential alternative to conventional contact- or proximity-based inspection methods. Unlike active thermography, passive thermography uses solar radiation and ambient temperature variation for thermal contrast, eliminating the need for traditional heat lamps, flash, or laser-based techniques.
A novel inspection method has been developed to semi-autonomously assess wind turbine blades (WTBs) while the wind turbine (WT) is operational, from ground level. This approach leverages optimal thermal contrast, which depends on prevailing weather conditions during field measurements, enabling the visualization of both external and internal features of the WTBs through post-processing techniques. In this study, thermal data obtained through passive thermography is compared with contemporaneous visual imagery to definitively classify observed features in thermal images as either surface or sub-surface features. This analysis, coupled with corresponding weather conditions, provides valuable insights into the capabilities and limitations of the inspection technique. Additionally, finite-element-based (FE) thermal simulations of a WTB section are employed to parametrically assess the influence of weather conditions, beyond those observed during field measurements, based on a validated model.
In addition, the thermal images also consist of thermal signatures of leading-edge turbulence due to possible leading-edge erosion in WTBs. These are primarily vortices, and their shape and size depend on the morphology of the damage as well as the rotational speed of the WTBs. The inspections are accompanied by automatic data evaluation of the thermal signatures. To improve the precision of erosion damage identification, a fully convolutional network (FCN) is employed, trained, and tested using over 1000 annotated thermographic blade images. Additionally, the study introduces strategies for grouping smaller damage indications and simplification rules based on realistic thermal imaging resolutions. As leading-edge erosion could potentially lead to annual energy production (AEP) losses, this technique could prove to be a powerful tool in establishing the presence of damage and the resulting AEP loss.
Parameter studies are a common step in selecting process parameters for powder bed fusion of metals with laser beam (PBF-LB/M). Density cubes manufactured with varied process parameters exhibit distinguishable surface structures visible to the human eye. Industrial visual in-situ monitoring systems for PBF-LB/M currently have limited resolution and are incapable of reliably capturing differences in the surface structures. For this work, a 65 MPixel high resolution monochrome camera is integrated in an industrial PBF-LB/M machine together with a high intensity led bar. Post-exposure images are taken to analyze differences in light reflection on the specimen’s surface. The grey level co-occurrence matrix is used to quantify the in-situ measured visual surface structure of nickel-based super alloy IN939 density cubes. The properties of the grey level co-occurrence matrix correlate to the energy input and resulting porosity of specimens. Low energy samples with lack of fusion flaws show an increased contrast in the grey level co-occurrence matrix compared to specimens with an optimal energy input. The potential of high-resolution images as reference data in in-situ process monitoring in PBF-LB/M is discussed.
The application of an external magnetic field has been found to significantly mitigate the porosity ratio in laser beam welded joints of AlMg3 aluminum alloy. To investigate the suppression mechanism, a 3D transient multi-physics coupled numerical model of laser beam welding (LBW), including laser propagation, laser-material interaction, and magnetohydrodynamic effects, has been developed to calculate the keyhole dynamics and weld pool behaviors during the welding process. The induced time-averaged Lorenz force is directed downward. Under the effects of the external magnetic field, the fluid flow pattern and the weld pool profile are both affected. The keyhole geometry reconstruction algorithm is proposed to calculate the keyhole diameter and its fluctuation, which is used to evaluate the keyhole stability. The results indicate that the oscillating magnetic field does not affect keyhole stability obviously in the LBW of aluminum alloy. Moreover, an electromagnetic expulsive force is induced on the bubble because of the time-averaged downward Lorentz force. This electromagnetic expulsive force can accelerate the bubble escape speed considerably. An analytical model is developed for investigating the bubble escape window, which shows that the bubble escape window is expanded by 45% under the effect of the external magnetic field. The calculated results based on the developed model agree well with the experimental results.
Advanced light weight applications like aircrafts and wind turbine blades are made of fibre reinforced plastics (FRP) with continuous fibre reinforcement and must withstand a high thermo-mechanical cyclic loading. The quality of the fibre matrix interface has a high impact on the fatigue life and was continuously improved over the years since the 50th. The fatigue life of glass fibre reinforced plastics (GFRP) used in aircraft industry is 10 to 100 times higher compared to glass fibre non crimp fabrics used for wind turbine blades.
To assure a constant and reliable high quality and strength of reinforcement fibres, synthetic fibre production is state of the art (CF, GF). There is a need for recycling GFRP and CFRP waste due to the upcoming use. Pyrolysis and solvolysis are more expensive than the mechanical route however enable a more sustainable recycling. Natural fibres and recycled synthetic fibres have a high scatter in quality and strength. Hence it is a challenge to optimize the production / recycling processes to get a reliable quality for any demanding (second life) application.
Chemical routes for using renewables resources and recycling, is going to be a good approach especially for polymer-matrix systems to get 100% quality (back) compared to the state of the art.
Finally, a proper design, life-time extension and repair is preferable to recycling to keep the carbon footprint as low as possible.
The Modified Varestraint Transvarestraint test is a local variant of the globally used Varestraint test. With these tests, measuring solidification cracking susceptibility as a function of welding parameters is possible. A wide range of welding parameters for four high-strength steel filler wires, including three solid wires and one-flux cored metal wire, were tested. All wires do show a very low solidification cracking susceptibility, regardless of the paramaters. On a low level, it could be shown that solidification cracking susceptibility increases with heat input and welding speed.
Testing of highly restraint high-strength fillet welds with regards to solidification cracking susceptibility. The Controlled Thermal Severity test was used to apply a high amount of strain to solidifying welds. Test welds were cut and observed under an optical light microscope. A clear positive correlation between restraint intensity and measured crack sizes, as well as heat input and measured crack sized could be observed.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Contemporary steels creep-resistant steels like the 13CrMoV9-10 are used as thick plates e.g., for applications in hydrocrackers. The large plate thickness requires high efficiency welding processes like submerged arc welding (SAW) and a mandatory post weld heat treatment (PWHT). The PWHT-parameters stem from a combination of empirical knowledge and traditional experiments on free shrinking (FS) welds. In that connection, the formation of so-called stress-relief cracking (SRC) must be anticipated. The SRC susceptibility of a welded component is a complex combination and interaction of com-ponent specific, thermal, and metallurgical factors. Many of which have to date not been conclusively researched. For example, it is well known that SRCs develop during PWHT due to formation and growth of carbides on prior austenite grain boundaries, resulting in a significant hardness increase (secondary hardening) and toughness decrease. This leads to a high SRC susceptibility of the coarse grain heat-affected zone (CGHAZ) of the last weld bead during PWHT. This is intensified in case of high residual stresses from the component-specific, structurally induced stiffness. In combination with multi-layer welding this leads to a multiaxial stress distribution. Nonetheless, the combined effect of PWHT and high-residual stresses on the SRC formation is merely unknown. For that reason, this study presents the effect of different heating rates in conjunction with a certain component stiffness. For that reason, SAW joints of 13CrMoV9-10 steel were investigated under FS and defined external restraint condition.
Based on the initial call in March 2024, an update time-frame is introduced on the working plan for a comprehensive review paper series on joining and welding technologies for the manufacturing of components and parts used in sustainable energy generation, conversion, and transport with focus on hydrogen and wind energy.
As energy carrier of the future, green hydrogen can make a decisive contribution to a sustainable energy supply. In Europe concrete plans for a hydrogen pipeline grid already exist, as the so called “European Hydrogen backbone”. As building a completely new pipeline grid is economically not justifiable, a dual-way strategy of repurposing natural gas (NG) pipelines and newly built pipelines is intended. Long distance pipeline grids require regular maintenance and repairs. In that conection, for natural gas (NG) pipelines in-service welding is state of the art. Concepts such as hot-tapping (drilling into pressurized pipelines) and “stoppling” (sealing off pipeline sections after installing bypasses or pressure relieves) allow the repair of damaged pipeline sections or the installation of new branches without shutting the pipeline down. The EIGA 121/14 guideline already pointed out in 2014 that “a hydrogen hot-tap shall not be considered a routine procedure”. This shows that the determination of the transferability of these repair concepts to hydrogen pipelines is of utmost importance. Due to the degrading effects of hydrogen on mechanical proper-ties, commonly referred to as “hydrogen embrittlement” it is necessary to understand and investigate the occurring effects. In the special case of repair welding on in-service hydrogen pipelines an increased hydro-gen uptake due to a large heat input and microstructural changes in the material needs to be considered. For this reason, this paper gives an overview on existing weld repair concepts and its risks and limitations in terms of hydrogen absorption and possible embrittlement effects when transferred to hydrogen pipelines. The complexity lies in a large variety of materials (low alloyed steels), pipeline diameters and corresponding welded joints. The material compatibility of materials in used (repurposed NG-pipelines) and new condition must be investigated. Particularly for repurposed/used pipelines the effect of a pre-matured/corroded inner surface and sometimes insufficient documentation of the material “history” needs to be considered. An overview on ongoing and completed R&D-projects with respect to repair concepts for hydrogen pipelines and hydrogen effects on pipeline materials is given.
Long-term dry interim storage may adversely affect the mechanical properties of spent fuel rods, possibly resulting in a reduced resilience during handling or transport after storage. The cladding is the first barrier for the spent fuel pellets. An established method for characterising the cladding material is the ring compression test (RCT), in which a small, cylindrical sample of the cladding tube is subjected to a compressive load. Radial hydrides may precipitate in zirconium-based alloys (Zircaloy) under pre-storage drying and during slow cooling, which result in embrittlement of the cladding material and eventually a possible sudden failure of cladding integrity under additional mechanical loads. The focus of the presented research is on the development of appropriate nu-merical methods for predicting the mechanical behaviour and identification of limiting conditions to prevent brittle fracture of Zircaloy claddings. A modelling approach based on cohesive zones is ex-plained which is able to reproduce the propagation of cracks initiated at radial hydrides in the zir-conium matrix. The developed methods are applied to defueled samples of cladding alloy ZIRLO®, which were subjected to a thermo-mechanical treatment to reorient existing circumferential hy-drides to radial hydrides. A selected sample showing sudden load drops during a quasi-static ring compression test is analysed by means of fracture mechanics for illustrative purposes. Based on the developed fracture mechanics approach, not only the deformation behaviour but also the fail-ure behaviour of irradiated as well as unirradiated Zircaloy claddings with radial hydrides under RCT loading conditions can be adequately described.