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The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures.
The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures.
Laser Powder Bed Fusion (PBF-LB/M) is a layer wise metal additive manufacturing (AM) technology, which enables significant advancements of component design, leading to potential efficiency and performance improvements. However, the thermal cycles inherent to the process comprising large localized thermal gradients and repeated melting and solidification cycles leads to the generation of high magnitude residual stresses. These residual stresses can be detrimental both during manufacturing of components and in subsequent application. Therefore, a deep understanding of the influence of process parameters on the residual stresses are crucial for efficient manufacturing and safe application. The experimental characterization of these residual stresses is therefore crucial and can provide a reliable baseline for simulations of both the process and applications.
Diffraction-based methods for residual stress analysis using penetrating neutrons and high energy X-rays enable non-destructive spatially resolved characterization of both surface and bulk residual stresses. However, the unique microstructural features inherent to the process can challenge some of our assumptions when using these methods. These challenges include the determination of a stress-free reference, the use of correct elastic constants (both SCEC and DEC) and the influence of surface roughness, texture, and porosity on residual stresses.
This presentation will detail recent insights and recommendations for the characterization of residual stresses in a range of PBF-LB/M metallic alloys (Fe, Ni, Al and Ti)
The determination of residual stress in additively manufactured materials is a challenge, even after decades from the establishment of the basics of residual stress analysis. This is due to the peculiar microstructure of such materials. In fact, researchers have discovered that conventional methods for the determination of RS in materials do not properly work for AM materials. In this tutorial, the basics of RS analysis will be explained, together with the basics of AM manufacturing techniques. The microstructure of the peculiar materials (AM) dealt with here will be elucidated. Successively, the necessary modifications to the conventional approaches to RS analysis will be explained and case studies will be displayed, for the attendant to touch with hands the peculiarities of the approaches. Finally, a few experimental and theoretical tips will be given on dos and don’ts for a correct determination of RS in AM materials.
Due to the advantages of Laser Powder Bed Fusion (PBF-LB), i.e., design freedom and the possibility to manufacture parts with filigree structures, and the considerable amount of knowledge available for 316L in its conventional variant, the mechanical behavior, and related microstructure-property relationships of PBF-LB/316L are increasingly subject of research. However, many aspects regarding the - application-relevant - mechanical behavior at high temperatures are not yet fully understood. Here, we present the results of an experimental study on the LCF behavior of PBF-LB/316L featuring a low defect population, which makes this study more microstructure-focused than most of the studies in the literature. The LCF tests were performed between room temperature (RT) and 600 °C. The mechanical response is characterized by strain-life curves, and hysteresis and cyclic deformation curves. The damage and deformation mechanisms are studied with X-ray computed tomography, and optical and electron microscopy. The PBF-LB/M/316L was heat treated at 450 °C for 4 h, and a hot‑rolled (HR) 316L variant with a fully recrystallized equiaxed microstructure was tested as a reference. Besides, selected investigations were performed after a subsequent heat treatment at 900 °C for 1 h. The PBF-LB/316L exhibits higher cyclic stresses than HR/316L for most of the fatigue life, especially at room temperature. At the smallest strain amplitudes, the fatigue lives of PBF-LB/M/316L are markedly shorter than in HR/316L. The main damage mechanisms are multiple cracking at slip bands (RT) and intergranular cracking (600 °C). Neither the melt pool boundaries nor the gas porosity have a significant influence on the LCF damage mechanism. The cyclic stress-strain deformation behavior of PBF-LB/M/316L features an initial hardening followed by a continuous softening. The additional heat treatment at 900 °C for 1 h led to decreased cyclic stresses, and a longer fatigue life.
The determination of residual stress in additively manufactured materials is a challenge, even after decades from the establishment of the basics of residual stress analysis. This is due to the peculiar microstructure of such materials. In fact, researchers have discovered that conventional methods for the determination of RS in materials do not properly work for AM materials. In this tutorial, the basics of RS analysis will be explained, together with the basics of AM manufacturing techniques. The microstructure of the peculiar materials (AM) dealt with here will be elucidated. Successively, the necessary modifications to the conventional approaches to RS analysis will be explained and case studies will be displayed, for the attendant to touch with hands the peculiarities of the approaches. Finally, a few experimental and theoretical tips will be given on dos and don’ts for a correct determination of RS in AM materials.
The experimental determination of residual stress becomes more complicated with increasing complexity of the structures investigated. Unlike the conventional and most of the additive manufacturing (AM) fabrication techniques, laser powder bed fusion (PBF-LB) allows the production of complex structures without any additional manufacturing step. However, due to the extremely localized melting and solidification, internal stress-induced deformation and cracks are often observed. In the best case, significant residual stress is retained in the final structures as a footprint of the internal stress during manufacturing.
Here we report solutions to the most prevalent challenges when dealing with the diffraction-based determination of residual stress in AM structures, in particular the choice of the correct diffraction elastic constants. We show that for Nickel-based alloys, the diffraction elastic constants of AM material significantly deviate from their conventional counterparts. Furthermore, measurement strategies to overcome the hurdles appearing when applying diffraction-based techniques to complex-shaped lattice structures are presented: a) proper sample alignment within the beam, b) the proper determination of the residual stress field in a representative part of the structure (i.e., with an engineering meaning). Beyond the principal stress magnitude, the principal direcions of residual stress are discussed for different geometries and scan strategies, as they are relevent for failure criteria.
We show that the RS in the lattice struts can be considered to be uniaxial and to follow the orientation of the strut, while the RS in the lattice knots is more hydrostatic. Additionally, we show that strain measurements in at least seven independent directions are necessary for the correct estimation of the principal stress directions. The measurement directions should be chosen according to the sample geometry and to an informed choice on the possible strain field (i.e., reflecting the scan strategy).
We finally show that if the most prominent direction is not measured, the error in the calculated stress magnitude increases in such a manner that no reliable assessment of RS state can be made.
The determination of residual stress in additively manufactured materials is a challenge, even after decades from the establishment of the basics of residual stress analysis. This is due to the peculiar microstructure of such materials. In fact, researchers have discovered that conventional methods for the determination of RS in materials do not properly work for AM materials. In this tutorial, the basics of RS analysis will be explained, together with the basics of AM manufacturing techniques. The microstructure of the peculiar materials (AM) dealt with here will be elucidated. Successively, the necessary modifications to the conventional approaches to RS analysis will be explained and case studies will be displayed, for the attendant to touch with hands the peculiarities of the approaches. Finally, a few experimental and theoretical tips will be given on dos and don’ts for a correct determination of RS in AM materials.
Structural health monitoring of hydrogen pressure vessels using distributed fiber optic sensing
(2024)
We report on distributed fiber optic sensing-based monitoring of hydrogen composite overwrapped pressure vessels (COPV) to simultaneously increase the operational lifespan and mitigate maintenance costs. Our approach represents, to the best of our knowledge, the first application of distributed fiber optic sensing for COPV Type IV monitoring, where the sensing fibers are attached to the surface, rather than integrated into the composite material. Specifically, we attach an optical fiber of 50 m to the pressure vessel's surface, covering both the cylindrical and dome sections. We note that our fiber optic sensing technique relies on swept wavelength interferometry providing strain information along the entire length of the optical fiber with high spatial resolution even at the millimeter scale. When the vessel is pressurized, the sensing optical fiber shows a linear strain response to pressure at every position along the fiber. After thousands of load cycles, the vessel finally fails with the optical fiber detecting and precisely localizing the damage in the vessel’s blind dome area. Furthermore, we discuss the potential of state-of-the-art signal processing methods and machine learning for advancing predictive maintenance. This could reduce the number of regular inspections, mitigate premature maintenance costs, and simultaneously increase the vessel’s remaining safe service life. We believe that the structural health monitoring of hydrogen pressure vessels with fiber optic sensors can enhance trust in hydrogen technology contributing to the energy transition in the future.
Laser Powder Bed Fusion (PBF-LB/M) of AISI 316L stainless steel has gained popularity due to its exceptional capacity to produce complex geometries and hierarchical microstructures, which can increase the yield strength while maintaining good ductility. Nevertheless, owing to high thermal gradients encountered during the process, the as printed 316L stainless steel often exhibit microstructural heterogeneities and residual stresses, which can limit its performance in demanding environments. Hence, employing heat treatments which balance the reduction of residual stresses while retaining improved static strength may be beneficial in various scenarios and applications. This study investigates the impact of post-processing heat treatments on the microstructure of 316L stainless steel manufactured via PBF-LB/M, along with its correlation with micro-hardness properties. To this end, 6 different heat treatments, i.e., 450 °C for 4h, 700 °C for 1h, 700 °C for 3h, 800 °C for 1h, 800 °C for 3h, and 900 °C for 1h, were applied to different specimens and Vickers hardness measurements (HV1) were performed in all states. At 800 °C, although the cellular structure appears to be retained, there is an observable increase in cellular size. However, while treatments exceeding 900 °C indicate no significant grain growth compared to other conditions, the cellular structure is entirely dissolved, which leads to a reduced Vickers hardness. The effect of the heat treatments on other microstructural features such as grain size and morphology, melt pool boundaries (MPB), crystallographic texture, chemical segregation, dispersoids and phase stability are also discussed in the present work
The general term additive manufacturing (AM) encompasses processes that enable the production of parts in a single manufacturing step. Among these, laser powder bed fusion (PBF-LB) is one of the most commonly used to produce metal components. In essence, a laser locally melts powder particles in a powder bed layer-by-layer to incrementally build a part. As a result, this process offers immense manufacturing flexibility and superior geometric design capabilities compared to conventional processes. However, these advantages come at a cost: the localized processing inevitably induces large thermal gradients, resulting in the formation of large thermal stress during manufacturing. In the best case, residual stress remains in the final parts produced as a footprint of this thermal stress. Since residual stress is well known to exacerbate the structural integrity of components, their assessment is important in two respects. First, to optimize process parameter to minimize residual stress magnitudes. Second, to study their effect on the structural integrity of components (e.g., validation of numerical models). Therefore, a reliable experimental assessment of residual stress is an important factor for the successful application of PBF-LB. In this context, diffraction-based techniques allow the non-destructive characterization of the residual stress. In essence, lattice strain is calculated from interplanar distances by application of Braggs law. From the known lattice strain, macroscopic stress can be determined using Hooke’s law. To allow the accurate assessment of the residual stress distribution by such methods, a couple of challenges in regard of the characteristic PBF-LB microstructures need to be overcome.
This presentation highlights some of the challenges regarding the accurate assessment of residual stress in PBF-LB on the example of the Nickel-based alloy Inconel 718. The most significant influencing factors are the use of the correct diffraction elastic constants, the choice of the stress-free reference, and the consideration of the crystallographic texture. Further, it is shown that laboratory X-ray diffraction methods characterizing residual stress at the surface are biased by the inherent surface roughness. Overall, the impact of the characteristic microstructure is most significant for the selection of the correct diffraction elastic constants. In view of the localized melting and solidification, no significant gradients of the stress-free reference are observed, even though the cell-like solidification sub-structure is known to be heterogeneous on the micro-scale.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer-wise additive manufacturing process that provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of a diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative lattice plane suitable for residual stress analysis. In this contribution, the selection of a suitable lattice plane family for residual stress analysis is explored. Furthermore, the determination of an appropriate set of diffraction and single-crystal elastic constants depending on the underlying microstructure is addressed.
In-situ loading experiments have been performed at the Swiss Spallation Neutron Source with the main scope to study the deformation behaviour of laser powder bed fused Inconel 718. Cylindrical tensile bars have been subjected to an increasing mechanical load. At pre-defined steps, neutron diffraction data has been collected. After reaching the yield limit, unloads have been performed to study the accumulation of intergranular strain among various lattice plane families.
Quantitative microstructural analysis of XCT 3D images is key for quality assurance of materials and components. In this paper we implement a Graph Convolutional Neural Network (GCNN) architecture to segment a complex Al-Si Metal Matrix composite XCT volume (3D image). We train the model on a synthetic dataset and we assess its performance on both synthetic and experimental, manually-labeled, datasets. Our simple GCNN shows a comparable performance, measured via the Dice score, to more standard machine learning methods, but uses a greatly reduced number of parameters (less than 1/10 of parameters), features low training time, and needs little hardware resources. Our GCNN thus achieves a cost-effective reliable segmentation.
Structural health monitoring of hydrogen pressure vessels using distributed fiber optic sensing
(2024)
We report on distributed fiber optic sensing-based monitoring of hydrogen composite overwrapped pressure vessels (COPV) to simultaneously increase the operational lifespan and mitigate maintenance costs. Our approach represents, to the best of our knowledge, the first application of distributed fiber optic sensing for COPV Type IV monitoring, where the sensing fibers are attached to the surface, rather than integrated into the composite material. Specifically, we attach an optical fiber of 50 m to the pressure vessel's surface, covering both the cylindrical and dome sections. We note that our fiber optic sensing technique relies on swept wavelength interferometry providing strain information along the entire length of the optical fiber with high spatial resolution even at the millimeter scale. When the vessel is pressurized, the sensing optical fiber shows a linear strain response to pressure at every position along the fiber. After thousands of load cycles, the vessel finally fails with the optical fiber detecting and precisely localizing the damage in the vessel’s blind dome area. Furthermore, we discuss the potential of state-of-the-art signal processing methods and machine learning for advancing predictive maintenance. This could reduce the number of regular inspections, mitigate premature maintenance costs, and simultaneously increase the vessel’s remaining safe service life. We believe that the structural health monitoring of hydrogen pressure vessels with fiber optic sensors can enhance trust in hydrogen technology contributing to the energy transition in the future.
Direct energy deposition additive manufacturing technologies that utilize an electric arc have great potential for generating large volume metal components. However, selecting process parameters that yield the desired near net shape design and requested mechanical component behavior is not a trivial task due to the complex relationship between all process parameters and material characteristics. This presentation exemplifies the application of a newly developed solid welding wire doped with TiB to enhance grain refinement in the deposited metal for additive manufacturing based on DED-Arc of high-strength precipitation hardening AlMgSi-aluminum alloys. It is worth noting that the solid wire is the result of our preliminary metallurgical studies on grain refinement in aluminum weld metal.
Consequently, research focuses on the correlation between process parameters and component quality to understand the underlying mechanisms. This is crucial for evaluating a robust process parameter space that yields component quality in line with corresponding standards which are mainly taken from welding technology.
Specifically, we examine component quality by analyzing pore size and distribution, as well as grain morphology. To enhance the mechanical properties of the deposited metal, a post-weld heat treatment was conducted, comprising of solution treatment, quenching, and artificial aging. The study also evaluates the effects of various heat treatment strategies on the final mechanical properties of the material.
To demonstrate the applicability of 3D metal printing of high-strength aluminium alloys, a more complex demonstrator was created. It has been shown that DED-Arc can produce high-volume aluminium parts with the same quality as the corresponding subtractive processing strategy.
Additionally, the entire additive manufacturing chain has been digitally integrated, enabling traceability of all relevant process steps, which is essential for reliable subsequent quality assessment.
Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables.
Various software products for the simulation of industrial X-ray radiography have been developed in recent years (e.g., aRTist 2, CIVA CT, Scorpius XLab, SimCT, Wilcore) and their application potential has been shown in numerous works. However, full systematic approaches to characterise a specific CT system for these simulation software products to obtain a truthful digital twin are still missing. In this contribution, we want to present two approaches to obtain realistic grey values in X-ray projections in aRTist 2 simulations based on measured projections. In aRTist 2, the displayed grey value of a pixel is based on the energy density incident on that pixel.
The energy density is calculated based on the X-ray tube spectrum, the attenuation between source and detector as well as an energy-dependent sensitivity curve of the detector. The first approach presented in this contribution uses the sensitivity curve as a free modelling parameter. We measured the signal response at different thicknesses of Al EN-AW6082 at different tube voltages (i.e., different tube spectra). We then regarded the grey values displayed by these projections as a data regression respectively an optimisation problem and obtained the sensitivity curve that is best able to reproduce the measured behaviour in aRTist 2. The resulting sensitivity curve does not necessarily hold physical meaning but is able to simulate the real system behaviour in the simulation software.
The second approach presented in this contribution is to estimate the sensitivity curve based on assumptions about the characteristics of the scintillation detector (e.g., scintillator material, scintillator thickness and signal processing characteristics). For this approach, a linear response function (linear relationship between the deposited energy per pixel and the resulting grey value) is assumed. If the detector characteristics, which affect the simulated deposited energy, are properly modelled, the slope and offset of the response function to match the measured grey values should be the same for different tube spectra. As the offset is constant and given by the grey values measured at no incident radiation, the slope is the remaining parameter to evaluate the success of the detector modelling. We therefore adapted the detector characteristics by changing the detector setup until the slope was nearly the same for all measured tube spectra. We are aware that the resulting parameters of the scintillator material and thickness might not be the real ones, but with those modelling parameters we are able to simulate realistic grey values in aRTist 2. Both of those approaches could potentially be a step forward to a full systematic approach for a digital twin of a real CT system in aRTist 2.
Sacrifice Few to Save Many: Fire Protective Interlayers in Carbon- Fiber-Reinforced Laminates
(2024)
The fire protection of carbon-fiber-reinforced polymer (CFRP) laminates often relies on flame-retardant coatings, but in some applications, their efficacy may diminish upon direct fire exposure due to rapid pyrolysis. This study introduces an innovative approach by integrating protective interlayers within the laminate structure to enhance the fire resistance. Various materials, including ceramic composite WHIPOX, titanium foil, poly(etherimide) (PEI) foil, basalt fibers, rubber mat, and hemp fibers, were selected as protective interlayers. These interlayers were strategically placed within the laminate layout to form a sacrificial barrier, safeguarding the integrity of the composite. Bench-scale fire resistance tests were conducted, where fire (180 kW/m2) was applied directly to the one side of the specimen by a burner while a compressive load was applied at the same time. Results indicate significant prolongation of time to failure for CFRP laminates with protective interlayers, which is up to 10 times longer. This innovative approach represents a potential advance in fire protection strategies for CFRP laminates, offering improved resilience against fire-induced structural failure.
Relation of craze to crack length during slow crack growth phenomena in high‐density polyethylene
(2024)
The craze‐crack mechanism occurring in high‐density polyethylene (HDPE) causing slow crack growth and environmental stress cracking is investigated in detail with respect to the relation of crack length and the related craze zone. This is essential for the understanding of the resulting features of the formed fracture surface and their interpretation in the context of the transition from crack propagation to ductile shear deformation. It turns out that an already formed craze zone does not inevitably result in formation of a propagating crack, but could also undergo ductile failure. For the examination, the full notch creep test (FNCT) was employed with a subsequent advanced fracture surface analysis that was performed using various imaging techniques: light microscopy, laser scanning microscopy, scanning electron microscopy, and X‐ray micro computed tomography scan. FNCT specimens were progressively damaged for increasing durations under standard test conditions applying Arkopal, the standard surfactant solution, and biodiesel as test media were used to analyze the stepwise growth of cracks and crazes. From considerations based on well‐established fracture mechanics approaches, a theoretical correlation between the length of the actual crack and the length of the preceding craze zone was established that could be evidenced and affirmed by FNCT fracture surface analysis. Moreover, the yield strength of a HDPE material exposed to a certain medium as detected by a classic tensile test was found to be the crucial value of true stress to induce the transition from crack propagation due to the craze‐crack mechanism to shear deformation during FNCT measurements.
Highlights
- Progress of crack formation in high‐density polyethylene is analyzed by different imaging techniques
- Determined growth rates depend on distinction between craze zone and crack
- The ratio of the present crack to the anteceding craze zone is validated theoretically
- The transition from crack propagation to ductile shear deformation is identified
- An already formed craze zone may still fail by ductile mechanisms
Confocal micro-X-ray fluorescence (micro-XRF) spectroscopy facilitates three-dimensional (3D) elemental imaging of heterogeneous samples in the micrometer range. Laboratory setups using X-ray tube excitation render the method accessible for diverse research fields but interpretation of results and quantification remain challenging. The attenuation of X-rays in composites depends on the photon energy as well as on the composition and density of the material. For confocal micro-XRF, attenuation severely impacts elemental distribution information, as the signal from deeper layers is distorted by superficial layers. Absorption correction and quantification of fluorescence measurements in heterogeneous composite samples have so far not been reported. Here, an absorption correction approach for confocal micro-XRF combining density information from microcomputed tomography (micro-CT) data with laboratory X-ray absorption spectroscopy (XAS) and synchrotron transmission measurements is presented. The energy dependency of the probing volume is considered during the correction. The methodology is demonstrated on a model composite sample consisting of a bovine tooth with a clinically used restoration material.
The stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation can provide a certain degree of plasticity to Ceria-stabilized (Ce-TZP) zirconia-based composites. Characterizing and monitoring this phase transition on a millimeter-size range, within the bulk and in-situ remains a challenge. In this work, the mechanical behavior of Ce-TZP based composite was studied in tension, combining microscopy and synchrotron Xray refraction techniques. In contrast with microscopy methods, which only provide surface information, X-ray refraction radiography (SXRR) allowed the visualization of all the transformation bands, over the entire length and thickness of tested specimens, opening up new avenues for in-situ stress-induced t-m transformation studies.
Adhesively bonded composite joints can develop voids and porosity during fabrication, leading to stress concentration and a reduced load-carrying capacity. Hence, adhesive porosity analysis during the fabrication is crucial to ensure the required quality and reliability. Ultrasonic-guided wave (UGW)-based techniques without advanced signal processing often provide low-resolution imaging and can be ineffective for detecting small-size defects. This article proposes a damage imaging process for adhesive porosity analysis of bonded composite plates using UGWs measured by scanning laser Doppler vibrometer (LDV). To implement this approach, a piezoelectric transducer is mounted on the composite joint specimen to generate UGWs, which are measured over a densely sampled area. The signals obtained from the scan are processed using the proposed signal processing in different domains. Through the utilization of filter banks in frequency and wavenumber domains, along with the root-mean-square calculation of filtered signals, damage images of the adhesive region are obtained. It has been observed that different filters provide information related to different void sizes. Combining all the images reconstructed by filters, a final image is obtained which contains damages of various sizes. The images obtained by the proposed method are verified by radiography results and the porosity analysis is presented. The results indicate that the proposed methodology can detect the pores with the smallest detectable pore area of 2.41 mm^2, corresponding to a radius of 0.88 mm, with an overall tendency to overestimate the pore size by an average of 11%.
This study investigates the room‐ and high‐temperature (650 °C) tensile and low‐cycle‐fatigue behavior of Inconel 718 produced by laser powder bed fusion (PBF‐LB/M) with a four‐step heat treatment and compares the results to the conventional wrought material. The microstructure after heat treatment is characterized on different length scales. Compared to the wrought variant, the elastic and yield properties are comparable at both test temperatures while tensile strength, ductility, and strain hardening capacity are lower. The fatigue life of the PBF‐LB/M variant at room temperature is slightly lower than that of the wrought material, while at 650 °C, it is vice versa. The cyclic stress response for both material variants is characterized by cyclic softening, which is more pronounced at the higher test temperature. High strain amplitudes (≥0.7%) at room temperature and especially a high testing temperature result in the formation of multiple secondary cracks at the transitions of regions comprising predominantly elongated grain morphology and columns of stacked grains with ripple patterns in the PBF‐LB/M material. This observation and pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients and local crystallite clusters.
Rechargeable alkali metal−CO2 batteries, which combine high theoretical energy density and environmentally friendly CO2 fixation ability, have attracted worldwide attention. Unfortunately, their electrochemical performances are usually inferior for practical applications. Aiming to reveal the underlying causes, a combinatorial usage of advanced nondestructive and postmortem characterization tools is used to intensively study the failure mechanisms of Li/Na−CO2 batteries. It is found that a porous interphase layer is formed between the separator and the Li/Na anode during the overvoltage rising and battery performance decaying process. A series of control experiments are designed to identify the underlying mechanisms dictating the observed morphological evolution of Li/Na anodes, and it is found that the CO2 synergist facilitates Li/Na chemical corrosion, the process of which is further promoted by the unwanted galvanic corrosion and the electrochemical cycling conditions. A detailed compositional analysis reveals that the as-formed interphase layers under different conditions are similar in species, with the main differences being their inconsistent quantity. Theoretical calculation results not only suggest an inherent intermolecular affinity between the CO2 and the electrolyte solvent but also provide the most thermodynamically favored CO2 reaction pathways. Based on these results, important implications for the further development of rechargeable alkali metal−CO2 batteries are discussed. The current discoveries not only fundamentally enrich our knowledge of the failure mechanisms of rechargeable alkali metal−CO2 batteries but also provide mechanistic directions for protecting metal anodes to build high-reversible alkali metal−CO2 batteries.
In this presentation, the results of the determination of the diffraction and single-crystal elastic constants of laser powder bed fused Inconel 718 are presented. The analysis is based on high-energy synchrotron diffraction experiments performed at the Deutsches Elektronen-Synchrotron. It is shown that the characteristic microstructure of laser powder bed fused Inconel 718 impacts the elastic anisotropy and therefore the diffraction and single-crystal elastic constants. Finally, the consequences on the diffraction-based residual stress determination of laser powder bed fused Inconel 718 are discussed.
Rechargeable sodium–oxygen batteries (NaOBs) are receiving extensive research interests because of their advantages such as ultrahigh energy density and cost efficiency. However, the severe failure of Na metal anodes has impeded the commercial development of NaOBs. Herein, combining in situ synchrotron X-ray computed tomography (SXCT) and other complementary characterizations, a novel electro-chemo-mechanical failure mechanism of sodium metal anode in NaOBs is elucidated. It is visually showcased that the Na metal anodes involve a three-stage decay evolution of a porous Na reactive interphase layer (NRIL): from the initially dot-shaped voids evolved into the spindle-shaped voids and the eventually-developed ruptured cracks. The initiation of this three-stage evolution begins with chemical-resting and is exacerbated by further electrochemical cycling. From corrosion science and fracture mechanics, theoretical simulations suggest that the evolution of porous NRIL is driven by the concentrated stress at crack tips. The findings illustrate the importance of preventing electro-chemo-mechanical degradation of Na anodes in practically
rechargeable NaOBs.
Determination of short carbon fiber orientation in zirconium diboride ceramic matrix composites
(2024)
In fiber-reinforced components, the fiber alignment and orientation have paramount influence on the thermomechanical properties of the resulting composite, for both short and continuous fiber. Here we present the case of an ultra-refractory matrix intended for extreme environment applications, ZrB2, reinforced with 20 vol% and 50 vol% short carbon fibers. In both cases, fibers tend to align perpendicular to the uniaxial pressure applied during shaping and sintering of a pellet, although the fiber tilt across the pellet thickness is difficult to determine. Moreover, for high volume fractions of reinforcement, the spatial distribution of the fibers is heterogeneous and tends to have domains of preferential orientations. We compare the information on the fiber distribution as collected by scanning electron microscopy images, X-ray computed tomography and synchrotron X-ray refraction radiography (SXRR). The three techniques prove to be complementary. Importantly, we demonstrate that SXRR yields the most statistically significant information due to the largest field of view, yet with a sensitivity down to the nanometer, and that can be successfully applied also to heavy matrix materials, such as zirconium boride.
AbstractIn this study, we compare the residual stress state in a laser powder bed fusion (PBF‐LB/M) AlSi10Mg alloy in the as‐built (AB) condition with that after two different heat treatments (265 °C for 1 h, HT1; and 300 °C for 2 h, HT2). The bulk residual stress (RS) is determined using synchrotron X‐ray diffraction (SXRD), and near‐surface profiles are determined using laboratory energy‐dispersive X‐ray diffraction (EDXRD). The EDXRD results do not reveal any notable difference between the conditions at a depth of 350 μm, suggesting that the machining process yields a comparable residual stress state in the near‐surface regions. On the other hand, the SXRD results show that HT1 is more effective in relieving the bulk RS. It is observed that HT1 reduces the RS state in both the aluminium matrix and the silicon network. In addtion, HT2 does not have a significant impact on relaxing the RS as‐built state of the matrix, although it does induce a reduction in the RS magnitudes of the Si phase. It is concluded that the heat treatment stress relieving is effective as long as the Si‐network is not disaggregated.
A new titanium alloy improving the operation of implants additively manufactured and including laterally closed lattice structures is proposed. The new alloy possesses an increased affinity to the bone. The measured bone–interface implant (BII) of less than 10 mm and bone–implant contact (BIC) of 95% demonstrated an excellent osseointegration. Furthermore, since additive manufacturing naturally leads to a high-roughness surface finish, the wettability of the implant is increased. The combination of these factors is pushing ossification beyond its natural limits. In addition, the quality and speed of the ossification and osseointegration in/around laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required.
Powder Bed Fusion – Laser Beam (PBF-LB) of high γ’ strengthened Ni-base superalloys, such as CM247LC, is of great interest for high temperature applications in gas turbines. However, PBF-LB of CM247LC is challenging due to the high cracking susceptibility during PBF-LB processing (solidification cracking) and heat treatment (strain age cracking, mostly caused by residual stresses). This study focuses on understanding the impact of process parameters on microstructure, residual stresses and solidification cracking. Laser power (P), speed (v) and hatch spacing (h) were varied while the layer thickness (t) was fixed. The melt pool size and shape were found to be key factors in minimizing solidification cracking. Narrower and shallower melt pools, achieved using a low line energy density (LED = P/v ≤ 0.1 J/mm), gave low crack densities (0.7 mm/mm2). A tight hatch spacing (h = 0.03 mm) resulted in reduced lack of fusion porosity. Electron backscatter diffraction investigations revealed that parameters giving finer microstructure with 〈100〉crystallographic texture had low crack densities provided they were processed with a low LED. Atom probe tomography elucidated early stages of spinodal decomposition in the as-built condition, where Cr and Al cluster separately. The extent of spinodal decomposition was found to be affected by the LED and the hatch spacing. Samples with low LED and small hatch spacing showed higher degrees of spinodal decomposition. X-ray diffraction residual stress investigations revealed that the residual stress is proportional to the volumetric energy density (VED = P/(v. h. t)). Although low residual stresses can be achieved by using low VED, there is a high risk of lack of fusion. Hence, other parameters such as modified scan strategy, build plate pre-heating and pulsed laser mode, must be further explored to minimize the residual stresses to reduce the strain age cracking susceptibility.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field material characterization by X-ray imaging is presented. The principle of X-ray Computed Tomography (XCT) is explained. The multiple examples of application of quantitative analysis by XCT are reported, such as additive manufacturing, Li-ion battery, concrete research.
A systematic, nature-inspired chemical engineering approach is employed to solve the issue of flooding in electrochemical devices. The mechanism of passive water transport utilized by lizards living in arid environments is leveraged to design flow-fields with a microchannel structure on their surface, through which capillary pressure rapidly removes the water generated in the electrochemical device. This water management strategy is implemented in proton exchange membrane fuel cells (PEMFCs) with a lunginspired flow-field, which ensures uniform distribution of reactants across the catalyst layer. Jointly, this nature-inspired approach results in flood-free, stable operation at 100% RH and a B60% increase in current (B1.9 A cm-2) and peak power density (B650 mW cm−2) compared to current PEMFCs with a flood-prone, serpentine flow-field (B0.8 A cm-2 and 280 mW cm-2, respectively). This significant advance allows for PEMFC operation at fully humidified conditions.
Currently, mandatory requirements and recommendations for the detection of irregularities in laser beam welded joints are based on classic micrographs as set out in the standard ISO 13919-1:2019. Compared to classic micrographs, computed tomography enables a non-destructive, three-dimensional and material-independent mode of operation, which delivers much more profound results. Even in building material testing, methods with limited informative value can be checked and supplemented by CT examinations.
Die Erzeugung rissschließfreier Anrisse in gekerbten bruchmechanischen Proben für anschließende Ermüdungsversuche kann durch eine zyklische Druckbelastung an der Kerbe erfolgen: Bei der Erstbelastung wird eine plastische Verformung an der Kerbspitze erzeugt, welche Zugeigenspannungen und damit eine risstreibende Kraft bei der folgenden zyklischen Druckbelastung hervorruft. Durch das Risswachstum kommt es zu einer Entspannung, bis der Riss schließlich arretiert, weil die effektive risstreibende Kraft auf den Schwellenwert abgesunken ist. Um Kurzrisswachstum in additiv, mittels pulverbettbasiertem Laserstrahlschmelzen (Laser Powder Bed Fusion - LPBF) gefertigtem AISI 316L Stahl und seinem konventionell erzeugten, warmgewalzten Pendant zu untersuchen, wurde dieses Verfahren im Rahmen der vorliegenden Arbeit genutzt. Im Falle des additiv gefertigten Materials kam es zu unerwartet langem Ermüdungsrisswachstum, bevor der Riss arretierte. Zur Ermittlung der Ursache erfolgte eine Messung der Eigenspannungsverteilungen mittels Neutronendiffraktion in der Kerbebene der additiv gefertigten Proben. Anschließend wurde ein Finite-Elemente-Modell zur Simulation des Ermüdungsrisswachstums in konventionellem und additiv gefertigtem Material implementiert. Im Rahmen dieses Vortrages wird insbesondere auf das Vorgehen bei der Simulation und auf die getroffenen Annahmen und Vereinfachungen eingegangen. Die Resultate werden mit den experimentellen Ergebnissen verglichen und das für die Simulation von Risswachstum genutzte Knoten-Freigabe-Verfahren (Node-Release), das Einbringen von Eigenspannungen als initiale Spannungen in der Simulation, und die Rechengrößen zur Quantifizierung der risstreibenden Kraft kritisch diskutiert.
Efficient density evolution during sintering of the as-printed component is vital to reach full densification and required properties of binder jet (BJT) components. However, due to the high porosity and brittle nature of the green compact, analysis of the microstructure development during sintering is very difficult, resulting in lack of understanding of the densification process. Density development from green state (57 ± 1.6 %) up to full density (99 ± 0.3 %) was characterized by high-resolution synchrotron X-Ray computed tomography (SXCT) on BJT 316L samples from ex-situ interrupted sintering tests. Periodicity of density fluctuations along the building direction was revealed for the first time and was related to the layer thickness of ~ 42 μm during printing that decreased down to ~ 33 μm during sintering. Sintering simulations, utilizing a continuum sintering model developed for BJT, allowed to replicate the density evolution during sintering with a mean error of 2 % and its fluctuation evolution from green (1.66 %) to sintered (0.56 %) state. Additionally, simulation of extreme particle size segregation (1 μm to 130 μm) suggested that non-optimized printing could lead to undesirable density fluctuation amplitude rapid increase (~10 %) during sintering. This might trigger the nucleation of defects (e.g., layer delamination, cracking, or excessive residual porosity) during the sintering process.
Simulation-Assisted Augmentation of Missing Wedge and Region-of-Interest Computed Tomography Data
(2024)
This study reports a strategy to use sophisticated, realistic X-ray Computed Tomography (CT) simulations to reduce Missing Wedge (MW) and Region-of-Interest (RoI) artifacts in FBP (Filtered Back-Projection) reconstructions. A 3D model of the object is used to simulate the projections that include the missing information inside the MW and outside the RoI. Such information augments the experimental projections, thereby drastically improving the reconstruction results. An X-ray CT dataset of a selected object is modified to mimic various degrees of RoI and MW problems. The results are evaluated in comparison to a standard FBP reconstruction of the complete dataset. In all cases, the reconstruction quality is significantly improved. Small inclusions present in the scanned object are better localized and quantified. The proposed method has the potential to improve the results of any CT reconstruction algorithm.
Manufacturing austenitic stainless steels (ASSs) using additive manufacturing is of great interest for cryogenic applications. Here, the mechanical and microstructural responses of a 316L ASS built by laser powder bed fusion were revealed by performing in situ neutron diffraction tensile tests at the low-temperature range (from 373 to 10 K). The stacking fault energy almost linearly decreased from 29.2 ± 3.1 mJm⁻² at 373 K to 7.5 ± 1.7 mJm⁻² at 10 K, with a slope of 0.06 mJm⁻²K⁻¹, leading to the transition of the dominant deformation mechanism from strain-induced twinning to martensite formation. As a result, excellent combinations of strength and ductility were achieved at the low-temperature range.
AbstractLithium‐ion cells connected in series are prone to an electrical safety risk called overdischarge. This paper presents a comprehensive investigation of the overdischarge phenomenon in lithium‐ion cells using operando nondestructive imaging. The study focuses on understanding the behavior of copper dissolution and deposition during overdischarge, which can lead to irreversible capacity loss and internal short‐circuits. By utilizing synchrotron X‐ray computed tomography (SXCT), the concentration of dissolved and deposited copper per surface area is quantified as a function of depth of discharge, confirming previous findings. The results also highlight for the first time a nonuniform distribution pattern for copper deposition on the cathode. This research provides insights for safer battery cell design.
Due to their increasing energy density, lithium-ion-batteries (LIBs) play a key role in the traffic energy transition. Regarding their safety behavior, the main challenge of LIB-cells remains the thermal runaway (TR) process. In situ/operando investigations of the TR on commercial cells is possible with radiographic and computer tomographic measurements. Nonetheless, high resolution visualization of the TR persists as a challenge due to the high progression speed of the TR-process itself. Generally, performing abuse tests at cryogenic temperatures allows to slow down or even prevent the TR. Nevertheless, not all abuse methods are suitable for TR investigations at low temperatures. Nail penetration is an appropriate option, however, contains numerous unknown parameters and therefore suffers regarding reproducibility.
Herein, a self-developed high precision nail-penetration-setup is introduced, approaching the necessary mechanically reproducibility with controlled temperatures down to -190°C. The setup allows the preparation of critically abused, however, at cryogenic temperatures stable LIB-cells. These cells were controlled rethermalized to room temperature during synchrotron x-ray computer tomography (SXCT) with a pixel size up to 0.7 μm. During this measurement, the temperature and voltage of the cell is monitored allowing the visualization of the initial internal cell reactions. This study reveals the relation between internal reactions and cell voltage. Finally, the developed set-up enables in-depth analysis of thermal runaway behavior down to material level for various commercial battery cells in the future.
The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). By fully utilizing these KETs, advanced and sustainable economies will be created. It is considered that Metrology is a key enabler for the advancement of these KETs. EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network for Advanced Manufacturing. The EMN is made up of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The EMN aims to provide a high-level coordination of European metrology activities for the Advanced Materials and Advanced Manufacturing community.
The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing and Advanced Materials (Large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider metrology community (including TCs) to provide input for the preparation of a Strategic Research Agenda (SRA) for Metrology for Advanced Manufacturing.
This presentation will describe the progress in the development of the SRA by the EMN for Advanced Manufacturing. The metrology challenges identified across the various key industrial sectors, which utilise Advanced Materials and Advanced Manufacturing will be presented.
The EMN for Advanced Manufacturing is supported by the project JNP 19NET01 AdvManuNet.
The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). It is considered that Metrology is a key enabler for the advancement of these KETs. Consequently, EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network (EMN) for Advanced Manufacturing. The EMN is comprised of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The aim of the EMN is to provide a high-level coordination of European metrology activities for the Advanced Manufacturing community.
The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing (large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider Metrology community, including Technical Committees, to provide input for the Strategic Research Agenda (SRA) on Metrology for Advanced Manufacturing.
This contribution will give an overview about the first version of the SRA prepared by the EMN for Advanced Manufacturing
Laser powder bed fusion is one of the most promising additive manufacturing techniques for printing complex-shaped metal components. However, the formation of subsurface porosity poses a significant risk to the service lifetime of the printed parts. In-situ monitoring offers the possibility to detect porosity already during manufacturing. Thereby, process feedback control or a manual process interruption to cut financial losses is enabled.
Short-wave infrared thermography can monitor the thermal history of manufactured parts which is closely connected to the probability of porosity formation. Artificial intelligence methods are increasingly used for porosity prediction from the obtained large amounts of complex monitoring data. In this study, we aim to identify the potential and the challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring.
Therefore, the porosity prediction task is studied in detail using an exemplary dataset from the manufacturing of two Haynes282 cuboid components. Our trained 1D convolutional neural network model shows high performance (R2 score of 0.90) for the prediction of local porosity in discrete sub-volumes with dimensions of (700 x 700 x 40) μm³.
It could be demonstrated that the regressor correctly predicts layer-wise porosity changes but presumably has limited capability to predict differences in local porosity. Furthermore, there is a need to study the significance of the used thermogram feature inputs to streamline the model and to adjust the monitoring hardware. Moreover, we identified multiple sources of data uncertainty resulting from the in-situ monitoring setup, the registration with the ground truth X-ray-computed tomography data and the used pre-processing workflow that might influence the model’s performance detrimentally.
Residual stresses Analysis in Additively Manufactured alloys using neutron diffraction (L-PBF)
(2023)
An overview of recent progress at BAM of residual stress analysis in additively manufactured, in particular Laser Powder Bed Fusion of metallics materials, using neutron diffraction will be presented. This will cover important topics of the stress-free reference, the diffraction elastic moduli and principal stress determination.
The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). It is considered that Metrology is a key enabler for the advancement of these KETs. Consequently, EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network (EMN) for Advanced Manufacturing. The EMN is comprised of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The aim of the EMN is to provide a high-level coordination of European metrology activities for the Advanced Manufacturing community.
The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing (large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider Metrology community, including Technical Committees, to provide input for the Strategic Research Agenda (SRA) on Metrology for Advanced Manufacturing.
This contribution will give an overview about the first version of the SRA prepared by the EMN for Advanced Manufacturing.
Ziel der Untersuchung: Evaluation der Eignung der Refraktions-Tomographie zur Analyse von Alterungserscheinungen innerhalb von adhäsiv verankerten Materialien vor und nach künstlicher Probenalterung.
Material und Methode: Vier humane mittlere Oberkieferfrontzähne wurden wurzelkanalbehandelt und ausgedehnte Klasse IV Defekte der Krone mit einer Aufbaufüllung aus dualhärtendem Komposit (Rebilda DC, VOCO) und einem Glasfaserstift (Rebilda Post, VOCO) restauriert. Alle Proben wurden feucht gelagert und in einer Synchrotron-Einrichtung (BAMline, BESSY II, HZB) mit einer Pixelgröße von 4,08 µm gescannt. Für diese Synchrotron-Refraktions-Tomographie (SXRCT) muss zunächst der Analysatorkristall (AK) zu einer Bragg-Reflexion (Beugung) angeregt werden, um eine SXRCT durchzuführen. Die SXRCT wird mit einer Transmissions-Tomographie (ohne AK) verrechnet. Darauf folgte eine künstliche Probenalterung mit 400.000 Kau- und 3.000 Thermozyklen (50N, 5-55°C). Anschließend wurden die Proben ein weiteres Mal gescannt. Die Datensätze beider SXRCT wurden mittels des „filtered back projection“ Algorithmus rekonstruiert, mit einer Bildanalyse-Software aufeinander registriert und ausgewertet. Hierdurch konnten die Veränderungen initialer Schädigungen analysiert werden.
Ergebnisse: Alle 4 Proben zeigten in den Scans Veränderungen des inneren Gefüges und an Grenzflächen nach Belastung. Es zeigten sich Ansammlungen von Wasser innerhalb eingeschlossener Hohlräume, subkritisches Risswachstum, Ausdehnung des Komposit und Quellung des Glasfaserstiftes um 0,4%. In den SXRCT Aufnahmen waren außerdem Dentintubuli, die bei Auflösungen von 4,08 µm sonst nicht deutlich sichtbar sind darstellbar. Dadurch konnte Eindringen von Wasser in die Tubuli im Anschluss an die Alterung belegt werden.
Zusammenfassung: SXRCT bietet die Möglichkeit, trotz einer vergleichbar geringen Auflösung, kleinste Strukturen und Veränderungen abzubilden. Dies ermöglicht unter anderem die detaillierte Analyse relativ großer Proben, wie eines vollständigen Zahnes in einem Scanvorgang.
We employ in-house generated synthetic Al-Si matrix composite XCT data for training deep convolutional neural networks for XCT data conditioning and automatic segmentation. We propose an in-house multilevel deep conditioning framework capable of rectifying noise and blur in corrupted XCT data sequentially. Furthermore, for automatic segmentation, we utilize a special in-house network coupled with a novel iterative segmentation algorithm capable of generalized learning from synthetic data. We report a consistent SSIM efficiency of 92%, 99%, and 95% for the combined denoising/deblurring, standalone denoising, and standalone deblurring, respectively. The overall segmentation precision was over 85% according to the Dice coefficient. We used experimental XCT data from various scans of Al-Si matrix composites reinforced with ceramic particles and fibers.
It is shown that preconditioning of experimental X‐ray computed tomography (XCT) data is critical to achieve high‐precision segmentation scores. The challenging experimental XCT datasets and deep convolutional neural networks (DCNNs) are used that are trained with low‐resemblance synthetic XCT data. The material used is a 6‐phase Al–Si metal matrix composite‐reinforced with ceramic fibers and particles. To achieve generalization, in our past studies, specific data augmentation techniques were proposed for the synthetic XCT training data. In addition, two toolsets are devised: (1) special 3D DCNN architecture (3D Triple_UNet), slicing the experimental XCT data from multiple views (MultiView Forwarding), the i.S.Sy.Da.T.A. iterative segmentation algorithm, and (2) nonlocal means (NLM) conditioning (filtering) for the experimental XCT data. This results in good segmentation Dice scores across all phases compared to more standard approaches (i.e., standard UNet architecture, single view slicing, standard single training, and NLM conditioning). Herein, the NLM filter is replaced with the deep conditioning framework BAM SynthCOND introduced in a previous publication, which can be trained with synthetic XCT data. This leads to a significant segmentation precision increase for all phases. The proposed methods are potentially applicable to other materials and imaging techniques.
Large temperature gradients inherent to additive manufacturing (AM) processes induce large residual stress (RS) in the final part. Because RS can influence the tribological properties, this study focuses on the relationship between wear sliding properties and RS in IN718 coatings. Such coatings were deposited with a Laser metal deposition (LMD) machine using two different scanning strategies.
The wear resistance and RS state were investigated after surface milling. RS were measured before and after wear tests on a reciprocating sliding test apparatus.
Two different X-ray diffraction techniques were employed to measure the surface and subsurface state RS: Laboratory Energy Dispersive X-ray Diffraction (LEDXD) and Synchrotron X-ray Energy Dispersive Diffraction (SXEDD). Due to the milling process, the coatings show similar depth distributions of RS from 22 to 92 μm depth, but exhibit different magnitudes depending on the scanning strategy used. Reciprocating sliding wear tests induced high compressive residual stresses that erased the initial RS state, and a similar wear behavior was observed in the two samples. These samples possess similar texture and grain morphology. This demonstrates that the influence of RS on wear resistance is a second-order effect. Nevertheless, it was observed that RS can still impact the wear performance at the early testing stages of the repaired parts.
The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the data handling pipeline is presented.
The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented.
The lack of traceability to meter of X-ray Computed Tomography (CT) measurements still hinders a more extensive acceptance of CT in coordinate metrology and industry. To ensure traceable, reliable, and accurate measurements, the determination of the task-specific measurement uncertainty is necessary. The German guideline VDI/VDE 2630 part 2.1 describes a procedure to determine the measurement uncertainty for CT experimentally by conducting several repeated measurements with a calibrated test specimen. However, this experimental procedure is cost and effort intensive. Therefore, the simulation of dimensional measurement tasks conducted with X-ray computed tomography can close these drawbacks. Additionally, recent developments towards a resource and cost-efficient production (“smart factory”) motivate the need for a corresponding numerical model of a CT system (“digital twin”) as well. As there is no standardized procedure to determine the measurement uncertainty of a CT system by simulation at the moment, the project series CTSimU was initiated, aiming at this gap. Concretely, the goal is the development of a procedure to determine the measurement uncertainty numerically by radiographic simulation. The first project (2019-2022), "Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation - CTSimU" developed a framework to qualify a radiographic simulation software concerning the correct simulation of physical laws and functionalities. The most important outcome was a draft for a new guideline VDI/VDE 2630 part 2.2, which is currently under discussion in the VDI/VDE committee. The follow-up project CTSimU2 "Realistic Simulation of real CT systems with a basic-qualified Simulation Software" will deal with building and characterizing a digital replica of a specific real-world CT system. The two main targets of this project will be a toolbox including methods and procedures to configure a realistic CT system simulation and to develop tests to check if this replica is sufficient enough. The result will be a draft for a follow-up VDI/VDE guideline proposing standardized procedures to determine a CT system's corresponding characteristics and test the simulation (copy) of a real-world CT system which we call a "digital twin".
The project series CTSimU was initiated with the goal to develop a set of procedures to enable the determination of the task-specific measurement uncertainty of a CT system numerically by radiographic simulation. The first project (2019-2022) “Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation - CTSimU” was focused on the sufficient physical correctness of the radiographic simulation and created as a result a test framework for simulation softwares and a draft of a VDI standard in the series VDI/VDE 2630 for this application. However, for the realistic simulation of a CT system in a simulation software (i.e. a digital twin), not only the correctness of the simulation software itself is crucial, but also the quality of the parameterization of the CT system in the simulation software - this represents the starting point of the 2nd project “Realistic Simulation of real CT systems with a basic-qualified Simulation Software - CTSimU2” (2022-2024).
The parameterization of a CT system in a simulation software can be divided into four steps: after the data acquisition at the real CT system (step 1) follows the evaluation of the acquired data for the generation of general parameter specifications (step 2). It follows the transfer of the parameters into the specific simulation software (step 3) and the validation of the resulting simulation parameters by a suitable test (step 4). The intended result of the project CTSimU2 is a draft VDI standard (for VDI/VDE 2630) for this test, which contains an informative annex on the state of the art regarding the possibilities for parameter determination.
Die Entwicklung von Werkzeugen zur realitätsnahen Nachbildung eines industriellen CT-Systems in einer Simulationssoftware ist derzeit Hauptaufgabe des WIPANO Forschungsprojektes CTSimU2 Realistische Simulation realer Röntgencomputertomografie - Systeme mit basisqualifizierter Simulationssoftware. Als Voraussetzung dienen dabei Simulationssoftwares, die durch das Testframework aus dem Vorprojekt CTSimU1 basisqualifiziert wurden. Das Testframework testet die hinreichende physikalische Korrektheit und Funktionalität einer Simulationssoftware (Basisqualifizierung der Software). Für eine realitätsnahe Nachbildung ist nicht nur die Güte der Simulationssoftware, sondern insbesondere die Güte der Parametrisierung des realen CT-Systems in der Simulationssoftware ausschlaggebend. Dabei kann das Vorgehen der Parametrisierung in vier Schritte unterteilt werden: die Datenaufnahme am realen CT-System (Schritt 1), die Auswertung der aufgenommenen Daten für die Generierung allgemeiner Parameterangaben (Schritt 2), die Übertragung der Parameter in die spezifischen Simulationssoftwares (Schritt 3) und die Validierung der resultierenden Simulationsparameter durch einen geeigneten Test (Schritt 4). Ziel des Projektes ist es daher neben der Erarbeitung eines Werkzeugkastens mit allgemeinen Methoden zur Datenaufnahme und Auswertung der Daten, die Entwicklung eines Tests, auf dessen Basis die ausreichend korrekte Simulation einer realen Anlage beurteilt werden kann. Die erarbeiteten Ergebnisse sollen wie bereits im Vorprojekt CTSimU1 in einen Richtlinienentwurf für die Richtlinienreihe VDI/VDE 2630 übertragen werden. Dieser Beitrag soll einen Überblick über das Projekt und die ersten Ergebnisse geben.
Virtual CT with aRTist
(2023)
The software aRTist is a simulation tool for the generation of realistic radiographs of virtual radiographic superstructures.
With radiographic simulations, virtual component models can be scanned as in a computer tomograph.
Industrial X-ray computed tomography (CT) enables the non-destructive detection of internal and external surfaces as well as inhomogeneities of technical objects. Virtual CT offers new possibilities for the investigation of parameter influences of this complex testing and measuring technique. In addition to the option of switching physical effects on and off, scanning movements can also be tested before their technical realization.
The virtual CT generates projection images from different directions for the subsequent reconstruction of a volume model of the examined object. The reconstruction of the simulated scans is carried out with the algorithms and programs for real scans. Tomographic scans consist of a large number of projections, which practically cannot be generated individually by the user of a simulation. The software offers various options for the automated simulation of tomographic scans. These range from standard CT to scans on free trajectories or with individual projection matrices.
Structural alloys are largely employed in key industrial sectors and their demand is predicted to rise rapidly for the next decades. Most of these materials require a large amount of energy for extraction and manufacturing, which causes the emission of greenhouse gases and other pollutants. Therefore, strategies for improving the sustainability of structural metallic alloys are urgently needed.
Additive Manufacturing (AM), in particular Laser Powder Bed Fusion (PBF-LB/M), aims to be a sustainable manufacturing process, as it allows the build-up of complex geometry in near net-shape from 3D models, while minimizing material waste and the energy required for the process and post-process treatments.
Nevertheless, the application of additively manufactured parts in structural safety-relevant applications is still hindered by the poor fatigue performance. The cause of this has been mainly attributed to the presence of manufacturing defects and surface roughness. Therefore, a huge effort has been made to optimize the process parameters and to introduce post-process treatments to minimize the defect content. However, material flaws cannot be fully eliminated, but these can be considered in a damage tolerance framework for the prediction of the fatigue performance of additively manufactured metallic materials, which is essential for part design and qualification.
This work aims at presenting different modelling strategies for the prediction of the fatigue limit of AM metals. Simple empirical models and more complex models based on fatigue short crack propagation are proposed. The investigated material is an AlSi10Mg alloy fabricated by PBF-LB/M and subjected to two different low-temperature heat-treatments (265°C for 1 h and 300°C for 2h). The results show that the models can provide good approximation of the fatigue limits and help in the interpretation of the scatter of fatigue data.
Li dendrites penetration through solid electrolytes (SEs) challenges the development of solid-state Li batteries (SSLBs). To date, significant efforts are devoted to understand the mechanistic dynamics of Li dendrites nucleation, growth, and propagation in SEs, and various strategies that aim to alleviate and even inhibit Li dendrite formation have been proposed. Nevertheless, most of these conventional strategies require either additional material processing steps or new materials/layers that eventually increase battery cost and complexity. In contrast, using external fields, such as mechanical force, temperature physical field, electric field, pulse current, and even magnetic field to regulate Li dendrites penetration through SEs, seems to be one of the most cost-effective strategies. This review focuses on the current research progress of utilizing external physical fields in regulating Li dendrites growth in SSLBs. For this purpose, the mechanical properties of Li and SEs, as well as the experimental results that visually track Li penetration dynamics, are reviewed. Finally, the review ends with remaining open questions in future studies of Li dendrites growth and penetration in SEs. It is hoped this review can shed some light on understanding the complex Li dendrite issues in SSLBs and potentially guide their rational design for further development.
The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique). Also, two successful research project in collaboration with CAM2, Sweden are presented.
This paper presents an automatic damage imaging technique by employing a signal processing approach based on applying hierarchically clustered filters across different domains. The technique involves time-frequency-wavenumber filter banks which are applied sequentially to ultrasonic guided wave (UGW) data. The study is conducted for a single lap joint composite specimen with a special focus on small voids which were formed due to manual adhesive component mixing. UGW data are acquired with a 3D Scanning Laser Doppler Vibrometer (LDV) over the scan area of the bonded plate. UGWs are excited at the central frequency of 100 kHz by a single piezoelectric transducer mounted on the surface of the single plate. Within each domain of time, frequency, and wavenumber, four filters are designed which results in 64 distinct filtered wavefields. From each filtered wavefield, an image is obtained by using root-mean-square (RMS) calculation of the signals. The obtained results are then combined to create a final, improved-resolution image of the scan area. The final image is compared to the image obtained through RMS calculation of full wavefield with interpolation through Delaunay triangulation and the image obtained by X-ray radiography. The results show that the smallest void that could be detected has a diameter of 2.14 mm.
In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate.
The industrial sintering process used to produce metallic matrix pads has been altered to diminish the amount of copper used. Unfortunately, replacing a large part of the copper with iron seems to have reached a limit. In the high-energy, emergency-type rail braking used in this study, the materials are put to the very limit of their usage capacity, allowing us to observe the evolution of the microstructure and mechanical properties of sintered, metallic matrix pads. After the braking test, their compressive behaviour was assessed using digital image correlation (DIC), and their microstructure with scanning electron microscopy (SEM). The worn material has three flat layers with different microstructures and compressive behaviours. The boom layer seems unmodified. Macroscopic and microscopic cracks run through the intermediate layer (2–15 mm depth). The top layer has stiffened thanks to resolidification of copper. The temperature reaches 1000 °C during the braking test, which also explains the carbon diffusion into iron that result in the weakening of iron–graphite interfaces in the pad. Finally, submicronic particles are detected at many open interfaces of the worn and compressed pad. Associated with the predominant role of graphite particles, this explains the weak compressive behaviour of the pads.
Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the “subgrains” quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains.
This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data.
X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, they can detect objects with size above a few wavelengths of the radiation.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing:
1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1).
2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again on much smaller fields-of-view.
Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
High energy X-ray synchrotron diffraction is used to investigate the elastic anisotropy of the nickel-based superalloy IN718 produced by laser powder bed fusion (PBF-LB). This material is characterized by a columnar grain morphology with some crystallographic texture. The material is subjected to elastic loading to determine the diffraction elastic constants (DECs). Furthermore, the single-crystal elastic constants (SCEC) are refined from these experiments using different micromechanical models. The results show that each micromechanical model predicts a specific set of SCEC that well describes the elastic anisotropy of PBF-LB/IN718.
Hot Isostatic Pressing (HIP) is often introduced to tackle the porosity issue in additively manufactured (AM) materials. For instance, HIP post-processing is recommended to improve fatigue resistance of Laser powder bed fusion (PBF-LB) manufactured parts [1, 2]. Even though HIP cannot completely remove porosity, it significantly decreases the defect population and its average size below the critical threshold value leading to early crack initiation.
In the present study, in-situ investigation of HIP procedure of PBF-LB Ti-6Al-4V parts was carried out to gain further insights into the densification mechanism occurring during HIP. The in-situ observations at high pressure and high temperature are uniquely possible at the PSICHE beamline of the Soleil synchrotron (France), thanks to the Ultrafast Tomography on a Paris-Edinburgh Cell (UToPEC) and the combination of the fast phase-contrast tomography and energy-dispersive diffraction [3, 4]. A detailed methodology was developed to ensure that the correct pressure and temperature were maintained during the experiments.
The results allowed an estimation of the global dentification rate during HIP of PBF-LB Ti-Al-4V material, as well as a detailed quantitative characterization of the influence of pore size and shape on the densification process, thereby understanding the effectiveness of HIP process on different pore categories. After 20 mins, 75% of porosity can be considered as closed or has size below the resolution of the XCT reconstruction. We also observed that the smallest defects showed higher densification rate, while the defect shape did not have significant effect on such rate. The current development of in-situ HIP experiment allows experimental quantification and validation of the simulation work. Ultimately it paves the road to tailoring the HIP procedure for different materials depending on the porosity and microstructure.
Laser powder bed fusion is one of the most promising additive manufacturing techniques for printing complex-shaped metal components. However, the formation of subsurface porosity poses a significant risk to the service lifetime of the printed parts. In-situ monitoring offers the possibility to detect porosity already during manufacturing. Thereby, process feedback control or a manual process interruption to cut financial losses is enabled.
Short-wave infrared thermography can monitor the thermal history of manufactured parts which is closely connected to the probability of porosity formation. Artificial intelligence methods are increasingly used for porosity prediction from the obtained large amounts of complex monitoring data. In this study, we aim to identify the potential and the challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring.
Therefore, the porosity prediction task is studied in detail using an exemplary dataset from the manufacturing of two Haynes282 cuboid components. Our trained 1D convolutional neural network model shows high performance (R² score of 0.90) for the prediction of local porosity in discrete sub-volumes with dimensions of (700 x 700 x 40) μm³.
It could be demonstrated that the regressor correctly predicts layer-wise porosity changes but presumably has limited capability to predict differences in local porosity. Furthermore, there is a need to study the significance of the used thermogram feature inputs to streamline the model and to adjust the monitoring hardware. Moreover, we identified multiple sources of data uncertainty resulting from the in-situ monitoring setup, the registration with the ground truth X-ray-computed tomography data and the used pre-processing workflow that might influence the model’s performance detrimentally.
The development of more powerful and more efficient lithium-ion batteries (LIBs) is a key area in battery research, aiming to support the ever-increasing demand for energy storage systems. To better understand the causes and mechanisms of degradation, and thus the diminishing cycling performance and lifetime often observed in LIBs, in operando techniques are essential, because battery chemistry can be monitored non-invasively, in real time. Moreover, there is increasing interest in developing new battery chemistries. Beyond LIBs, sodium ion batteries (NIBs) have gained increasing interest in recent years, as they are a promising candidate to complement LIBs, owing to their improved sustainability and lower cost, while still maintaining high energy density.[1] Initial phases of NIB commercialisation have occurred in the past year. However, for the widespread commercialisation of NIBs, there are still challenges that need to be overcome in developing optimized electrode materials and electrolytes. For the development of such materials and greater understanding of sodium storage mechanisms, solid electrolyte interface (SEI) formation and stability, and degradation processes, in operando methodologies are crucial.
Among the techniques available for in operando analysis, nuclear magnetic resonance spectroscopy (NMR) and imaging (MRI) are becoming increasingly used to characterize the chemical composition of battery materials, study the growth and distribution of dendrites, and investigate battery storage and degradation mechanisms. In situ and in operando 1H, 7Li and 23Na NMR and MRI have recently been used to study LIBs and NIBs, identifying chemical changes in Li and Na species respectively, in metallic, quasimetallic and electrolytic environment as well as directly and indirectly studying dendrite formation in both systems.[2-4] The ability of NMR and MRI to probe battery systems across multiple environments can further be complemented by the enhanced spatial resolution of micro-computed X-ray tomography (μ-CT) which can provide insight into battery material microstructure and defect distribution.
Here, we report in operando 1H and 7Li NMR and MRI experiments that investigate LIB performance, and the identification of changes in the Li signal during charge cycling, as well as the observation of signals in both 1H and 7Li NMR spectra that we attribute to diminishing battery performance, capacity loss and degradation. Additionally, recent operando methodology are adapted and implemented to study Sn based anodes in NIBs. 23Na spectroscopy is performed to monitor the formation and evolution of peaks assigned to stages of Na insertion into Sn, while 1H MRI is used to indirectly visualize the volume expansion of Sn anodes during charge cycling. Battery operation and degradation is further explored in these NIBs, using μ-CT, where the anode is directly visualized to a higher resolution and the loss of electrolyte in the cell, during cycling is observed
Inconel 718 (IN718) is a traditional age-hardenable nickel-based alloy that has been increasingly processed by additive manufacturing (AM) in recent years. In the as-solidified condition, IN718 exhibits chemical segregation and the undesired Laves phase, requiring a solution annealing (SA) prior to aging. The material produced by AM does not respond to the established thermal routines in the same way as conventionally produced IN718, and there is still no consensus on which routine yields optimal results. This work aims to provide a fundamental understanding of the heat treatment (HT) response by continuously monitoring the microstructural evolution during SA via time-resolved synchrotron x-ray diffraction, complemented by ex-situ scanning electron microscopy (SEM). The samples were produced by laser powder bed fusion to a geometry of 10x20x90 mm³, from which Ø1x5 mm³ cylindric specimens were extracted. Two different scanning strategies – incremental 67° rotations, Rot, and alternating 0°/67° tracks, Alt – were used, leading to two different as-built conditions. 1-hour SAs were carried out in the beamline ID22 of the ESRF at 50 KeV. Two SA temperatures, SA1 = 1020 °C, and SA2 = 1080 °C were tested for each scanning strategy. Data were processed using the software PDIndexer. In the as-built state, all samples showed typical subgrain columnar cell structures with predominant Nb/Mo segregation and Laves phase at the cell walls, as seen by SEM. The Alt scan induced higher intensity on the Laves peaks than the Rot scan, suggesting a greater content of Laves. Chemical homogenization in the SA was largely achieved during the heating ramp (Fig. 1). SA2 eliminated the Laves peaks just before reaching 1080 °C, and mitigated differences between Rot and Alt samples. On the other hand, SA1 induced the precipitation of the generally detrimental δ phase, also observed by SEM. Furthermore, the Rot scan showed higher δ peak intensities than the Alt scan, indicating a higher content of δ in the latter. No signs of recrystallization were observed in any of the investigated SAs.
The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of different kind of materials in FB8.5 Micro-NDT BAM. For instance, the manufacturing defects and high RS are inherent of additively manufacturing techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
Material extrusion of thermoplastic polymers enables the realization of complex specific designs with high performance composites. The present study aims at evaluating the mechanical properties of carbon fiberreinforced semi-crystalline thermoplastic polymer polyether ether ketone (CFR-PEEK) manufactured by material extrusion and correlating them with results obtained by micro-CT. Samples in the shape of small bars were provided by Kumovis (Munich, Germany). The determination of surface roughness and density was followed by three-point bending tests. To reveal the pore distribution as well as the fusion quality of CFR PEEK when applied with external forces, micro-CT scans were performed with an X-ray microscope before and after the mechanical test to localize the sites where the fracture is generated. The density of CFR-PEEK bars indicated that they had superior mechanical properties compared with our previous study on unfilled 3D printed PEEK (bending modulus: (5.4 ± 0.5) GPa vs. (1.05 ± 0.05) GPa to (1.48 ± 0.10) GPa; bending strength: (167 ± 11) MPa vs. (51 ± 15) to (193 ± 7) MPa). Micro-CT analyses revealed the local 3D-distribution of voids. Voids of 30 μm diameter are nearly spherical and make up the main part of the total porosity. The larger the voids, the more they deviate from a spherical shape. Significant lack-of-fusion voids are located between the deposited filaments. By growing and merging, they act as seeds for the forming fracture line in the region of the flexural specimens where the maximum local tensile stresses occurred under bending load. Our work provides a detailed analysis of printed PEEK with fiber additive and relates this with mechanical properties.
The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of additively manufactured (AM) materials in BAM (Berlin, Germany). The manufacturing defects and high RS are inherent of AM techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads.
The stress–strain behavior of ceramics, such as aluminum titanate, has certain features that are unusual for brittle materials—in particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the sharp increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and are attributed to microcracking. Here we compare different degrees of stress–strain nonlinearity of aluminum titanate materials and quantitatively model them. We use advanced mechanical testing to observe the mechanical response at room and high temperature; electron microscopy, and X-ray refraction radiography to observe the microstructural changes. Experiments show that two types of microcracks can be distinguished: (i) microcracks induced by cooling from the sintering temperature (due to heterogeneity and anisotropy of thermal expansion), with typical sizes of the order of grain size, and (ii) much larger microcracks generated by the mechanical loading. The two microcrack types produce different effects on the stress–strain curves. Such microcracks and the features of the stress–strain behavior depend on the density of the cooling-induced microcracks and on the distribution of grain sizes. They are modeled analytically and numerically.
The global demand for concrete is growing, and with it, its carbon footprint. Current literature proposes biochar, a product of pyrolysis, as a possible car-bon sink to reduce the carbon footprint of concrete. This work investigates the microstructure of Portland cement pastes with 0%, 5%, and 25% of the cement replaced with wood biochar, since this should influence its macro-scopic mechanical properties. MIP, gas sorption, NMR, and µ-CT were used to analyze the pore space of the three materials. The combination of these methods, each with different resolution, enables a multi-scale investigation of biochar impact on the microstructure of cement pastes. NMR confirmed that biochar can absorb moisture and, thus, reduces the effective water-to-cement ratio. MIP and gas sorption results show 0% and 5% volume re-placement have similar gel pore structure. The results from µ-CT investiga-tions suggest that biochar may reduce the formation of larger pores. The in-clusion of non-reactive porous particles such as biochar increase the porosity of the material and should act as a weakness in terms of mechanical proper-ties. Overall, this study highlights the need to carefully tailor replacement rates to control the impact of biochar on the microstructure concrete mixtures and sees a strong need for further studies on mechanical properties.
We discuss the non-linear stress–strain behavior of microcracked polycrystalline ceramics under uniaxial tension and compression (displacement control).
Micromechanics explanation and modeling of its basic features, such as non-linearity and hysteresis in stress–strain curves, are developed, with stable microcrack propagation and “roughness” of intergranular cracks playing critical roles in tension and crack sliding playing a critical role in compression. Experiments involving complex loading histories are explained, and themodel is shown to reproduce the basic features of the observed stress–strain curves.
Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc.
In dentistry it is of great interest to achieve good sealing interzones between tooth tissue and restoration materials to avoid, e. g. secondary caries. μXRF and CμXRF are suitable to investigate the elemental composition at these interzones in respect to diffusion of elements. Synchrotron X-ray refraction radiography (SXRR) and μCT measurements deliver highly resolved structural information and make structural changes such as micro cracks within the filling and the tooth tissue visible. The presented measurements are part of the DFG funded project IXdent (Integrative X-ray techniques for chemical and structural characterizations of dental interzones.)
The depth-resolved CμXRF measurements are affected by absorption effects, making a quantitative investigation of the interzone in depth difficult. Full 3D quantification of heterogenous samples requires a complete model including dark matrix and density for each voxel. The combination of different techniques paves the way for a quantitative analysis of dental interzones.
Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution.
With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research.
The microstructure has a great influence on short fatigue crack growth in metallic materials. Laser-based Powder Bed Fusion AlSi10Mg alloys exhibit in the as-built condition a fine fibrous Si structure and a supersaturated solid solution of Si in the α-Al matrix, which is significantly modified by heat treatments starting already at temperatures under 260 °C. This study focuses on the influence of post-process heat treatments on the microstructural evolution and the resulting fatigue crack growth resistance. As compared to the as-built condition, two heat treatments at 265 °C/1 h and at 300 °C/2 h are found to be beneficial to the fatigue crack growth resistance of the investigated material.
One of the main advantages of metal additive manufacturing (MAM) techniques is their ability to produce components with site-specific microstructural features. Nevertheless, microstructural defects and lack of repeatability are still major concerns in MAM. In this study, a laser powder bed fusion (PBF-LB/M) IN718 material, produced using two different scan length vectors, is investigated using Bragg-edge neutron 2D imaging (BENI) combined with electron backscatter diffraction (EBSD) analysis. BENI is able to detect, on a macroscopic scale, process-induced changes in texture in a large field of view covering the entire sample (20×80 mm2). In addition, high-resolution BENI (HR-BENI), with a pixel size of 12.8 µm, provides a micro-scale examination of the local variations of texture and grain morphology, otherwise undistinguishable using the standard resolution. As such, HR-BENI offers a straightforward and detailed way of screening the integrity of MAM parts at cm-length scales.
Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, leading to potential efficiency and performance improvements. However, the rapid cooling rates associated with the process consequently leads to the generation of high magnitude residual stresses (RS). Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterization of these RS is essential for safety related engineering application and supporting the development of reliable numerical models. Diffraction-based methods for RS analysis using high energy synchrotron X-rays and neutrons enable non-destructive spatially resolved characterization of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research conducted by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys. Special focus will be given to the challenges posed by textured LPBF materials for the reliable choice of the diffraction elastic constants (DECs), which is crucial to the accurate calculation of the level of RS.
The high cooling rates (~106 K/s) occurring during Laser Powder Bed Fusion (PBF-LB/M) of AlSi10Mg induce to the formation of a fine nanometric silicon network in the as-built condition. Such unprecedented microstructure enhances the mechanical strength when compared to equivalent as-cast materials. Nevertheless, PBF-LB/M also leads to high magnitude residual stress (RS) due to the extreme localized temperature gradients. The presence of RS can be detrimental to the fatigue life of engineering components, and great efforts are focused on understanding their generation and evolution after post-process heat treatments. Typically, T6 heat treatments are used to mitigate RS and improve mechanical performances by Mg2Si precipitation during ageing at 160-180°C. Nevertheless, the solutionizing at 500-540°C vanishes the fine silicon network, leading to the formation of micrometric (average of ~2-5 µm) polygonal Si particles, similar to those observed in T6 heat-treated Al-Si cast materials. Therefore, the aim of this work is to evaluate the ability of two so-called low temperature heat treatments (i.e., at 265°C and 300°C) to mitigate RS while retaining the fine as-built microstructure inherent to PBF-LB/M AlSi10Mg. The fatigue behavior of the as-built material is subsequently compared to the two low temperature conditions.
Synchrotron X-ray computed tomography (SXCT) at BAMline has been paired with in-situ tensile loading to monitor damage evolution in LPBF Metal Matrix Composite (MMC) 7017 Aluminium alloy + 3 wt% Zr + 0.5 wt% TiC. The processing of the material leads formation to different categories of Zr-rich inclusions, precipitates and defects. In-situ SXCT test disclosed the critical role of the pre-cracks in the reinforcement phases in the failure mechanisms of LPBF MMC. The damage was initiated from lack-of-fusion defects and cracks propagated through coalescence with other defects.
LTCCs (Low-temperature co-fired ceramics) consist of three-dimensionally distributed, hermetically bonded ceramic and metallic components with structure sizes within [10; 100] µm. A non-destructive imaging technique is needed that provides 3D, sharp, high-contrast resolution of these structures, as well as porosity and defect analysis, which is made difficult by the very different X-ray absorption coefficients of the individual components of the microstructure. A HDR method is being developed that allows a combination of different tomograms, each with X-ray energies adapted to individual materials.
Quantification of Deep Discharge Mechanism in a Li-Ion Battery by operando X-ray Computed Tomography
(2023)
Lithium-ion batteries connected in series are prone to an electrical abuse called over discharge. We present a comprehensive investigation of the over discharge abuse mechanism in lithium-ion batteries using operando non-destructive imaging. The study focuses on understanding the behavior of copper dissolution and deposition during over discharge, which can lead to irreversible capacity loss and internal short circuits. By utilizing synchrotron X-ray computed tomography (SXCT), the concentration of dissolved and deposited copper per surface area is quantified as a function of depth of discharge (DoD).
The osseointegration in/around additively manufactured (AM) lattice structures of a new titanium alloy, Ti–19Nb–14Zr, was evaluated. Different lattices with increasingly high sidewalls gradually closing them were manufactured and implanted in sheep. After removal, the bone–interface implant (BII) and bone–implant contact (BIC) were studied from 3D X-ray computed tomography images. Measured BII of less than 10 µm and BIC of 95% are evidence of excellent osseointegration.
Since AMnaturally leads to a high-roughness surface finish, the wettability of the implant is increased.
The new alloy possesses an increased affinity to the bone. The lattice provides crevices in which the biological tissue can jump in and cling. The combination of these factors is pushing ossification beyond its natural limits. Therefore, the quality and speed of the ossification and osseointegration in/around these Ti–19Nb–14Zr laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required. Thus, this new titanium alloy and such laterally closed lattice structures are appropriate candidates to be implemented in a new generation of implants.
Functionally graded porous scaffolds (FGPS) constructed with pores of different size arranged as spatially continuous structure based on sheet-based gyroid with three different scaling factors of 0.05, 0.1 and 0.2 were produced by electron beam powder bed fusion. The pore dimensions of the obtained scaffolds satisfy the values required for optimal bone tissue ingrowth. Agglomerates of residual powder were found inside all structures, which required post-manufacturing treatment. Using X-ray Computed Tomography powder agglomerations were visualized and average wall thickness, wall-to-wall distances, micro- and macro-porosities were evaluated. The initial cleaning by powder recovery system (PRS) was insufficient for complete powder removal. Additional treatment by dry ultrasonic vibration (USV) was applied and was found successful for gyroids with the scaling factors of 0.05 and 0.1. Mechanical properties of the samples, including quasi-elastic gradients and first maximum compressive strengths of the structures before and after USV were evaluated to prove that additional treatment does not produce structural damage. The estimated quasi-elastic gradients for gyroids with different scaling factors lie in a range between 2.5 and 2.9 GPa, while the first maximum compressive strength vary from 52.5 for to 59.8 MPa, compressive offset stress vary from 46.2 for to 53.2 MPa.
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
In this study, we present an enhanced deep learning framework for the prediction of porosity based on thermographic in-situ monitoring data of laser powder bed fusion processes. The manufacturing of two cuboid specimens from Haynes 282 (Ni-based alloy) powder was monitored by a short-wave infrared camera. We use thermogram feature data and x-ray computed tomography data to train a convolutional neural network classifier. The classifier is used to perform a multi-class prediction of the spatially resolved porosity level in small sub-volumes of the specimen bulk.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenkung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
The peak broadening in neutron diffraction experiments on tensile specimens of pure Al (99.8%) and an Al-Mg alloy pre-deformed at different creep strains is analysed. These results are combined with the kernel angular misorientation of electron backscatter diffraction data from the creep-deformed microstructures. It is found that differently oriented grains possess different microstrains. These microstrains vary with creep strain in pure Al, but not in the Al-Mg alloy. It is proposed that this behaviour can explain the power-law breakdown in pure Al and the large creep strain observed in Al-Mg. The present findings further corroborate a description of the creep-induced dislocation structure as a fractal, predicated on previous work.
The prediction of porosity is a crucial task for metal based additive manufacturing techniques such as laser powder bed fusion. Short wave infrared thermography as an in-situ monitoring tool enables the measurement of the surface radiosity during the laser exposure. Based on the thermogram data, the thermal history of the component can be reconstructed which is closely related to the resulting mechanical properties and to the formation of porosity in the part. In this study, we present a novel framework for the local prediction of porosity based on extracted features from thermogram data. The framework consists of a data pre-processing workflow and a supervised deep learning classifier architecture. The data pre-processing
workflow generates samples from thermogram feature data by including feature information from multiple subsequent layers.
Thereby, the prediction of the occurrence of complex process phenomena such as keyhole pores is enabled. A custom convolutional neural network model is used for classification. Themodel is trained and tested on a dataset from thermographic in-situ monitoring of the manufacturing of an AISI 316L stainless steel test component. The impact of the pre-processing parameters and the local void distribution on the classification performance is studied in detail. The presented model achieves an accuracy of 0.96 and an f1-Score of 0.86 for predicting keyhole porosity in small sub-volumes with a dimension of (700 × 700 × 50) μm3. Furthermore, we show that pre-processing parameters such as the porosity threshold for sample
labeling and the number of included subsequent layers are influential for the model performance. Moreover, the model prediction is shown to be sensitive to local porosity changes although it is trained on binary labeled data that disregards the actual sample porosity.
Adopting X-ray computed tomography (XCT) for ex-situ characterization of battery materials has gained interest in the past decade. The main goal of this paper is to demonstrate the effectiveness of several X-ray computer tomography techniques to study commercial batteries. General guidelines are provided to select the most suitable imaging equipment and parameters for investigations of lithium-ion batteries, spanning the length scales from cell to electrode, down to particle level. Relevantly, such parameters would also be suitable for operando experiments.
Safety mechanisms and manufacturing inconsistencies at cell level as well as defects and inhomogeneity in cathode and anode is illustrated and quantified. Furthermore, relation of beam energy and sample-detector-distance on contrast retrieved from attenuation and phase shift is inspected using Synchrotron XCT.