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Automated Wall Thickness Evaluation for Turbine Blades Using Robot-Guided Ultrasonic Array Imaging
(2024)
Nondestructive testing has become an essential part of the maintenance of modern gas turbine blades and vanes since it provides an increase in both safety against critical failure and efficiency of operation. Targeted repairs of the blade’s airfoil require localized wall thickness information. This information, however, is hard to obtain by nondestructive testing due to the complex shapes of surfaces, cavities, and material characteristics. To address this problem, we introduce an automated nondestructive testing system that scans the part using an immersed ultrasonic array probe guided by a robot arm. For imaging, we adopt a two-step, surface-adaptive Total Focusing Method (TFM) approach.
For each test position, the TFM allows us to identify the outer surface, followed by calculating an adaptive image of the interior of the part, where the inner surface’s position and shape are obtained. To handle the large volumes of data, the surface features are automatically extracted from the TFM images using specialized image processing algorithms. Subsequently, the collection of 2D extracted surface data is merged and smoothed in 3D space to form the outer and inner surfaces, facilitating wall thickness evaluation. With this approach, representative zones on two gas turbine vanes were tested, and the reconstructed wall thickness values were evaluated via comparison with reference data from an optical scan. For the test zones on two turbine vanes, average errors ranging from 0.05 mm to 0.1 mm were identified, with a standard deviation of 0.06–0.16 mm.
An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests.
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.
AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management.
In this work, the thermal properties of ternary Li₃ₓCo₇₋₄ₓSb₂₊ₓO₁₂ solid solutions are studied for different concentrations in the range 0 ≤ x ≤ 0.7. Samples are elaborated at four different sintering temperatures: 1100, 1150, 1200 and 1250 °C. The effect of increasing the content of Li⁺ and Sb⁵⁺, accompanied by the reduction of Co²⁺, on the thermal properties is studied. It is shown that a thermal diffusivity gap, which is more pronounced for low values of x, can be triggered at a certain threshold sintering temperature (around 1150 °C in this study). This effect is explained by the increase of contact area between adjacent grains. Nevertheless, this effect is found to be less pronounced in the thermal conductivity. Moreover, a new framework for heat diffusion in solids is presented that establishes that both the heat flux and the thermal energy (or heat) satisfy a diffusion equation and therefore highlights the importance of thermal diffusivity in transient heat conduction phenomena.
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.
Offshore wind turbines continuously increase in size and weight and demand adequate offshore foundations concepts like monopiles, tripods, or jackets. These components are typically constructed using submerged arc welding (SAW) with high-strength thick steel plates like the S420ML. During welding, the occurrence of delayed hydrogen-assisted cracking (HAC) must be anticipated. HAC is a critical combination of the local hydrogen concentration within a susceptible microstructure under certain mechanical load, i.e., the occurring (welding) residual stresses. The welding sequence of the thick-walled plates complicates the residual stress distribution due to the necessary repeated thermal cycling, i.e., welding seam/layer deposition to fill the joint. For that purpose, SAW with two-wire-technique was used to weld a specially designed and prototype-like mock-up of a real component with a thickness of 50 mm, filled with over 20 passes and a seam length of 1000 mm. Additional welded stiffeners simulated the effect of a high restraint, to achieve critical HAC conditions. The necessity of a minimum waiting time (MWT) before the NDT can be conducted (to exclude HAC) was critically verified by the application of ultrasonic testing of the welded joint at different time-steps of the NDT of up to 48 h after the completion welding. The residual stresses were determined by a robot XRD goniometer. Tensile residual stresses up to the yield limit are found both in the weld metal and in the heat-affected zone. Numerical modeling allowed the qualitative estimation of the hydrogen diffusion in the weld. No noticeable HAC occurrence was identified and confirms the high cracking resistance of the investigated material. Finally, the applicability of the MWT concept should be critically discussed.
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.
This data article introduces a dataset comprising 1630 alkali-activated concrete (AAC) mixes, compiled from 106 literature sources. The dataset underwent extensive curation to address feature redundancy, transcription errors, and duplicate data, yielding refined data ready for further data-driven science in the field of AAC, where this effort constitutes a novelty. The carbon footprint associated with each material used in the AAC mixes, as well as the corresponding CO2 footprint of every mix, were approximated using two published articles. Serving as a foundation for future expansions and rigorous data applications, this dataset enables the characterization of AAC properties through machine learning algorithms or as a benchmark for performance comparison among different formulations. In summary, the dataset provides a resource for researchers focusing on AAC and related materials and offers insights into the environmental benefits of substituting traditional Portland concrete with AAC.
Large-language models (LLMs) such as GPT-4 caught the interest of many scientists. Recent studies suggested that these models could be useful in chemistry and materials science. To explore these possibilities, we organized a hackathon. This article chronicles the projects built as part of this hackathon. Participants employed LLMs for various applications, including predicting properties of molecules and materials, designing novel interfaces for tools, extracting knowledge from unstructured data, and developing new educational applications. The diverse topics and the fact that working prototypes could be generated in less than two days highlight that LLMs will profoundly impact the future of our fields. The rich collection of ideas and projects also indicates that the applications of LLMs are not limited to materials science and chemistry but offer potential benefits to a wide range of scientific disciplines.
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.
The capability to produce complexly and individually shaped metallic parts is one of the main advantages of the laser powder bed fusion (PBF LB/M) process. Development of material and machine specific process parameters is commonly based on results acquired from small cubic test coupons of about 10 mm edge length. Such cubes are usually used to conduct an optimization of process parameters to produce dense material. The parameters are then taken as the basis for the manufacturing of real part geometries. However, complex geometries go along with complex thermal histories during the manufacturing process, which can significantly differ from thermal conditions prevalent during the production of simply shaped test coupons. This may lead to unexpected and unpredicted local inhomogeneities of the microstructure and defect distribution in the final part and it is a root cause of reservations against the use of additive manufacturing for the production of safety relevant parts. In this study, the influence of changing thermal conditions on the resulting melt pool depth of 316L stainless steel specimens is demonstrated. A variation of thermo-graphically measured intrinsic preheating temperatures was triggered by an alteration of inter layer times and a variation of cross section areas of specimens for three distinct sets of process parameters. Correlations between the preheating temperature, the melt pool depth, and occurring defects were analyzed. The limited expressiveness of the results of small density cubes is revealed throughout the systematic investigation. Finally, a clear recommendation to consider thermal conditions in future process parameter optimizations is given.
We introduce a novel approach that combines the scaled boundary finite element method (SBFEM) with a mortar coupling to enhance the computational modelling of elastic wave propagation and interaction with local features in the ultrasonic range. The key objective is to achieve decoupling between different regions of interest, enabling independent meshes for the zones where waves either propagate or interact with localised discontinuities in the elastic media. This decoupling allows us to exploit the benefits offered by various SBFEM formulations. Thus, we can select the most suitable solution for each specific region. An important concept we emphasise is the differentiation between the near field and far field regions. The near field encompasses zones where the precise representation of small features compared to the wavelength is crucial. At the same time, the far field comprises homogeneous regions where the waves propagate without interactions, eventually radiating towards infinity if the domain is unbounded. By separating these two zones, we can improve the computational performance by employing finer discretisation only where necessary. Furthermore, this decoupling enables the reuse of far field models in parametric analyses, making it highly valuable for scenarios focused particularly on local elastic wave interactions. This approach offers considerable potential in such cases. The modelling technique is validated, and its potential is demonstrated through practical applications.
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.
This paper presents a novel approach for developing sustainable building materials through Sequential Learning. Data sets with a total of 1367 formulations of different types of alkali-activated building materials, including fly ash and blast furnace slag-based concrete and their respective compressive strength and CO2-footprint, were compiled from the literature to develop and evaluate this approach. Utilizing this data, a comprehensive computational study was undertaken to evaluate the efficacy of the proposed material design methodologies, simulating laboratory conditions reflective of real-world scenarios. The results indicate a significant reduction in development time and lower research costs enabled through predictions with machine learning. This work challenges common practices in data-driven materials development for building materials. Our results show, training data required for data-driven design may be much less than commonly suggested. Further, it is more important to establish a practical design framework than to choose more accurate models. This approach can be immediately implemented into practical applications and can be translated into significant advances in sustainable building materials development.
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.
Many advanced materials consist of fibers. They are used as nonwovens, fabrics, or in composite materials. Characterization of individual fibers allows us to predict resulting material properties. We present a measurement setup and analysis software to characterize individual, micrometer-sized fibers fast and reliably. The setup is based on the lock-in thermography principle. Thermal diffusivity values of seven reference samples agree very well with previously reported values. We use our setup to investigate critical measurement parameters like excitation frequency, excitation power, pixel size, and fiber orientation. Our results show that fibers with subpixel diameters can be measured even if they are not aligned. However, special care has to be taken to choose an adequate excitation power. Measurements at high intensities can underestimate thermal diffusivity even though the raw data looks reasonable. By automatically measuring at different excitation powers, our setup solves this issue.
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.
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.
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.
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 application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE.
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.
The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis.
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.
Fused filament fabrication (FFF) is a material extrusion-based technique often used in desktop 3D printers. Polymeric filaments are melted and are extruded through a heated nozzle to form a 3D object in layers. The extruder temperature is therefore a key parameter for a successful print job but also one of the main emission driving factors as harmful pollutants (e.g., ultrafine particles) are formed by thermal polymer degradation. The awareness of potential health risks has increased the number of emission studies in the past years. However, studies usually refer their calculated emission data to the printer set extruder temperature for comparison purposes. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperature and found significant temperature deviations to the displayed set temperature among printer models. Our result shows that printing the same filament feedstocks with three different printer models and with identical printer set temperature resulted in a variation in particle emission of around two orders of magnitude. A temperature adjustment has reduced the variation to approx. one order of magnitude. Thus, it is necessary to refer the measured emission data to the actual extruder temperature as it poses a more accurate comparison parameter for evaluation of the indoor air quality in user scenarios or for health risk assessments.
The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications.
The electron backscatter diffraction (EBSD) technique is used to investigate the dislocation structures formed after steady-state creep deformation of an Al-3.85%Mg alloy. This material is crept at two different stress levels, corresponding to the so-called power-law and power-law breakdown regimes. The results show that, regardless of the creep stress level, the strain tends to localize, leading to the formation of intragranular bands. The thickness of such bands is larger when the material is tested at loads corresponding to the power-law breakdown. This suggests enhanced diffusion by dislocation pipes.
Performance of calcium phosphate cements in the augmentation of sheep vertebrae - An ex vivo study
(2021)
Oil-based calcium phosphate cement (Paste-CPC) shows not only prolonged shelf life and injection times, but also improved cohesion and reproducibility during application, while retaining the advantages of fast setting, mechanical strength, and biocompatibility. In addition, poly(L-lactideco-glycolide) (PLGA) fiber reinforcement may decrease the risk for local extrusion. Bone defects (diameter 5 mm; depth 15 mm) generated ex vivo in lumbar (L) spines of female Merino sheep (2–4 years) were augmented using: (i) water-based CPC with 10% PLGA fiber reinforcement (L3); (ii) Paste-CPC (L4); or (iii) clinically established polymethylmethacrylate (PMMA) bone cement (L5). Untouched (L1) and empty vertebrae (L2) served as controls. Cement performance was analyzed using micro-computed tomography, histology, and biomechanical testing. Extrusion was comparable for Paste-CPC(-PLGA) and PMMA, but significantly lower for CPC + PLGA. Compressive strength and Young’s modulus were similar for Paste-CPC and PMMA, but significantly higher compared to those for empty defects and/or CPC + PLGA. Expectedly, all experimental groups showed significantly or numerically lower compressive strength and Young’s modulus than those of untouched controls. Ready-to-use Paste-CPC demonstrates a performance similar to that of PMMA, but improved biomechanics compared to those of water-based CPC + PLGA, expanding the therapeutic arsenal for bone defects. O, significantly lower extrusion of CPC + PLGA fibers into adjacent lumbar spongiosa may help to reduce the risk of local extrusion in spinal surgery.
This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material.
While laser powder-bed fusion has overcome some of the design constraints of conventional manufacturing methods, it requires careful selection of process parameters and scan strategies to obtain favorable properties. Here we show that even simple scan strategies, complex ones being inevitable when printing intricate designs, can inadvertently produce local alterations of the microstructure and preferential grain orientation over small areas – which easily remain unnoticed across the macroscale. We describe how a combined usage of neutron imaging and electron backscatter diffraction can reveal these localized variations and explain their origin within cm-sized parts. We explain the observed contrast variations by linking the neutron images to simulated data, pole figures and EBSD, providing an invaluable reference for future studies and showing that presumably minor changes of the scan strategy can have detrimental effects on the mechanical properties. In-situ tensile tests reveal that fracture occurs in a region that was re-melted during the building process.
Electron Beam Powder Bed Fusion-manufactured (E-PBF) porous components with narrow pores or channels and rough walls or struts can be filled with trapped powder after the manufacturing process. Adequate powder removal procedures are required, especially for high-density porous structures. In the present research, sheetbased porous structures with different thicknesses based on triply periodic minimal surfaces fabricated by EPBF were subjected to different post-processing methods, including a traditional powder recovery system for EPBF, chemical etching and ultrasound vibration-assisted powder removal. Wall thickness, internal defects, microstructure and morphology features, powder distribution inside the specimens, mechanical properties and deformation modes were investigated. A powder recovery system could not remove all residual powder from dense structures. In turn, chemical etching was effective for surface morphology changes and subsurface layers elimination but not for powder removal, as it affected the wall thickness, considerably influencing the mechanical properties of the whole structure. The ultrasound vibration method was quite effective for the removal of residual powder from sheet-based TMPS structures and without a severe degradation of mechanical properties. 10.1016/j.msea.2022.144479 Ultrasound vibration also caused grain refinement.
A steel pipeline segment of 2.5 m length was subjected to quasi-static four-point bending load in three steps for studying the initial cracking and damage accumulation based on the Acoustic Emission (AE) technique and by the direct current potential drop (DCPD) technique. For the latter, a new post-test analysis method was established.
AE is found more sensitive to crack initiation than DCPD. Formation of mesoscopic and macroscopic cracks as well as their closure and the resulting friction generate weighted peak frequencies below 400 kHz, whereas microscopic cracking produces AE with broad band spectra identifiable by weighted peak frequencies above 400 kHz. Critical states alike the maximum load level and the leak opening were accompanied by peak amplitudes above 85 dBAE. This rather fundamental study provides a data base for possibly developing advanced strategies of detection and alarm systems based on acoustic monitoring of pipelines, or at least, steel structures.
Influence of a 265 °C heat treatment on the residual stress state of a PBF-LB/M AlSi10Mg alloy
(2022)
Laser Powder Bed Fusion (PBF-LB/M) additive manufacturing (AM) induces
high magnitude residual stress (RS) in structures due to the extremely heterogeneous cooling and heating rates. As the RS can be deleterious to the fatigue resistance of engineering components, great efforts are focused on understanding their generation and evolution after post-process heat treatments. In this study, one of the few of its kind, the RS relaxation induced in an as-built PBF-LB/M AlSi10Mg material by a low-temperature heat treatment (265 °C for 1 h) is studied by means of X-ray and neutron diffraction. Since the specimens are manufactured using a baseplate heated up to 200 °C, low RS are found in the as-built condition. After heat treatment a redistribution of the RS is observed, while their magnitude remains constant. It is proposed that the redistribution is induced by a repartition of stresses between the a-aluminium matrix and the silicon phase, as the morphology of the silicon phase is affected by the heat treatment. A considerable scatter is observed in the neutron diffraction RS profiles, which is principally correlated to the presence (or absence) of pockets of porosity developed at the borders of the chessboard pattern.
Influence of the Composition on the Compressive Behaviour of a Semi-Metallic Brake-Pad Material
(2022)
The contact interface between the rotation and static part of a friction brake is central to the optimal functioning of the brake system due to the occurrence of heat dissipation, mechanical interaction and thermal exchanges. Generally, braking performances are evaluated by the energetic efficiency and wear rates of the contact surface. However, the compressive behaviour of the contact materials has also a significant contribution to the overall performances. In this work, the meso- and microscopic compressive behaviour of a sintered semi-metallic brake-pad material is investigated mainly via compression testing coupled with Digital Image Correlation (DIC) technique, as well as optical and scanning electron microscopy (SEM) analysis. The composition of a reference material (RM) is simplified to a selection of nine components, as opposed to up to thirty components typically used in commercial brake-pad materials. The retained components are considered as the most crucial for safe-operating performances. At the studied stress levels, the RM material is flexible (E = 5330 MPa), deformable (Ezz−plastic = −0.21%), and exhibits hysteresis loops. Subsequently, the contribution to the mechanical response of each individual component is investigated by producing the so-called dissociated materials, where the number of components is, at a time, further reduced. It is observed that the macroscopic behaviour is mainly controlled by the content (i.e., size distribution, shape and nature) of graphite particles, and that the hysteresis is only related to one of the two types of graphite used (G2 particles). Moreover, RM containing 13 wt% of G2 particles embedded in a relatively soft matrix (10.86 GPa) is able to increase the hysteresis (by 35%) when compared to the dissociated material containing 20 wt% of G2 particles which is embedded in a stiffer matrix (E = 106 GPa).
Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale.
The printability of artificial defects inside the additively manufactured laser powder bed fusion (LPBF) 316L stainless steel is investigated. The printing parameters of the LPBF process are optimized to produce artificial defects with reproducible sizes at desired positions while minimizing redundant porosity. The smallest obtained artificial defect is 90 μm in diameter. The accuracy of the geometry of the printed defect depends on both the height and the diameter in the input model. The effect of artificial defects on the very-high-cycle fatigue (VHCF) behavior of LPBF 316L stainless steel is also studied. The specimens printed with artificial defects in the center are tested under VHCF using an ultrasonic machine. Crack initiation is accompanied by the formation of a fine granular area (FGA), typical of VHCF. Despite the presence of relatively large artificial defects, FGA formation is observed around accidental natural printing defects closer to the surface, which can still be considered as internal. The causes for this occurrence are discussed.
Direct Laser Writing (DLW) and X-ray computed tomography (XCT) both offer unique possibilities in their respective fields. DLW produces full three-dimensional (3D) polymer structures on the microscale with resolutions below 100 nm. The fabricated structures can be analysed by XCT or X-ray microscopy (XRM), which incorporates additional X-ray lenses, in three dimensions down to a minimal basic spatial resolution of about 500 nm or 50 nm, respectively. In this work, two different DLW structures are analysed via XCT. Internal defects are detected and analysed for the purpose of quality control. Defects and structures with sizes down to 1.5 µm are successfully analysed. A 3D reconstruction and internal, hidden features of the fabricated structures are shown and discussed. In a first-of-its-kind study, we demonstrate the detectability of a single-voxel line inside a fabricated structure that would not be detectable with SEM or light microscopy. Furthermore, the direct fabrication on a PET substrate is shown to overcome the high X-ray absorbance of commonly used glass substrates. Attenuation spectra of SZ2080 and glass substrates are compared to a fabrication route direct on a 170 µm PET foil. The practical aspects of XCT measurements for DLW structures on different substrates will be discussed.
Shape memory alloy structures for actuator and vibration damper applications may be manufactured using wire arc additive manufacturing (W AAM), which is one of the additive manufacturing technologies. Multilayer deposition causes heat accumulation during W AAM, which rises the preheat temperature of the previously created layer. This leads to process instabilities, which result in deviations from the desired dimensions and mechanical properties changes. During W AAM deposition of the wall structure, a systematic research is carried out by adjusting the interlayer delay from 10 to 30 s. When the delay period is increased from 10 to 30 s, the breadth decreases by 45% and the height increases by 33%. Grain refinement occurs when the interlayer delay duration is increased, resulting in better hardness, phase transformation temperature, compressive strength, and shape recovery behavior. This study shows how the interlayer delay affects the behavior of W AAM-built nickel-titanium alloy (NiTi) structures in a variety of applications.
During their life span, concrete structures interact with many kinds of external mechanical loads. Most of these loads are considered in advance and result in reversible deformations. Nevertheless, some of the loads cause irreversible, sometimes unnoticed changes below the macroscopic scale depending on the type and dimension of the impact. As the functionality of concrete structures is often relevant to safety and society, their condition must be known and, therefore, assessed on a regular basis. Out of the spectrum of non-destructive monitoring methods, Coda Wave Interferometry using embedded ultrasonic sensors is one particularly sensitive technique to evaluate changes to heterogeneous media. However, there are various influences on Coda waves in concrete, and the interpretation of their superimposed effect is ambiguous. In this study, we quantify the relations of uniaxial compression and uniaxial tension on Coda waves propagating in normal concrete. We found that both the signal correlation of ultrasonic signals as well as their velocity variation directly reflect the stress change in concrete structures in a laboratory environment. For the linear elastic range up to 30% of the strength, we calculated a velocity variation of −0.97‰/MPa for compression and 0.33%/MPa for tension using linear regression. In addition, these parameters revealed even weak irreversible changes after removal of the load. Furthermore, we show the time-dependent effects of shrinkage and creep on Coda waves by providing the development of the signal parameters over time during half a year together with creep recovery. Our observations showed that time-dependent material changes must be taken into account for any comparison of ultrasonic signals that are far apart in time. The study’s results demonstrate how Coda Wave Interferometry is capable of monitoring stress changes and detecting even small-size microstructural changes. By indicating the stated relations and their separation from further impacts, e.g., temperature and moisture, we anticipate our study to contribute to the qualification of Coda Wave Interferometry for its application as an early-warning system for concrete structures.
Additive manufacturing (AM) techniques have risen to prominence in many industrial sectors. This rapid success of AM is due to the freeform design, which offers enormous possibilities to the engineer, and to the reduction of waste material, which has both environmental and economic advantages. Even safety-critical parts are now being produced using AM. This enthusiastic penetration of AM in our daily life is not yet paralleled by a thorough characterization and understanding of the microstructure of materials and of the internal stresses of parts. The same holds for the understanding of the formation of defects during manufacturing. While simulation efforts are sprouting and some experimental techniques for on-line monitoring are available, still little is known about the propagation of defects throughout the life of a component (from powder to operando/service conditions). This Issue was aimed at collecting contributions about the advanced characterization of AM materials and components (especially at large-scale experimental facilities such as Synchrotron and Neutron sources), as well as efforts to liaise on-line process monitoring to the final product, and even to the component during operation. The goal was to give an overview of advances in the understanding of the impacts of microstructure and defects on component performance and life at several length scales of both defects and parts.
The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed.
Till now application of printed magnetoelectronics is hindered by lack of large area exchange coupled metallic multilayers required to produce printable magneto-sensory inks. Large-scale roll-to-roll (R2R) fabrication process is an attractive approach owing to its capabilities for high volume, high throughput, and large area manufacturing. Precise and high performance R2R sputtering technology is developed to fabricate large area giant magnetoresistive (GMR) thin-films stacks that contain 30 metallic bilayers prepared by continuous R2R sputtering of Co and Cu sequential on a hundred meters long polyethylene terephthalate (PET) web. The R2R sputtered Co/Cu multilayer on a 0.2 × 100 m2 PET web exhibits a GMR ratio of ≈40% achieving the largest area exchange coupled room temperature magneto-sensitive system demonstrated to date. The prepared GMR thin-film is converted to magnetosensitive ink that enables printing of magnetic sensors with high performance in a cost-efficient way, which promotes integration with printed electronics. An average GMR ratio of ≈18% is obtained for 370 printed magnetic sensors. The realized precise R2R sputtering approach can also be extended to a wide range of hybrid thin-film material systems opening up a path for new functional inks applied with printing technologies.
In the present work, electron backscatter diffraction was used to determine the microscopic dislocation structures generated during creep (with tests interrupted at the steady state) in pure 99.8% aluminium. This material was investigated at two different stress levels, corresponding to the power-law and power-law breakdown regimes. The results show that the formation of subgrain cellular structures occurs independently of the crystallographic orientation. However, the density of these cellular structures strongly depends on the grain crystallographic orientation with respect to the tensile axis direction, with <111> grains exhibiting the highest densities at both stress levels. It is proposed that this behaviour is due to the influence of intergranular stresses, which is different in <111> and <001> grains.