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Organisationseinheit der BAM
- 8.5 Röntgenbildgebung (339) (entfernen)
Paper des Monats
- ja (1)
Eingeladener Vortrag
- nein (124)
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.