TY - JOUR A1 - Schröder, Jakob A1 - Fritsch, Tobias A1 - Ferrari, Bruno A1 - Altmann, Mika León A1 - Bruno, Giovanni A1 - Toenjes, Anastasiya T1 - Laser powder bed fusion: Defect type influences critical porosity re-growth during reheating after hot isostatic pressing N2 - Despite the remarkable product design flexibility offered by additive manufacturing (AM) techniques, such as laser powder bed fusion, AM processes are susceptible to the formation of defects. In this context, the control of process parameters and the application of post-processing treatments, such as hot isostatic pressing (HIP), are of paramount importance to achieve the desired mechanical properties. The present study investigates the effectiveness of HIP as a function of process parameters in laser powder bed fused Ti-6V-4Al (PBF-LB/Ti64) using X-ray computed tomography. The process parameters are modified to obtain reference samples with low porosity, lack of fusion defects, or keyhole porosity. In all instances, subsurface keyhole porosity was observed in the as-built parts. Moreover, it was found that the efficacy of pore closure is dependent on the specific defect type. In the case of low porosity and keyhole pores, HIP resulted in effective closure. Conversely, larger lack of fusion defects were not closed due to their interconnectivity and the entrapment of argon gas. Subsequent heat treatments above the β-transus temperature allowed the investigation of the impact of defect type on porosity re-growth. For the first time, we reveal that lack of fusion defects are affected by considerable pore re-growth during post-HIP heat treatments of PBF-LB/Ti64. Such phenomenon is driven by the increasing internal pore pressure and local creep deformation at high temperatures. In contrast, re-growth is limited in samples with low porosity or keyhole pores. KW - Additive Manufacturing KW - Hot Isostatic Pressing KW - Titanium KW - Laser Powder Bed Fusion KW - X-ray Computed Tomography KW - Heat Treatment KW - Porosity PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629289 DO - https://doi.org/10.1016/j.jmatprotec.2025.118839 VL - 340 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-62928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Han, Ying A1 - Fritsch, Tobias A1 - Hejazi, Bardia A1 - Ulbricht, Alexander A1 - Skrotzki, Birgit A1 - Bruno, Giovanni T1 - X-ray computed tomography quantifies primary phases and reveals crack morphology in high-cycle fatigue of aluminum alloy EN AW-2618A N2 - Since the introduction of high-strength aluminum alloys understanding their fatigue behavior is of high interest for the structural integrity of engineering components, in this context, the alloy EN AW-2618A gains its high strength from both nanometer size precipitates and micrometer size primary phases. The latter phases are often identified as crack initiation sites. In this study, it uses a combination of synchrotron and laboratory-based X-ray computed tomography to image and quantify such primary phases and the fatigue cracks appearing in interrupted tests. Based on the gray-level differences in the synchrotron X-ray computed tomography scans, this study is able to distinguish low- and high-absorbing particles. The dominant (volume fraction >99%) high absorbing primary phase can be quantified in good agreement with results of Thermo-Calc calculations. To image the fatigue crack, laboratory X-ray computed tomography scans are performed at different tensile loads to open the crack. The results show that with an appropriate crack opening tensile load, the fatigue crack morphology can be reliably revealed. Based on these results, the influence of the primary phases on the fatigue crack initiation and propagation are discussed. KW - X-ray computed tomography KW - Fatigue KW - Aluminum KW - Primary phases PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632724 DO - https://doi.org/10.1002/adem.202500235 SN - 1527-2648 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-63272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Reimann, T. A1 - Giovannelli, F. A1 - Rabe, Torsten T1 - Influence of pressure and dwell time on pressure‐assisted sintering of calcium cobaltite N2 - Calcium cobaltite Ca3Co4O9, abbreviated Co349, is a promising thermoelectric material for high‐temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure‐assisted sintering (PAS) are a possible future way for a cost‐effective mass‐production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape‐cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab‐direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry‐pressed, pressureless‐sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK2 at 800°C, which is 11 times higher than the dry‐pressed reference (30 MPa) from the same powder. KW - Hot pressing KW - Texture KW - Thermoelectric properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515973 DO - https://doi.org/https://doi.org/10.1111/jace.17541 SN - 0002-7820 VL - 104 IS - 2 SP - 917 EP - 927 PB - Wiley Periodicals LLC AN - OPUS4-51597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Altenburg, Simon A1 - Sprengel, Maximilian A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Fritsch, Tobias A1 - Mishurova, Tatiana A1 - Serrano-Munoz, Itziar A1 - Evans, Alexander A1 - Hofmann, M. A1 - Bruno, Giovanni T1 - Separation of the Formation Mechanisms of Residual Stresses in LPBF 316L N2 - Rapid cooling rates and steep temperature gradients are characteristic of additively manufactured parts and important factors for the residual stress formation. This study examined the influence of heat accumulation on the distribution of residual stress in two prisms produced by Laser Powder Bed Fusion (LPBF) of austenitic stainless steel 316L. The layers of the prisms were exposed using two different border fill scan strategies: one scanned from the centre to the perimeter and the other from the perimeter to the centre. The goal was to reveal the effect of different heat inputs on samples featuring the same solidification shrinkage. Residual stress was characterised in one plane perpendicular to the building direction at the mid height using Neutron and Lab X-ray diffraction. Thermography data obtained during the build process were analysed in order to correlate the cooling rates and apparent surface temperatures with the residual stress results. Optical microscopy and micro computed tomography were used to correlate defect populations with the residual stress distribution. The two scanning strategies led to residual stress distributions that were typical for additively manufactured components: compressive stresses in the bulk and tensile stresses at the surface. However, due to the different heat accumulation, the maximum residual stress levels differed. We concluded that solidification shrinkage plays a major role in determining the shape of the residual stress distribution, while the temperature gradient mechanism appears to determine the magnitude of peak residual stresses. KW - Additive Manufacturing KW - Laser Powder Bed Fusion KW - LPBF KW - AISI 316L KW - Online Process Monitoring KW - Thermography KW - Residual Stress KW - Neutron Diffraction KW - X-ray Diffraction KW - Computed Tomography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512903 DO - https://doi.org/10.3390/met10091234 VL - 10 IS - 9 PB - MDPI CY - Basel AN - OPUS4-51290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Advancing spray granulation by ultrasound atomization N2 - The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the Approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA. KW - Alumina KW - Granules KW - Spray drying KW - Ultrasound KW - Zirconia KW - Zirconia-toughened alumina PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510696 DO - https://doi.org/10.1111/ijac.13534 VL - 17 IS - 5 SP - 2212 EP - 2219 AN - OPUS4-51069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state. KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515060 DO - https://doi.org/10.1088/1757-899X/942/1/012035 SN - 1757-8981 SN - 1757-899X VL - 942 SP - 012035-1 EP - 012035-9 PB - IOP publishing CY - Bristol, UK AN - OPUS4-51506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadammal, Naresh A1 - Mishurova, Tatiana A1 - Fritsch, Tobias A1 - Serrano-Munoz, Itziar A1 - Kromm, Arne A1 - Haberland, C. A1 - Portella, Pedro Dolabella A1 - Bruno, Giovanni T1 - Critical role of scan strategies on the development of microstructure, texture, and residual stresses during laser powder bed fusion additive manufacturing N2 - Laser based powder bed fusion additive manufacturing offers the flexibility to incorporate standard and userdefined scan strategies in a layer or in between the layers for the customized fabrication of metallic components. In the present study, four different scan strategies and their impact on the development of microstructure, texture, and residual stresses in laser powder bed fusion additive manufacturing of a nickel-based superalloy Inconel 718 was investigated. Light microscopy, scanning electron microscopy combined with electron backscatter diffraction, and neutron diffraction were used as the characterization tools. Strong textures with epitaxially grown columnar grains were observed along the build direction for the two individual scan strategies. Patterns depicting the respective scan strategies were visible in the build plane, which dictated the microstructure development in the other planes. An alternating strategy combining the individual strategies in the successive layers and a 67◦ rotational strategy weakened the texture by forming finer microstructural features. Von Mises equivalent stress plots revealed lower stress values and gradients, which translates as lower distortions for the alternating and rotational strategies. Overall results confirmed the scope for manipulating the microstructure, texture, and residual stresses during laser powder bed fusion additive manufacturing by effectively controlling the scan strategies. KW - Additive manufacturing KW - Laser powder bed fusion KW - Nickel-based superalloys KW - Scan strategies KW - Residual stresses KW - Microstructure and texture PY - 2021 DO - https://doi.org/10.1016/j.addma.2020.101792 VL - 38 SP - 1792 PB - Elsevier B.V. AN - OPUS4-51944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, T. A1 - Kalinka, Gerhard A1 - Mieller, Björn T1 - Manufacturing and deformation behavior of alumina and zirconia helical springs at room temperature N2 - Ceramic helical springs with identical dimensions were produced by hard machining from alumina, alumina toughened zirconia (ATZ), and tetragonal zirconia polycrystals (TZP) stabilized with different oxides. According to the results of the spring constant determination under deformation rates of 3 mm/min, the deformation behavior of all ceramic springs obeys to Hook’s law. However, variation of the deformation rate, tests under constant load, and spring recovery behavior revealed differences in the deformation behavior of alumina, TZP, and ATZ springs. Alumina springs exhibited time-independent deformation in all tests. In contrast, anelastic deformation at room temperature was demonstrated in all springs containing TZP. This deformation is completely reversible over a period of several days. Anelastic behavior is particularly pronounced in Y-TZP springs, whereas Ce-TZP springs exhibit comparatively very low but still reliably detectable anelasticity. Oxygen vacancies in the TZP ceramic are considered the most likely explanation for the anelastic behavior of TZP springs at room temperature. KW - Alumina KW - Creep KW - Elastic properties KW - Zirconia PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571858 DO - https://doi.org/10.1111/jace.19085 SN - 0002-7820 SP - 1 EP - 14 PB - Wiley-Blackwell CY - Oxford [u.a.] AN - OPUS4-57185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Narsabadi, Hossein A1 - Vafaeenezhad, H. A1 - Klotz, U.E. A1 - Tiberto, D. A1 - Hosseinabadi, F. A1 - Mishurova, Tatiana A1 - Bruno, Giovanni A1 - Skrotzki, Birgit T1 - XCT-assisted micromechanical modeling of the effect of pores on the plastic deformation and mechanical characteristics of PBF-LB/M-produced copper alloys N2 - Due to the low absorption of fiber laser by copper particles, the laser-based powder bed fusion (PBF-LB/M) processing of copper components is accompanied by the development of different types of porosities within the printed samples. This research aims to assess the consequences of various process-induced pores on the me chanical characteristics and deformation of PBF-LB/M-produced copper alloys. Several copper alloys were processed using metal-coated particles and varied laser intensities, yielding samples with different types and amounts of porosities. For instance, CuCrZr alloys processed at 325 J/mm³ and 257 J/mm³ had 0.009 % and 1.117 % porosities, dominated by keyhole and lack-of-fusion pores, respectively. Moreover, PBF-LB/M pro cessing of Cr- and Nb-coated CuNi3SiCr particles accompanied by the generation of 0.004 % and 1.861 % porosities within the samples, predominantly featuring metallurgical and oxidation pores, respectively. Compression and nanoindentation tests revealed that the CuNi3SiCr alloy exhibited superior mechanical properties compared to the CuCrZr sample (nanoindentation hardness values 2.2 GPa and 1.4 GPa, respectively), while the presence of lack-of-fusion pores notably diminished their mechanical performance. X-ray computed tomography (XCT) reconstruction slices and scanning electron microscopy (SEM) images were then used for developing the representative volume elements (RVEs) based micromechanical models. The micromechanical simulations established a structure-property correlation that can simulate the compressive deformation and mechanical characteristics of PBF-LB/M-produced copper alloys as a function of their incorporated pore characteristics. Due to the closure of the pores at the first stages of deformation, samples with minimal keyhole and metallurgical porosities exhibited homogeneous plastic deformation. On the other side, based on the JohnsonCook model, strain concentration and crack propagation around the lack-of-fusion pores lead to damage initi ation in the printed samples at a strain level of 5 % KW - X-ray Computed tomography KW - Defects KW - Copper alloys KW - PBF-LB/M KW - Micromechanics PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624004 DO - https://doi.org/10.1016/j.msea.2025.147836 SN - 0921-5093 VL - 924 PB - Elsevier B.V. AN - OPUS4-62400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eddah, Mustapha A1 - Markötter, Henning A1 - Mieller, Björn A1 - Sintschuk, Michael A1 - Beckmann, Jörg A1 - Bruno, Giovanni T1 - Mitigation of DMM-induced stripe patterns in synchrotron X-ray radiography through dynamic tilting N2 - In synchrotron X-ray radiography, achieving high image resolution and an optimal signal-to-noise ratio (SNR) is crucial for the subsequent accurate image analysis. Traditional methods often struggle to balance these two parameters, especially in situ applications where rapid data acquisition is essential to capture specific dynamic processes. For quantitative image data analysis, using monochromatic X-rays is essential. A double multilayer monochromator (DMM) is successfully used for this aim at the BAMline, BESSY II (Helmholtz Zentrum Berlin, Germany). However, such DMMs are prone to producing an unstable horizontal stripe pattern. Such an unstable pattern renders proper signal normalization difficult and thereby causes a reduction of the SNR. We introduce a novel approach to enhance SNR while preserving resolution: dynamic tilting of the DMM. By adjusting the orientation of the DMM during the acquisition of radiographic projections, we optimize the X-ray imaging quality, thereby enhancing the SNR. The corresponding shift of the projection during this movement is corrected in post-processing. The latter correction allows a good resolution to be preserved. This dynamic tilting technique enables the homogenization of the beam profile and thereby effectively reduces noise while maintaining high resolution. We demonstrate that data captured using this proposed technique can be seamlessly integrated into the existing radiographic data workflow, as it does not need hardware modifications to classical X-ray imaging beamline setups. This facilitates further image analysis and processing using established methods. KW - Double multilayer monochromators KW - Synchrotron X-ray imaging KW - Signal normalization KW - BAMline KW - Dynamic tilting PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615049 DO - https://doi.org/10.1107/S1600577524008646 SN - 1600-5775 VL - 31 SP - 1551 EP - 1560 PB - International Union of Crystallography (IUCr) AN - OPUS4-61504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -