TY - JOUR A1 - Ferrari, Bruno A1 - Fantin, Andrea A1 - Said, D. A1 - Fitch, A. N. A1 - Suárez Ocano, Patricia A1 - Mishurova, Tatiana A1 - Roveda, Ilaria A1 - Kromm, Arne A1 - Darvishi Kamachali, Reza A1 - Bruno, Giovanni A1 - Evans, Alexander A1 - Requena, G. A1 - Agudo Jácome, Leonardo A1 - Serrano Munoz, Itziar T1 - The impact of scanning strategy on cell structures in PBF-LB/M/IN718: an in situ synchrotron x-ray diffraction study N2 - In additive manufacturing, any change of the process parameters, such as scanning strategy, directly affects the cooling rates, heat accumulation, and overall thermal history of the build. Consequently, parts built with different process parameters tend to have different levels of crystallographic texture, residual stress, and dislocation density. These features can influence the properties of the material and their development during post-processing operations. In this study, IN718 prisms were built by laser powder bed fusion (PBF-LB/M) using two different scanning strategies (continuous 67° rotations around the build direction, ROT, and alternating 0°/67° scans, ALT) to provide two different as-built conditions. In situ time-resolved synchrotron diffraction was performed during a solution heat treatment at 1027 °C for 1 h. Ex situ scanning electron microscopy was used to support and complement the in situ observations. An approach to quantify the effect of elemental microsegregation at the cell walls is developed based on the deconvolution of asymmetric γ-nickel matrix peaks. Following this approach, the scanning strategies are shown to affect the as-built fraction of cell walls in the material, resulting in a difference of approximately 5 %, in weight fraction, between ROT and ALT (19 % vs. 24 %, respectively). This microsegregation was observed to be rapidly homogenized during the heating ramp, and no significant changes to the peak shape in the γ peaks occurred during the isothermal part of the heat treatment, regardless of the scanning strategy. KW - Additive manufacturing KW - Inconel 718 KW - Synchrotron x-ray diffraction KW - Heat treatment KW - Laser powder bed fusion KW - Cellular microstructure PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650958 DO - https://doi.org/10.1016/j.jmrt.2025.11.214 SN - 2238-7854 VL - 41 SP - 593 EP - 608 PB - Elsevier B.V. AN - OPUS4-65095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mehta, B. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Markötter, Henning A1 - Bruno, Giovanni A1 - Hryha, E. A1 - Nyborg, L. A1 - Virtanen, E. T1 - Microstructure, mechanical properties and fracture mechanisms in a 7017 aluminium alloy tailored for powder bed fusion – laser beam N2 - 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. KW - Additive manufacturing KW - Powder bed fusion Laser beam KW - X-ray computed tomography KW - Strengthening mechanisms KW - Crack propagation KW - Zirconium PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568243 DO - https://doi.org/10.1016/j.matdes.2023.111602 SN - 0264-1275 VL - 226 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Mohr, Gunther A1 - Altenburg, Simon A1 - Oster, Simon A1 - Maierhofer, Christiane A1 - Bruno, Giovanni ED - Czujko, T. ED - Benedetti, M. T1 - Can Potential Defects in LPBF Be Healed from the Laser Exposure of Subsequent Layers? A Quantitative Study N2 - Additive manufacturing (AM) of metals and in particular laser powder bed fusion (LPBF) enables a degree of freedom in design unparalleled by conventional subtractive methods. To ensure that the designed precision is matched by the produced LPBF parts, a full understanding of the interaction between the laser and the feedstock powder is needed. It has been shown that the laser also melts subjacent layers of material underneath. This effect plays a key role when designing small cavities or overhanging structures, because, in these cases, the material underneath is feed-stock powder. In this study, we quantify the extension of the melt pool during laser illumination of powder layers and the defect spatial distribution in a cylindrical specimen. During the LPBF process, several layers were intentionally not exposed to the laser beam at various locations, while the build process was monitored by thermography and optical tomography. The cylinder was finally scanned by X-ray computed tomography (XCT). To correlate the positions of the unmolten layers in the part, a staircase was manufactured around the cylinder for easier registration. The results show that healing among layers occurs if a scan strategy is applied, where the orientation of the hatches is changed for each subsequent layer. They also show that small pores and surface roughness of solidified material below a thick layer of unmolten material (>200 µm) serve as seeding points for larger voids. The orientation of the first two layers fully exposed after a thick layer of unmolten powder shapes the orientation of these voids, created by a lack of fusion. KW - Computed tomography KW - Laser Powder Bed Fusion KW - In situ monitoring KW - infrared Thermography KW - Optical Tomography KW - Additive manufacturing KW - AISI 316L PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528778 DO - https://doi.org/10.3390/met11071012 VL - 11 IS - 7 SP - 1012 PB - MDPI CY - Basel AN - OPUS4-52877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evans, Alexander A1 - Schröder, Jakob A1 - Pirling, T. A1 - Ulbricht, Alexander A1 - Suárez Ocaño, Patricia A1 - Bruno, Giovanni T1 - Resolving the Subsurface Residual Stress Maximum in Laser Powder Bed-Fused 316L Stainless Steel by Diffraction-Based Analysis N2 - Laser powder bed fusion (PBF-LB/M) is a metal additive manufacturing process. Due to the complex nature of the layer-wise, repeated heating and cooling cycles, it tends to generate high-magnitude residual stresses. If not correctly understood and mitigated through in- or post-process approaches, these residual stresses can be detrimental as they are often tensile at the surface. However, determining the magnitude and location of peak tensile residual stresses is not trivial as they are often located subsurface. This work focuses on determining the magnitude and location of these deleterious tensile residual stresses in a PBF-LB/316L specimen. Two diffraction-based Methods are used to reveal the relationship between the residual stresses and the underlying microstructure. On the one hand, high spatial resolution Neutron diffraction is used to determine triaxial stresses from the bulk to a depth of 0.15 mm. On the other hand, laboratory X-ray diffraction coupled with electrolytical layer removal allows the biaxial residual stress depth profile to be probed from the surface to a depth of about 0.6 mm. The results show a good agreement between the two methods. The peak residual stress is shown to be 500 MPa, which appears as a plateau between 0.08 and 0.35 mm in depth. KW - Residual stress KW - Diffraction KW - Laser Powder Bed Fusion KW - 316L KW - Additive manufacturing KW - Microstructure KW - AGIL PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652138 DO - https://doi.org/10.1007/s11837-025-07719-y SN - 1543-1851 VL - 77 IS - 12 SP - 9726 EP - 9737 PB - Springer Nature AN - OPUS4-65213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Polatidis, E. A1 - Čapek, J. A1 - Mohr, Gunther A1 - Serrano-Munoz, Itziar A1 - Bruno, Giovanni T1 - Understanding the impact of texture on the micromechanical anisotropy of laser powder bed fused Inconel 718 N2 - 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. KW - Laser powder bed fusion KW - Additive manufacturing KW - Electron backscatter diffraction KW - Tensile testing KW - Diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555840 DO - https://doi.org/10.1007/s10853-022-07499-9 SN - 1573-4803 VL - 2022 IS - 57 SP - 15036 EP - 15058 PB - Springer Science + Business Media B.V. CY - Dordrecht AN - OPUS4-55584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Cabeza, Sandra A1 - Artzt, Katia A1 - Haubrich, J. A1 - Klaus, M. A1 - Genzel, Ch. A1 - Requena, G. A1 - Bruno, Giovanni T1 - An Assessment of Subsurface Residual Stress Analysis in SLM Ti-6Al-4V N2 - Ti-6Al-4V bridges were additively fabricated by selective laser melting (SLM) under different scanning speed conditions, to compare the effect of process energy density on the residual stress state. Subsurface lattice strain characterization was conducted by means of synchrotron diffraction in energy dispersive mode. High tensile strain gradients were found at the frontal surface for samples in an as-built condition. The geometry of the samples promotes increasing strains towards the pillar of the bridges. We observed that the higher the laser energy density during fabrication, the lower the lattice strains. A relief of lattice strains takes place after heat treatment. KW - Selective laser melting KW - Additive manufacturing KW - Heat treatment KW - Ti-6Al-4V KW - Synchrotron X-ray diffraction KW - Residual stress PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395759 DO - https://doi.org/10.3390/ma10040348 SN - 1996-1944 VL - 10 IS - 4 SP - Article 348, 1 EP - 14 AN - OPUS4-39575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kasperovich, G. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - X-ray refraction distinguishes unprocessed powder from empty pores in selective laser melting Ti-6Al-4V N2 - For the first time, X-ray refraction techniques are proven for the identification of void formation in Ti-6Al-4V parts produced by selective laser melting. The topology and volume fraction of pores are measured in samples produced with different laser energy density. Unique X-ray refraction methods identify different kinds of defects, characteristic to the regions below and above the Optimum laser energy density, namely unprocessed powder (unmolten powder particles, balling effect, and Fusion defects) from empty keyhole pores. Furthermore, it is possible to detect small inhomogeneities (voids or cracks) with sizes below the spatial resolution of optical microscopy and X-ray computed tomography. KW - Additive manufacturing KW - X-ray refraction KW - Microscopy KW - X-ray computed tomography KW - Porosity PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434041 DO - https://doi.org/10.1080/21663831.2017.1409288 SN - 2166-3831 VL - 6 IS - 2 SP - 130 EP - 135 PB - Taylor & Francis Group CY - London, UK AN - OPUS4-43404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Artzt, K. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Exploring the correlation between subsurface residual stresses and manufacturing parameters in laser powder bed fused Ti-6Al-4V N2 - Subsurface residual stresses (RS) were investigated in Ti-6Al-4V cuboid samples by means of X-ray synchrotron diffraction. The samples were manufactured by laser powder bed fusion (LPBF) applying different processing parameters, not commonly considered in open literature, in order to assess their influence on RS state. While investigating the effect of process parameters used for the calculation of volumetric energy density (such as laser velocity, laser power and hatch distance), we observed that an increase of energy density led to a decrease of RS, although not to the same extent for every parameter variation. Additionally, the effect of support structure, sample roughness and LPBF machine effects potentially coming from Ar flow were studied. We observed no influence of support structure on subsurface RS while the orientation with respect to Ar flow showed to have an impact on RS.We conclude recommending monitoring such parameters to improve part reliability and reproducibility. KW - Additive manufacturing KW - Synchrotron X-ray diffraction KW - Residual stress KW - Ti-6Al-4V PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474281 DO - https://doi.org/10.3390/met9020261 SN - 2075-4701 VL - 9 IS - 2 SP - 261, 1 EP - 13 PB - MDPI AN - OPUS4-47428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiede, Tobias A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Serrano-Munoz, Itziar A1 - Gollwitzer, Christian A1 - Bruno, Giovanni T1 - 3D shape analysis of powder for laser beam melting by synchrotron X-ray CT N2 - The quality of components made by laser beam melting (LBM) additive manufacturing is naturally influenced by the quality of the powder bed. A packing density <1 and porosity inside the powder particles lead to intrinsic voids in the powder bed. Since the packing density is determined by the particle size and shape distribution, the determination of these properties is of significant interest to assess the printing process. In this work, the size and shape distribution, the amount of the particle’s intrinsic porosity, as well as the packing density of micrometric powder used for LBM, have been investigated by means of synchrotron X-ray computed tomography (CT). Two different powder batches were investigated: Ti–6Al–4V produced by plasma atomization and stainless steel 316L produced by gas atomization. Plasma atomization particles were observed to be more spherical in terms of the mean anisotropy compared to particles produced by gas atomization. The two kinds of particles were comparable in size according to the equivalent diameter. The packing density was lower (i.e., the powder bed contained more voids in between particles) for the Ti–6Al–4V particles. The comparison of the tomographic results with laser diffraction, as another particle size measurement technique, proved to be in agreement. KW - Additive manufacturing KW - Laser beam melting KW - Synchrotron computed tomography KW - Powder analysis KW - Imaging PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474070 DO - https://doi.org/10.3390/qubs3010003 SN - 2412-382X VL - 3 IS - 1 SP - 3, 1 EP - 12 PB - MDPI AN - OPUS4-47407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Surmeneva, M. A1 - Koptioug, A. A1 - Evsevleev, Sergei A1 - Léonard, Fabien A1 - Bruno, Giovanni A1 - Surmenev, R. T1 - X-ray computed tomography of multiple-layered scaffolds with controlled gradient cell lattice structures fabricated via additive manufacturing N2 - In this paper we report on the characterization by X-ray computed tomography of calcium phosphate (CaP) and polycaprolactone (PCL) coatings on Ti-6Al-4V alloy scaffolds used as a material for medical implants. The cylindrical scaffold has greater porosity of the inner part than the external part, thus, mimicking trabecular and cortical bone, respectively. The prismatic scaffolds have uniform porosity. Surface of the scaffolds was modified with calcium phosphate (CaP) and polycaprolactone (PCL) by dip-coating to improve biocompatibility and mechanical properties. Computed tomography performed with X-ray and synchrotron radiation revealed the defects of structure and morphology of CaP and PCL coatings showing small platelet-like and spider-web-like structures, respectively. KW - Additive manufacturing KW - Lattice structure KW - Multiple-layered scaffold KW - Coating KW - Medical implants KW - Computed tomography KW - Polycaprolactone KW - Calcium phosphate PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471931 UR - http://stacks.iop.org/1742-6596/1145/i=1/a=012044 DO - https://doi.org/10.1088/1742-6596/1145/1/012044 SN - 1742-6596 VL - 1145 SP - 012044, 1 EP - 7 PB - IOP AN - OPUS4-47193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -