TY - JOUR A1 - Artzt, K. A1 - Mishurova, Tatiana A1 - Bauer, P.-P. A1 - Gussone, J. A1 - Barriobero-Vila, P. A1 - Evsevleev, Sergei A1 - Bruno, Giovanni A1 - Requena, G. A1 - Haubrich, J. T1 - Pandora’s Box–Influence of Contour Parameters on Roughness and Subsurface Residual Stresses in Laser Powder Bed Fusion of Ti-6Al-4V JF - Materials N2 - The contour scan strategies in laser powder bed fusion (LPBF) of Ti-6Al-4V were studied at the coupon level. These scan strategies determined the surface qualities and subsurface residual stresses. The correlations to these properties were identified for an optimization of the LPBF processing. The surface roughness and the residual stresses in build direction were linked: combining high laser power and high scan velocities with at least two contour lines substantially reduced the surface roughness, expressed by the arithmetic mean height, from values as high as 30 μm to 13 μm, while the residual stresses rose from ~340 to about 800 MPa. At this stress level, manufactured rocket fuel injector components evidenced macroscopic cracking. A scan strategy completing the contour region at 100 W and 1050 mm/s is recommended as a compromise between residual stresses (625 MPa) and surface quality (14.2 μm). The LPBF builds were monitored with an in-line twin-photodiode-based melt pool monitoring (MPM) system, which revealed a correlation between the intensity quotient I2/I1, the surface roughness, and the residual stresses. Thus, this MPM system can provide a predictive estimate of the surface quality of the samples and resulting residual stresses in the material generated during LPBF. KW - Additive manufacturing KW - Ti-6Al-4V KW - Contour scan strategy KW - Surface roughness KW - Melt pool monitoring KW - Residual stress KW - Synchrotron X-ray diffraction PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510585 DO - https://doi.org/10.3390/ma13153348 VL - 13 IS - 15 SP - 3348 AN - OPUS4-51058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Cabeza, S. A1 - Mishurova, Tatiana A1 - Garcés, G. A1 - Sevostianov, I. A1 - Requena, G. A1 - Boin, M. A1 - Hofmann, M. A1 - Bruno, Giovanni T1 - Stress-induced damage evolution in cast AlSi12CuMgNi alloy with one and two ceramic reinforcements. Part II: Effect of reinforcement orientation JF - Journal of Materials Science N2 - While there is a large body of literature on the micro-mechanical behavior of metal matrix composites (MMCs) under uniaxial applied stress, very little is available on multi-phase MMCs. In order to cast light on the reinforcement mechanisms and damage processes in such multi-phase composites, materials made by an Al-based piston alloy and containing one and two ceramic reinforcements (planar-random oriented alumina fibers and SiC particles) were studied. In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while X-ray computed tomography on pre-strained samples was used to monitor and quantify damage. We found that damage progresses differently in composites with different orientations of the fiber mat. Because of the presence of intermetallic network, it was observed that the second ceramic reinforcement changed the load transfer scenario only at very high applied load, when also intermetallic particles break. We rationalized the present results combining them with previous investigations and using a micromechanical model. KW - Multi-phase KW - Metal matrix composites KW - Intermetallics KW - Computed tomography KW - In-situ neutron diffraction KW - Piston alloy KW - Load transfer PY - 2020 DO - https://doi.org/10.1007/s10853-019-04069-4 SN - 1573-4803 VL - 55 IS - 3 SP - 1049 EP - 1068 PB - Springer AN - OPUS4-49460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Cabeza, Sandra A1 - Koos, R. A1 - Sevostianov, I. A1 - Garces, G. A1 - Requena, G. A1 - Fernández, R. A1 - Bruno, Giovanni T1 - The role of intermetallics in stress partitioning and damage evolution of AlSi12CuMgNi alloy JF - Materials Science & Engineering A N2 - Load partitioning between phases in a cast AlSi12CuMgNi alloy was investigated by in-situ compression test during neutron diffraction experiments. Computed tomography (CT) was used to determine volume fractions of eutectic Si and intermetallic (IM) phases, and to assess internal damage after ex-situ compression tests. The CT reconstructed volumes showed the interconnectivity of IM phases, which build a 3D network together with eutectic Si. Large stresses were found in IMs, revealing their significant role as a reinforcement for the alloy. An existing micromechanical model based on Maxwell scheme was extended to the present case, assuming the alloy as a three-phase composite (Al matrix, eutectic Si, IM phases). The model agrees well with the experimental data. Moreover, it allows predicting the principal stresses in each phase, while experiments can only determine stress differences between the axial and radial sample directions. Finally, we showed that the addition of alloying elements not only allowed developing a 3D interconnected network, but also improved the strength of the Al matrix, and the ability of the alloy constituents to bear mechanical load. KW - Aluminum alloys KW - Neutron diffraction KW - Micromechanical modeling KW - Internal stress KW - Computed tomography PY - 2018 DO - https://doi.org/10.1016/j.msea.2018.08.070 VL - 736 SP - 453 EP - 464 PB - Elsevier B.V. AN - OPUS4-45927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Khrapov, D. A1 - Paveleva, A. A1 - Meinel, Dietmar A1 - Surmenev, R. A1 - Surmeneva, M. A1 - Koptyug, A. A1 - Bruno, Giovanni T1 - X-ray Computed Tomography Procedures to Quantitatively Characterize the Morphological Features of Triply Periodic Minimal Surface Structures JF - Materials N2 - Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control, which can prevent their successful application. In fact, the optimization of the AM process is impossible without considering structural characteristics as manufacturing accuracy, internal defects, as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of X-ray computed tomography (XCT). Several advanced image analysis workflows are presented to evaluate the effect of build orientation on wall thicknesses distribution, wall degradation, and surface roughness reduction due to the chemical etching of TPMSS. It is shown that the manufacturing accuracy differs for the structural elements printed parallel and orthogonal to the manufactured layers. Different strategies for chemical etching show different powder removal capabilities and both lead to the loss of material and hence the gradient of the wall thickness. This affects the mechanical performance under compression by reduction of the yield stress. The positive effect of the chemical etching is the reduction of the surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of retained powder with the pore size of the functionally graded TPMSS, which can further improve the manufacturing process. KW - Metamaterials KW - Functionally graded porous structure KW - Triply periodic minimal surface structures KW - Roughness analysis KW - Powder removal KW - Deep learning segmentation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528142 DO - https://doi.org/10.3390/ma14113002 VL - 14 IS - 11 SP - 3002 PB - MDPI AN - OPUS4-52814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Paciornik, S. A1 - Bruno, Giovanni T1 - Advanced Deep Learning-Based 3D Microstructural Characterization of Multiphase Metal Matrix Composites JF - Advanced Engineering Materials N2 - The quantitative analysis of microstructural features is a key to understanding the micromechanical behavior of metal matrix composites (MMCs), which is a premise for their use in practice. Herein, a 3D microstructural characterization of a five-phase MMC is performed by synchrotron X-ray computed tomography (SXCT). A workflow for advanced deep learning-based segmentation of all individual phases in SXCT data is shown using a fully convolutional neural network with U-net architecture. High segmentation accuracy is achieved with a small amount of training data. This enables extracting unprecedently precise microstructural parameters (e.g., volume fractions and particle shapes) to be input, e.g., in micromechanical models. KW - Computed tomography KW - Convolutional neural networks KW - Deep learning KW - Metal matrix composites KW - Segmentations PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504261 DO - https://doi.org/10.1002/adem.201901197 SN - 1438-1656 VL - 22 IS - 4 SP - 1901197 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Sevostianov, I. A1 - Mishurova, Tatiana A1 - Hofmann, M. A1 - Garcés, G. A1 - Bruno, Giovanni T1 - Explaining Deviatoric Residual Stresses in Aluminum Matrix Composites with Complex Microstructure JF - Metallurgical and Materials Transactions A N2 - The residual stresses in multiphase metal Matrix composites with both random planar-oriented short fibers and particles were studied by neutron diffraction and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observed that randomly oriented phases possess non-hydrostatic residual stress. The recently developed modeling Approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses Accounting for the interaction of random oriented phases with fibers having preferential orientation. KW - Metal matrix composite KW - Residual stress KW - Deviatoric KW - Micromechanics PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506472 DO - https://doi.org/10.1007/s11661-020-05697-1 VL - 51 IS - 6 SP - 3104 EP - 3113 PB - Springer AN - OPUS4-50647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khimich, M. A. A1 - Prosolov, K. A. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Monforte, X. A1 - Teuschl, A. H. A1 - Slezak, P. A1 - Ibragimov, E. A. A1 - Saprykin, A. A. A1 - Kovalevskaya, Z. G. A1 - Dmitriev, A. I. A1 - Bruno, Giovanni A1 - Sharkeev, Y. P. T1 - Advances in Laser Additive Manufacturing of Ti-Nb Alloys: From Nanostructured Powders to Bulk Objects JF - Nanomaterials N2 - The additive manufacturing of low elastic modulus alloys that have a certain level of porosity for biomedical needs is a growing area of research. Here, we show the results of manufacturing of porous and dense samples by a laser powder bed fusion (LPBF) of Ti-Nb alloy, using two distinctive fusion strategies. The nanostructured Ti-Nb alloy powders were produced by mechanical alloying and have a nanostructured state with nanosized grains up to 90 nm. The manufactured porous samples have pronounced open porosity and advanced roughness, contrary to dense samples with a relatively smooth surface profile. The structure of both types of samples after LPBF is formed by uniaxial grains having micro- and nanosized features. The inner structure of the porous samples is comprised of an open interconnected system of pores. The volume fraction of isolated porosity is 2 vol. % and the total porosity is 20 vol. %. Cell viability was assessed in vitro for 3 and 7 days using the MG63 cell line. With longer culture periods, cells showed an increased cell density over the entire surface of a porous Ti-Nb sample. Both types of samples are not cytotoxic and could be used for further in vivo studies. KW - Additive manufacturing KW - Biomaterials KW - Ti-Nb alloy KW - Nanostructured powder KW - Laser methods KW - Powder methods KW - Laser powder bed fusion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525344 DO - https://doi.org/10.3390/nano11051159 VL - 11 IS - 5 SP - 1159 PB - MDPI AN - OPUS4-52534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Kozadayeva, M. A1 - Manabaev, K. A1 - Panin, A. A1 - Sjöström, W. A1 - Koptyug, A. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Meinel, Dietmar A1 - Bruno, Giovanni A1 - Cheneler, D. A1 - Surmenev, R. A1 - Surmeneva, M. T1 - Different approaches for manufacturing Ti-6Al-4V alloy with triply periodic minimal surface sheet-based structures by electron beam melting JF - Materials N2 - Targeting biomedical applications, Triply Periodic Minimal Surface (TPMS) gyroid sheet-based structures were successfully manufactured for the first time by Electron Beam Melting in two different production Themes, i.e., inputting a zero (Wafer Theme) and a 200 µm (Melt Theme) wall thickness. Initial assumption was that in both cases, EBM manufacturing should yield the structures with similar mechanical properties as in a Wafer-mode, as wall thickness is determined by the minimal beam spot size of ca 200 µm. Their surface morphology, geometry, and mechanical properties were investigated by means of electron microscopy (SEM), X-ray Computed Tomography (XCT), and uniaxial tests (both compression and tension). Application of different manufacturing Themes resulted in specimens with different wall thicknesses while quasi-elastic gradients for different Themes was found to be of 1.5 GPa, similar to the elastic modulus of human cortical bone tissue. The specific energy absorption at 50% strain was also similar for the two types of structures. Finite element simulations were also conducted to qualitatively analyze the deformation process and the stress distribution under mechanical load. Simulations demonstrated that in the elastic regime wall, regions oriented parallel to the load are primarily affected by deformation. We could conclude that gyroids manufactured in Wafer and Melt Themes are equally effective in mimicking mechanical properties of the bones. KW - Electron beam melting KW - Scaffold KW - Lightweight structures KW - Computed tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531595 DO - https://doi.org/10.3390/ma14174912 SN - 1996-1944 VL - 14 IS - 17 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-53159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Paveleva, A. A1 - Kozadayeva, M. A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Bruno, Giovanni A1 - Surmenev, R. A1 - Koptyug, A. A1 - Surmeneva, M. T1 - Trapped powder removal from sheet-based porous structures based on triply periodic minimal surfaces fabricated by electron beam powder bed fusion JF - Materials Science & Engineering A N2 - 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. KW - Additive manufacturing KW - Residual powder removal KW - Ti6Al4V alloy KW - Electron beam powder bed fusion KW - TPMS structures PY - 2023 DO - https://doi.org/10.1016/j.msea.2022.144479 VL - 862 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-56564 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 JF - IOP Conf. Series: Journal of Physics 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 - Mechanical Engineering KW - Maskinteknik PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510763 DO - https://doi.org/10.1088/1742-6596/1145/1/012044 SN - 17426588 VL - 1145 SP - 012044 PB - IOP AN - OPUS4-51076 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 JF - Journal of Physics Conference Series 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 - TY - JOUR A1 - Markötter, Henning A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Evsevleev, Sergei A1 - Arlt, T. A1 - Ulbricht, Alexander A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - A Review of X-Ray Imaging at the BAMline (BESSY II) JF - Advanced Engineering Materials N2 - 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. KW - Material science KW - Radiography KW - Refraction KW - Tomography KW - X-ray imaging PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572417 DO - https://doi.org/10.1002/adem.202201034 SN - 1438-1656 SP - 1 EP - 22 PB - Wiley VHC-Verlag AN - OPUS4-57241 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 JF - Materials and Design 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 - Mishurova, Tatiana A1 - Artzt, K. A1 - Haubrich, J. A1 - Evsevleev, Sergei A1 - Evans, Alexander A1 - Meixner, M. A1 - Serrano Munoz, Itziar A1 - Sevostianov, I. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Connecting Diffraction-Based Strain with Macroscopic Stresses in Laser Powder Bed Fused Ti-6Al-4V JF - Metallurgical and Materials Transactions A N2 - The laser powder bed fusion (LPBF) production process often results in large residual stress (RS) in the parts. Nondestructive techniques to determine RS are badly needed. However, a reliable quantification of macro-RS (i.e., stress at the component level) by means of diffraction-based techniques is still a great challenge, because the link between diffraction-based strain and macro-RS is not trivial. In this study, we experimentally determine (by means of in-situ synchrotron radiation diffraction) this link for LPBF Ti-6Al-4V. We compare our results with commonly used models to determine the so-called diffraction elastic constants (DECs). We show that LPBF materials possess different DECs than wrought alloys, simply because their microstructural and mechanical properties are different. We also show that the existing models can be used to calculate DECs only if high accuracy of the RS values is not required. If the peculiarities of the microstructure have to be taken into account (as is the case of additively manufactured materials), a radically new approach is desirable. KW - Tiatanium KW - Synchrotron X-ray diffraction KW - Macroscopic stress KW - Laser powder bed fusion KW - Texture KW - Diffraction elastic constants PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506483 DO - https://doi.org/10.1007/s11661-020-05711-6 VL - 51 IS - 6 SP - 3194 EP - 3204 PB - Springer AN - OPUS4-50648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Bruno, Giovanni A1 - Evsevleev, Sergei A1 - Sevostianov, I. T1 - Determination of macroscopic stress from diffraction experiments: A critical discussion JF - Journal of Applied Physics N2 - The paper is motivated by some inconsistencies and contradictions present in the literature on the calculation of the so-called diffraction elastic constants. In an attempt at unifying the views that the two communities of Materials Science and Mechanics of Materials have on the subject, we revisit and define the terminology used in the field. We also clarify the limitations of the commonly used approaches and Show that a unified methodology is also applicable to textured materials with a nearly arbitrary grain shape. We finally compare the predictions based on this methodology with experimental data obtained by in situ synchrotron radiation diffraction on additively manufactured Ti-6Al4V alloy. We show that (a) the transverse isotropy of the material yields good agreement between the best-fit isotropy approximation (equivalent to the classic Kröner’s model) and the experimental data and (b) the use of a general framework allows the calculation of all components of the tensor of diffraction elastic constants, which are not easily measurable by diffraction methods. This allows us to extend the current state-of-the-art with a predictive tool. KW - Additive manufacturing KW - X-ray diffraction KW - Elastic constants KW - Stress concentration tensor PY - 2020 DO - https://doi.org/10.1063/5.0009101 VL - 128 IS - 2 SP - 025103 PB - AIP Publishing AN - OPUS4-50993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Artzt, K. A1 - Haubrich, J. A1 - Sevostianov, I. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Micromechanical behavior of annealed Ti-6Al-4V produced by Laser Powder Bed Fusion JF - European Journal of Materials N2 - The micromechanical behavior of an annealed Ti-6Al-4V material produced by Laser Powder Bed Fusion was characterized by means of in-situ synchrotron X-ray diffraction during a tensile test. The lattice strain evolution was obtained parallel and transversal to the loading direction. The elastic constants were determined and compared with the conventionally manufactured alloy. In the plastic regime, a lower plastic anisotropy exhibited by the lattice planes was observed along the load axis (parallel to the building direction) than in the transverse direction. Also, the load transfer from α to β phase was observed, increasing global ductility of the material. The material seems to accumulate a significant amount of intergranular strain in the transverse direction. KW - Additive manufacturing KW - Ti-6Al-4V KW - Anisotropy KW - Intergranular strain KW - Synchrotron X-ray diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547406 DO - https://doi.org/10.1080/26889277.2022.2063763 VL - 2 IS - 1 SP - 186 EP - 201 PB - Taylor & Francis AN - OPUS4-54740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Piault, Pierre A1 - King, Andrew A1 - Henry, Laura A1 - Bruno, Giovanni T1 - Understanding the hot isostatic pressing efectiveness of laser powder bed fusion Ti‑6Al‑4V by in‑situ X‑ray imaging and difraction experiments JF - Scientific reports N2 - 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. KW - Additive manufacturing KW - Laser powder bed fusion KW - X-ray computed tomography KW - Hot isostatic pressing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587702 DO - https://doi.org/10.1038/s41598-023-45258-1 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 11 AN - OPUS4-58770 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauzon, C. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Dubiez-Le Goff, S. A1 - Murugesan, S. A1 - Bruno, Giovanni A1 - Hryha, E. T1 - Residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion as a function of process atmosphere and component design JF - Additive Manufacturing N2 - The influence of the process gas, laser scan speed, and sample thickness on the build-up of residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion was studied. Pure argon and helium, as well as a mixture of those (30% helium), were employed to establish process atmospheres with a low residual Oxygen content of 100 ppm O2. The results highlight that the subsurface residual stresses measured by X-ray diffraction were significantly lower in the thin samples (220 MPa) than in the cuboid samples (645 MPa). This difference was attributed to the shorter laser vector length, resulting in heat accumulation and thus in-situ stress relief. The addition of helium to the process gas did not introduce additional subsurface residual stresses in the simple geometries, even for the increased scanning speed. Finally, larger deflection was found in the cantilever built under helium (after removal from the baseplate), than in those produced under argon and an argon-helium mixture. This result demonstrates that complex designs involving large scanned areas could be subjected to higher residual stress when manufactured under helium due to the gas’s high thermal conductivity, heat capacity, and thermal diffusivity. KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Process atmosphere KW - Helium PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534209 DO - https://doi.org/10.1016/j.addma.2021.102340 VL - 47 SP - 2340 PB - Elsevier B.V. AN - OPUS4-53420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shashev, Yury A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Osenberg, Markus A1 - Manke, Ingo A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni T1 - Optimizing the visibility of X-ray phase grating interferometry JF - Materials Testing N2 - The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup. KW - Synchrotron, BAMline KW - Talbot-Lau interferometer KW - X-ray imaging KW - X-ray refraction KW - Grating interferometry KW - X-ray phase contrast PY - 2017 DO - https://doi.org/10.3139/120.111097 SN - 0025-5300 VL - 59 IS - 11-12 SP - 974 EP - 980 PB - Hanser Verlag AN - OPUS4-42955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Surmeneva, M. A1 - Koptyug, A. A1 - Khrapov, D. A1 - Ivanov, Yuriy A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Prymak, O. A1 - Loza, K. A1 - Epple, M. A1 - Bruno, Giovanni A1 - Surmenev, R. T1 - In situ synthesis of a binary Ti–10at% Nb alloy by electron beam melting using a mixture of elemental niobium and titanium powders JF - Journal of Materials Processing Technology N2 - This study reports the results of the preliminary assessment to fabricate Ti-10at% Nb alloy by electron beam melting (EBM®) from a blend of elemental Nb and Ti powders. The microstructure of the EBM-manufactured Ti-10at% Nb alloys is sensitive to the following factors: different sintering properties of Nb and Ti powders, powder particle properties, material viscosities at varying melt pool temperatures, β-stabilizer element content and the EBM® process parameters. Three phases were observed in as-manufactured Ti-10at% Nb alloy: μm-size Nb phase, a Nb-rich β-solid solution surrounding Nb phase, lamellar structured α-phase and β-solid solution with different distribution and volume fraction. Thus, the combination of powder particle characteristics, very short time material spends in molten condition and sluggish kinetics of mixing and diffusional process in Ti-Nb alloy results in heterogeneous microstructures depending on the local Nb content in the powder blend and the EBM® process conditions. KW - Additive manufacturing KW - Electron beam melting KW - Ti-Nb alloy KW - In situ alloying PY - 2020 DO - https://doi.org/10.1016/j.jmatprotec.2020.116646 VL - 282 SP - 116646 PB - Elsevier B.V. AN - OPUS4-50457 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 JF - Quantum Beam Science 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 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Bruno, Giovanni T1 - Noise and blur removal from corrupted X-ray computed tomography scans: A multilevel and multiscale deep convolutional framework approach with synthetic training data (BAM SynthCOND) JF - Tomography of Materials and Structures N2 - Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc. KW - XCT Data Conditioning KW - Denoising Deblurring Sharpening KW - Deep Convolutional Neural Network (DCNN) KW - Synthetic Training Data KW - ACEnet KW - Metal Matrix Composite (MMC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579129 DO - https://doi.org/10.1016/j.tmater.2023.100011 VL - 2 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-57912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - Synthetic Data Generation for Automatic Segmentation of X-ray Computed Tomography Reconstructions of Complex Microstructures JF - Journal of Imaging N2 - The greatest challenge when using deep convolutional neural networks (DCNNs) for automatic segmentation of microstructural X-ray computed tomography (XCT) data is the acquisition of sufficient and relevant data to train the working network. Traditionally, these have been attained by manually annotating a few slices for 2D DCNNs. However, complex multiphase microstructures would presumably be better segmented with 3D networks. However, manual segmentation labeling for 3D problems is prohibitive. In this work, we introduce a method for generating synthetic XCT data for a challenging six-phase Al–Si alloy composite reinforced with ceramic fibers and particles. Moreover, we propose certain data augmentations (brightness, contrast, noise, and blur), a special in-house designed deep convolutional neural network (Triple UNet), and a multi-view forwarding strategy to promote generalized learning from synthetic data and therefore achieve successful segmentations. We obtain an overall Dice score of 0.77. Lastly, we prove the detrimental effects of artifacts in the XCT data on achieving accurate segmentations when synthetic data are employed for training the DCNNs. The methods presented in this work are applicable to other materials and imaging techniques as well. Successful segmentation coupled with neural networks trained with synthetic data will accelerate scientific output. KW - Automatic segmentation KW - 3D deep convolutional neural network (3D DCNN) KW - Dice score KW - Metal matrix composite (MMC) KW - Modified U-Net architectures KW - Multi-phase materials PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571243 DO - https://doi.org/10.3390/jimaging9020022 VL - 9 IS - 2 SP - 1 EP - 23 PB - MDPI AN - OPUS4-57124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - A novel iterative algorithm to improve segmentations with deep convolutional neural networks trained with synthetic X-ray computed tomography data (i.S.Sy.Da.T.A) JF - Computational Materials Science N2 - We propose a novel iterative segmentation algorithm (i.S.Sy.Da.T.A: Iterative Segmentation Synthetic Data Training Algorithm) employing Deep Convolutional Neural Networks and synthetic training data for X-ray tomographic reconstructions of complex microstructures. In our method, we reinforce the synthetic training data with experimental XCT datasets that were automatically segmented in the previous iteration. This strategy produces better segmentations in successive iterations. We test our algorithm with experimental XCT re constructions of a 6-phase Al-Si Matrix Composite reinforced with ceramic fibers and particles. We perform the analysis in 3D with a special network architecture that demonstrates good generalization with synthetic training data. We show that our iterative algorithm returns better segmentations compared to the standard single training approach. More specifically, phases possessing similar attenuation coefficients can be better segmented: for Al2O3 fibers, SiC particles, and Intermetallics, we see an increase of the Dice score with respect to the classic approach: from 0.49 to 0.54, from 0.66 to 0.72, and from 0.55 to 0.66 respectively. Furthermore, the overall Dice score increases from 0.77 to 0.79. The methods presented in this work are also applicable to other materials and imaging techniques. KW - Metal matrix composites (MMC) KW - Multi-phase materials KW - 3D imaging KW - Dice score KW - Automatic segmentation KW - Deep convolutional neural network (DCNN) KW - Modified U-net architectures PY - 2023 DO - https://doi.org/10.1016/j.commatsci.2023.112112 SN - 0927-0256 VL - 223 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-57482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, Rita A1 - Faglioni, Francesco A1 - Bruno, Giovanni T1 - A Complete Strategy to Achieve High Precision Automatic Segmentation of Challenging Experimental X‐Ray Computed Tomography Data Using Low‐Resemblance Synthetic Training Data JF - Advanced Engineering Materials N2 - It is shown that preconditioning of experimental X‐ray computed tomography (XCT) data is critical to achieve high‐precision segmentation scores. The challenging experimental XCT datasets and deep convolutional neural networks (DCNNs) are used that are trained with low‐resemblance synthetic XCT data. The material used is a 6‐phase Al–Si metal matrix composite‐reinforced with ceramic fibers and particles. To achieve generalization, in our past studies, specific data augmentation techniques were proposed for the synthetic XCT training data. In addition, two toolsets are devised: (1) special 3D DCNN architecture (3D Triple_UNet), slicing the experimental XCT data from multiple views (MultiView Forwarding), the i.S.Sy.Da.T.A. iterative segmentation algorithm, and (2) nonlocal means (NLM) conditioning (filtering) for the experimental XCT data. This results in good segmentation Dice scores across all phases compared to more standard approaches (i.e., standard UNet architecture, single view slicing, standard single training, and NLM conditioning). Herein, the NLM filter is replaced with the deep conditioning framework BAM SynthCOND introduced in a previous publication, which can be trained with synthetic XCT data. This leads to a significant segmentation precision increase for all phases. The proposed methods are potentially applicable to other materials and imaging techniques. KW - Automatic Segmentation KW - XCT KW - Artificial Intelligence KW - Synthetic Training Data KW - i.S.Sy.Da.T.A. KW - BAM SynthMAT KW - BAM SynthCOND KW - Triple UNet KW - Convolutional Neural Network (DCNN) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590912 DO - https://doi.org/10.1002/adem.202301030 SN - 1438-1656 VL - 26 IS - 2 SP - 1 EP - 9 PB - Wiley online library AN - OPUS4-59091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -