TY - JOUR A1 - Van Tran, K. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography JF - Materials & Design N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561649 DO - https://doi.org/10.1016/j.matdes.2022.111037 SN - 0264-1275 VL - 222 SP - 111037 PB - Elsevier Ltd. AN - OPUS4-56164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Pfretzschner, B. A1 - Taparli, Ugur Alp A1 - Kardjilov, N. T1 - Time-Resolved Neutron Bragg-Edge Imaging: A Case Study by Observing Martensitic Phase Formation in Low Temperature Transformation (LTT) Steel during GTAW JF - Applied Sciences N2 - Polychromatic and wavelength-selective neutron transmission radiography were applied during bead-on-plate welding on 5 mm thick sheets on the face side of martensitic low transformation temperature (LTT) steel plates using gas tungsten arc welding (GTAW). The in situ visualization of austenitization upon welding and subsequent α’-martensite formation during cooling could be achieved with a temporal resolution of 2 s for monochromatic imaging using a single neutron wavelength and of 0.5 s for polychromatic imaging using the full spectrum of the beam (white beam). The spatial resolution achieved in the experiments was approximately 200 µm. The transmitted monochromatic neutron beam intensity at a wavelength of λ = 0.395 nm was significantly reduced during cooling below the martensitic start temperature Ms since the emerging martensitic phase has a ~10% higher attenuation coefficient than the austenitic phase. Neutron imaging was significantly influenced by coherent neutron scattering caused by the thermal motion of the crystal lattice (Debye–Waller factor), resulting in a reduction in the neutron transmission by approx. 15% for monochromatic and by approx. 4% for polychromatic imaging. KW - Austenite-to-martensite transformation KW - Neutron radiography KW - Bragg-edge imaging KW - Gas tungsten arc welding (GTAW) KW - Debye–Waller factor KW - Low transformation temperature (LTT) steel PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538016 DO - https://doi.org/10.3390/app112210886 VL - 11 IS - 22 SP - 10886 PB - MDPI CY - Basel AN - OPUS4-53801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peruzzi, N. A1 - Galli, S. A1 - Helmholz, H. A1 - Kardjilov, N. A1 - Krüger, D. A1 - Markötter, Henning A1 - Moosmann, J. A1 - Orlov, D. A1 - Prgomet, Z. A1 - Willumeit-Römer, R. A1 - Wennerberg, A. A1 - Bech, M. T1 - Multimodal ex vivo methods reveal that Gd-rich corrosion byproducts remain at the implant site of biodegradable Mg-Gd screws JF - Acta Biomaterialia N2 - Extensive research is being conducted on magnesium (Mg) alloys for bone implant manufacturing, due to their biocompatibility, biodegradability and mechanical properties. Gadolinium (Gd) is among the most promising alloying elements for property control in Mg alloy implants; however, its toxicity is contro- versial. Investigating Gd behavior during implant corrosion is thus of utmost importance. In this study, we analyzed the degradation byproducts at the implant site of biodegradable Mg-5Gd and Mg-10Gd implants after 12 weeks healing time, using a combination of different imaging techniques: histology, energy-dispersive x-ray spectroscopy (EDX), x-ray microcomputed tomography (μCT) and neutron μCT. The main finding has been that, at the healing time in exam, the corrosion appears to have involved only the Mg component, which has been substituted by calcium and phosphorus, while the Gd remains localized at the implant site. This was observed in 2D by means of EDX maps and extended to 3D with a novel application of neutron tomography. X-ray fluorescence analysis of the main excretory organs also did not reveal any measurable accumulation of Gd, further reinforcing the conclusion that very limited or no removal at all of Gd-alloy happened during degradation. KW - Magnesium-gadolinium alloy KW - Biodegradable implant KW - Multimodal analysis KW - Energy-dispersive x-ray spectroscopy KW - Micro-computed tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535910 DO - https://doi.org/10.1016/j.actbio.2021.09.047 SN - 1742-7061 SP - 1 EP - 10 PB - Elsevier Ltd. AN - OPUS4-53591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Pfretzschner, Beate A1 - Taparli, Ugur Alp A1 - Kardjilov, N. T1 - Time-Resolved Neutron Bragg-Edge Imaging: A Case Study by Observing Martensitic Phase Formation in Low Temperature Transformation (LTT) Steel during GTAW JF - Novel Approaches for Nondestructive Testing and Evaluation N2 - Polychromatic and wavelength-selective neutron transmission radiography were applied during bead-on-plate welding on 5 mm thick sheets on the face side of martensitic low transformation temperature (LTT) steel plates using gas tungsten arc welding (GTAW). The in situ visualization of austenitization upon welding and subsequent α’-martensite formation during cooling could be achieved with a temporal resolution of 2 s for monochromatic imaging using a single neutron wavelength and of 0.5 s for polychromatic imaging using the full spectrum of the beam (white beam). The spatial resolution achieved in the experiments was approximately 200 µm. The transmitted monochromatic neutron beam intensity at a wavelength of λ = 0.395 nm was significantly reduced during cooling below the martensitic start temperature M s since the emerging martensitic phase has a ~10% higher attenuation coefficient than the austenitic phase. Neutron imaging was significantly influenced by coherent neutron scattering caused by the thermal motion of the crystal lattice (Debye–Waller factor), resulting in a reduction in the neutron transmission by approx. 15% for monochromatic and by approx. 4% for polychromatic imaging. KW - Neutron radiography KW - Debye–Waller factor KW - Austenite-to-martensite transformation KW - Low transformation temperature (LTT) steel KW - Bragg-edge imaging KW - Gas tungsten arc welding (GTAW) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559077 DO - https://doi.org/10.3390/app112210886 VL - 11 IS - 22 PB - MDPI AN - OPUS4-55907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pacheco, V. A1 - Marattukalam, J. J. A1 - Karlsson, D. A1 - Dessieux, L. A1 - Tran, K. V. A1 - Beran, P. A1 - Manke, I. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Sahlberg, M. A1 - Woracek, R. T1 - On the relationship between laser scan strategy, texture variations and hidden nucleation sites for failure in laser powder-bed fusion JF - Materialia N2 - While laser powder-bed fusion has overcome some of the design constraints of conventional manufacturing methods, it requires careful selection of process parameters and scan strategies to obtain favorable properties. Here we show that even simple scan strategies, complex ones being inevitable when printing intricate designs, can inadvertently produce local alterations of the microstructure and preferential grain orientation over small areas – which easily remain unnoticed across the macroscale. We describe how a combined usage of neutron imaging and electron backscatter diffraction can reveal these localized variations and explain their origin within cm-sized parts. We explain the observed contrast variations by linking the neutron images to simulated data, pole figures and EBSD, providing an invaluable reference for future studies and showing that presumably minor changes of the scan strategy can have detrimental effects on the mechanical properties. In-situ tensile tests reveal that fracture occurs in a region that was re-melted during the building process. KW - Laser powder-bed fusion KW - Texture KW - Preferential orientation KW - Diffraction contrast neutron imaging KW - Bragg-edge PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568054 DO - https://doi.org/10.1016/j.mtla.2022.101614 VL - 26 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-56805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kardjilov, N. A1 - Hilger, A. A1 - Manke, I. A1 - Banhart, J. A1 - Griesche, Axel T1 - Imaging with Cold Neutrons at the CONRAD-2 Facility T2 - Physics Procedia N2 - CONRAD-2 is an imaging instrument using low-energy (cold) neutrons. The instrument is installed at the end of a curved neutron guide which avoids the direct line of sight towards the reactor core. This ensures a very low background of high-energy neutrons and. photons at the sample position. The cold neutron beam provides a wavelength range which is suitable for phase-and diffraction-contrast imaging such as grating interferometry and Bragg edge mapping. The instrument is well suited for high resolution imaging due to the high efficiency of the very thin scintillators that can be used for the detection of cold neutrons. An instrument upgrade was performed recently as a part of an upgrade program for the cold neutron instrumentation at HZB. The parameters of the instrument as well as some research highlights will be presented. T2 - 10th World Conference on Neutron Radiography (WCNR) CY - Grindelwald, SWITZERLAND DA - 05.10.2014 KW - iron embrittlement KW - neutron imaging KW - neutron instrumentation KW - cold neutrons PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-373239 DO - https://doi.org/10.1016/j.phpro.2015.07.008 SN - 1875-3892 VL - 69 SP - 60 EP - 66 PB - Elsevier B.V. CY - Amsterdam, NL AN - OPUS4-37323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dabah, Eitan A1 - Pfretzschner, Beate A1 - Schaupp, Thomas A1 - Kardjilov, N. A1 - Manke, I. A1 - Boin, M. A1 - Woracek, R. A1 - Griesche, Axel T1 - Time-resolved Bragg-edge neutron radiography for observing martensitic phase transformation from austenitized super martensitic steel JF - Journal of Materials Science N2 - Neutron Bragg-edge imaging was applied for the visualization of a γ-Austenite to α'-martensite phase transformation. In the present study, a super martensitic stainless steel sample was heated until complete austenitization and was subsequently cooled down to room temperature. The martensitic phase Transformation started at Ms = 190 °C. Using a monochromatic neutron beam with λ = 0.390 nm, the transmitted intensity was significantly reduced during cooling below Ms, since the emerging martensitic phase has a higher attenuation coefficient than the austenitic phase at this wavelength. The phase Transformation process was visualized by filming the transmission images from a scintillator screen with a CCD camera with a temporal resolution of 30 s and a spatial resolution of 100 µm. KW - Neutron imaging KW - Bragg-edge imaging KW - Phase transformation PY - 2017 DO - https://doi.org/10.1007/s10853-016-0642-9 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 6 SP - 3490 EP - 3496 AN - OPUS4-38574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel A1 - Pfretzschner, Beate A1 - Schaupp, Thomas A1 - Schulz, M. A1 - Kardjilov, N. ED - Duprez, Lode T1 - Hydrogen in steel visualized by neutron imaging T2 - Proceedings of the Third International Conference on Metals & Hydrogen N2 - Neutron cameras allow visualizing hydrogen distributions with radiographic or tomographic imaging methods in iron and steel. The necessary contrast between hydrogen and iron stems from the high difference in the total neutron cross section of both elements. This allows e.g. the in situ measurement of hydrogen mass flow inside cm thick steel samples with a temporal resolution of 20 s using neutron radiography as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples with neutron tomography. We could detect directly gaseous hydrogen in the crack cavities and we measured the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of hydrogen-induced damage mechanisms. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 µm. In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography methods in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed at the research reactor BER II of the HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in Garching. T2 - Third International Conference on Metals & Hydrogen CY - Ghent, Belgium DA - 29.05.2018 KW - Hydrogen KW - Steel KW - Neutron imaging PY - 2018 SN - 978-9-08179-422-0 SP - J01 AN - OPUS4-45359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tran, K. V. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Hilger, A. A1 - Kockelmann, W. A1 - Kelleher, J. A1 - Puplampu, S. B. A1 - Penumadu, D. A1 - Tremsin, A. S. A1 - Banhart, J. A1 - Manke, I. T1 - Spectral neutron tomography JF - Materials Today Advances N2 - Combined three-dimensional (3D) mapping of (micro-)structures with elemental and crystalline phase variations is of significant importance for the characterization of materials. Neutron wavelength selective imaging is a spectral imaging technique that exploits unique contrast differences e.g. for mapping dissimilar elemental, isotope, or phase compositions, and has the particular advantage of being applicable to sample volumes on the meso- and macroscale. While being mostly applied as radiography (2D) so far, we herein report that the extension to tomography allows for the display of the full spectral information for every voxel and in 3D. The development is supported by example data from a continuous as well as a pulsed neutron source. As a practical example, we collected 4D data sets (3D + spectral) of plastically deformed metastable stainless steel and herein demonstrate an improved quantification strategy for crystalline phase fractions. These exemplary results illustrate that localized phase transformations can be quantified even in complex geometries within centimeter-sized samples, and we will discuss the limits and future prospects of the technique that is not limited to crystalline materials. KW - 4D tomographic data KW - Multi-energy CT KW - Spectral CT KW - Phase distribution KW - Full-field phase tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521668 DO - https://doi.org/10.1016/j.mtadv.2021.100132 VL - 9 SP - 132 PB - Elsevier Ltd. AN - OPUS4-52166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel A1 - Pfretzschner, Beate A1 - Schaupp, Thomas A1 - Kannengießer, Thomas A1 - Kardjilov, N. ED - Somerday, B. P. ED - Sofronis, P. T1 - Measurement of hydrogen distributions in metals by neutron radiography and tomography T2 - Material Perfomance in Hydrogen Environments - Proceedings of the 2016 International Hydrogen Conference N2 - Neutron imaging has become a valuable tool for measuring hydrogen distributions qualitatively and quantitatively in metals. Hydrogen mass flow can be measured inside cm thick Steel samples with 10 s temporal resolution. Hydrogen accumulations around craclcs in embrittled iron samples can be visualized three-dimensionally. The gas pressure of hydrogen in crack cavities has been measured to be in the ränge of 5 MPa to 15 MPa. This quality of information allows new insights for the analysis of damage mechanisms on a micrometer scale, e.g., of hydrogen blistering. Further, this method is nondestructive and provides local information in situ and in three dimensions with a spatial resolution of 20 µm - 30 µm. T2 - International Hydrogen Conference 2016 CY - Jackson Lake Lodge, Wyoming, USA DA - 11.09.2017 KW - Hydrogen KW - Neutron imaging KW - Neutron radiography KW - Neutron tomography PY - 2017 SN - 978-0-7918-6138-7 DO - https://doi.org/10.1115/1.861387_ch46 SP - 416 EP - 422 AN - OPUS4-42505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano Munoz, Itziar A1 - Pfretzschner, Beate A1 - Kromm, Arne A1 - Nadammal, Naresh A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Neuwirth, T. A1 - Schulz, M. A1 - Griesche, Axel T1 - High-resolution Bragg-edge neutron radiography detects grain morphology in PBF-LB/M IN718 JF - Materialia N2 - One of the main advantages of metal additive manufacturing (MAM) techniques is their ability to produce components with site-specific microstructural features. Nevertheless, microstructural defects and lack of repeatability are still major concerns in MAM. In this study, a laser powder bed fusion (PBF-LB/M) IN718 material, produced using two different scan length vectors, is investigated using Bragg-edge neutron 2D imaging (BENI) combined with electron backscatter diffraction (EBSD) analysis. BENI is able to detect, on a macroscopic scale, process-induced changes in texture in a large field of view covering the entire sample (20×80 mm2). In addition, high-resolution BENI (HR-BENI), with a pixel size of 12.8 µm, provides a micro-scale examination of the local variations of texture and grain morphology, otherwise undistinguishable using the standard resolution. As such, HR-BENI offers a straightforward and detailed way of screening the integrity of MAM parts at cm-length scales. KW - Bragg-edge neutron 2D imaging (BENI) KW - Metal additive manufacturing (MAM) KW - IN718 PBF-LB/M KW - Crystallographic texture control KW - Electron backscatter diffraction (EBSD) PY - 2023 DO - https://doi.org/10.1016/j.mtla.2023.101827 SN - 2589-1529 VL - 30 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-57819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tran, K. V. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography JF - Materials & Design N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569101 DO - https://doi.org/10.1016/j.matdes.2022.111037 VL - 222 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jamro, R. A1 - Mente, Tobias A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Al-Falahat, Ala'A. M. A1 - Woracek, R. A1 - Manke, I. A1 - Griesche, Axel T1 - Temperature distribution during welding measured by neutron imaging JF - Journal of Physics: Conference Series N2 - This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data. KW - Neutron imaging KW - Debye-Waller-Faktor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586268 DO - https://doi.org/10.1088/1742-6596/2605/1/012026 VL - 2605 SP - 1 EP - 10 PB - IOP Publishing Ltd. AN - OPUS4-58626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel A1 - Mente, Tobias A1 - Markötter, Henning A1 - Al-Falahat, M. A1 - Kardjilov, N. T1 - Neutron Bragg edge imaging for in situ mapping of crystallographic phase-transformations and of temperature distributions during GTAW of supermartensitic stainless steel N2 - In Neutron-Bragg-Edge Imaging (NBEI) experiments, we studied the phase transition during butt-welding of supermartensitic steel plates. Gas tungsten arc welding (GTAW) was used with a motorized torch allowing for automated weldments. The austenitization in the heat affected zone (HAZ) underneath the welding head could be clearly visualized at λ = 0.39 nm, a wavelength smaller than the Bragg edge wavelengths of both austenite and martensite. Also, the re-transformation into the martensitic phase upon cooling was detected. However, we observed an unexpected additional change in transmission at λ = 0.44 nm that is a wavelength larger than the wavelength of the Bragg edges of both the martensitic and austenitic phases. We attribute this change to the Deybe-Waller-Factor that describes the temperature dependence of coherent scattering at a crystal lattice. The observed two-dimensional attenuation map corresponds well with a temperature distribution modelling by software macros in ANSYS. Here, the absolute temperature values could be achieved by calibrating the modelled attenuation with help of a thermocouple placed at the steel plate. This allows in return for a direct two-dimensional temperature reading based on the Debye-Waller-relation between neutron attenuation and sample temperature. T2 - ITMNR-9 CY - Buenos Aires, Argentina DA - 12.10.2022 KW - Debye-Waller-Faktor PY - 2023 AN - OPUS4-58627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -