Microstructural effects of tungsten deposition on 415 steel during PBF-LB/M additive manufacturing of plasma facing components Natan Garrivier, Steven Van Petegem, Markus Strobl, Manuel Pouchon, Sergio Soria, Florencia Malamud, Enrico Tosoratti, Adam Cretton, Eliot Jermann, Ken Vidar Falch, Malgorzata Grazyna Makowska Materials and Design, 2026 Microstructure and mechanical properties of tungsten/415 stainless steel samples manufactured by Laser Powder Bed Fusion (PBF-LB/M) were investigated. The influence of the parameters used to process tungsten was investigated, focusing on the resulting microstructure at the steel-tungsten interface and its vicinity. Chemical imaging techniques were employed, in particular scanning micro X-ray diffraction (μXRD) and micro X-Ray Fluorescence (μXRF) imaging. The microstructure at the interface between W and steel was analyzed using Electron Backscatter Diffraction and XRD, and the formation of crystalline phases in the area of the interface was also analyzed by operando XRD measurements. μXRD-imaging showed the formation of retained austenite within the lower interface region, reaching up to 1 wt% locally and 0.4 wt% on average. Fe<sub>7</sub>W<sub>6</sub> was identified as the major intermetallic phase at the interface. Its formation could be mitigated using a layer-wise energy grading strategy. The presence of tungsten within the steel lattice just below the intermetallic region was found to favor the formation of large martensitic grains by suppressing the formation of austenite during cooling. Neutron Bragg-Edge Imaging revealed the formation of a residual strain gradient in the steel domain, strongly depending on the energy density, heat input and energy gradient employed.
Neutron Bragg edge imaging for strain and texture characterization of steel-copper multi-material obtained by laser powder-bed fusion Sergio R. Soria, Florencia Malamud, Efthymios Polatidis, Matteo Busi, Jan Capek, Léa Deillon, Markus Bambach, Adrian Losko, Markus Strobl Materials and Design, 2026 • Neutron Bragg edge imaging was applied to study 316 L/CuCrZr multimaterials specimens. • Texture depends on the orientation between the interfaces and the building direction. • 316 L had a texture along the (200) orientation, CuCrZr layer had a random texture. • Compressive strain was observed in the CuCrZr layer and tensile strain in 316 L layer. Bragg edge imaging has been applied to multi-material laser powder-bed fusion (M2LPBF) samples of 316 L stainless steel and CuCrZr. A multilayer sample with interfaces perpendicular to the building direction and a bilayer sample with parallel interfaces to the building direction were studied. The results demonstrate that this non-destructive approach does not only succeed in characterizing the different interdiffusion zones, but also strain and texture variations across the multiple material regions. In both samples the 316 L layers are found to display a strong (200) texture, while the CuCrZr layers exhibited either a random or weak (110) texture. In the multilayer samples, the difference in thermal expansion between CuCrZr and 316 L led to tensile residual strain in the steel layers and compressive residual strain in CuCrZr. The multilayer sample showed narrower intermixing zones at its horizontal interfaces, especially where CuCrZr was printed onto 316 L steel which is attributed to adjustments in the printing parameters that increase local heating in the formed layers. These results agree with conventional destructive characterizations used in this work. The non-destructive nature of the analyses can enable corresponding observations on the same sample before and after post treatments and/or mechanical testing, implying significant potential for future studies.
Residual strain and strain evolution of dissimilar aluminium-steel friction stir lap welding during lap shear tests Sergio R. Soria, Florencia Malamud, Markus Strobl, Leonardo N. Tufaro, Hernán G. Svoboda Journal of Advanced Joining Processes, 2025 • Welds of carbon steel and dual-phase steel with 5000-series aluminium were studied. • In all cases, residual tensile strains along the welding direction were measured. • Maximum strains of approximately 3000 µε were observed. • Formation of steel inclusions were detected using AISI 1010 carbon steel. • In lap shear tests, lateral contraction reduces the effective strain in the steel. Friction Stir Lap Welding (FSLW) is a technique used to join dissimilar materials, such as aluminium alloys and steel sheets, applied in the automotive industry. The residual strain distribution generated during the process, strongly affects the mechanical performance and long-term durability of the welded components. In this study, the residual strains generated during FSLW of aluminium alloy and steel sheets were investigated using Bragg edge neutron imaging (BEI). Different combinations of thin aluminium alloy and steel sheets with thicknesses between 0.8 mm and 2 mm were analysed. 5052 and 5182 alloys, in combination with AISI 1010 carbon steel and dual phase (DP) 1000 steel were employed. Additionally, the evolution of the actual strain under lap shear tests was monitored. The presence of the steel inclusions was detected by neutron transmission imaging. The BEI results showed tensile residual strain along the longitudinal direction in the steel sheets after the welding process, in all cases displaying a M-shaped strain field. During the lap shear tests, a reduction of the actual tensile strains was observed due to the lateral contraction produced in the mechanical testing.
Large scale stabilization of the BCC phase in copper-steel laser powder bed fusion enabling statistical microstructural analysis and mechanical testing A.M. Jamili, J. Jhabvala, C. Cayron, F. Malamud, V. Pejchal, A. Nicholas Grundy, B. Rouxel, M. Van der Meer, S. Soria, Roland E. Logé Materials and Design, 2025 • 15 wt% 316L significantly affects optical and thermophysical properties of CuCrZr. • Fe-rich BCC phase formation refines the microstructure and weaken texture. • BCC phase and solid solution strengthening improve mechanical properties. • High-temp BCC nucleation alters solidification behavior during LPBF. It has been shown that a Body-Centered Cubic (BCC) phase appears in the L-PBF additively manufactured Copper/Steel bimetallic system, at the interface between the two materials. This study aimed to stabilize the BCC phase on a larger scale to enable statistical analysis of its effects on solidification and microstructure, as well as mechanical performance. Thermodynamic CALPHAD calculations identified a mixture of 85 % CuCrZr and 15 % 316L as optimal for BCC stabilization. Compared with pure CuCrZr processed under identical conditions, the 15 % 316L addition increased laser absorptivity, reduced thermal conductivity, refined the microstructure, weakened texture, and promoted significant BCC phase formation. The BCC phase altered solidification by inducing heterogeneous nucleation, producing a bimodal microstructure. These microstructural changes markedly enhanced mechanical performance, with room-temperature compression yield strength rising from 250 MPa (CuCrZr) to 535 MPa. Finite element simulations, coupled with CALPHAD modelling, were used to investigate the influence of 316L on CuCrZr’s thermophysical properties and its role in the observed improvements. The findings of this study suggest that the presence of the BCC phase can enhance the mechanical properties of the interfacial region, and potentially influence the resistance to interfacial cracking—a common issue in multi-material printing.
Phase formation and texture evolution in 316L-CuCrZr multi-material structures fabricated by laser powder bed fusion Antonios Baganis, Florencia Malamud, Jan Čapek, Fedor F. Klimashin, Efthymios Polatidis, Matteo Busi, Miroslav Šmíd, Michal Jambor, Johann Michler, Markus Strobl, Christian Leinenbach Materials and Design, 2025 Steel-copper multi-material structures produced via Additive Manufacturing pose challenges in laser co-processing and microstructural control. This work employs neutron imaging, Electron Backscatter Diffraction (EBSD), and Energy Dispersive Spectroscopy (EDS) mapping to characterize 316L-CuCrZr Functionally Graded Structures (FGS) fabricated via Laser Powder Bed Fusion. Polarization Contrast Neutron Imaging (PNI) tracks ferrite formation in 316L-CuCrZr premixtures, while Neutron Bragg Edge Imaging (BEI) examines the texture evolution of the 316L-CuCrZr mixtures. PNI and EBSD phase mapping confirm ferrite formation in mixtures exceeding 50 wt% CuCrZr, appearing as spherical particles that locally increase hardness, as shown by nano-indentation mapping. The ferrite fraction peaks between 70–80 wt% CuCrZr. Simultaneously, BEI and EBSD Inverse Pole Figures (IPF) mapping reveal a crystallographic texture transition and grain refinement for mixtures containing more than 50 wt% CuCrZr. Microstructure analysis shows cracks in 10–40 wt% CuCrZr mixtures, while compositions with more than 50 wt% CuCrZr result in crack-free structures. EDS mapping and thermodynamic modeling suggest ferrite formation mechanisms in both liquid and solid states. This study highlights how FGS engineering enables precise control over crack formation, microstructure, and crystallographic texture in steel-copper multi-material structures.
Texture analysis implementation at the neutron strain diffractometer POLDI Florencia Malamud, Steve Gaudez, Jan Capek, Ezequiel Oscar Fogliatto, Markus Strobl Materials Characterization, 2025 Neutron strain scanners have been proven to be a key tool to non-destructively determine the crystallographic texture at selected locations within a macroscopic object. In particular, time-of-flight neutron strain scanners present the advantage that several crystalline reflections can be measured simultaneously for a given specimen direction, allowing the determination of several (incomplete) pole figures from a single experimental arrangement. Here we will present the implementation of a novel data analysis methodology to perform spatially resolved texture analyses in bulk specimens at POLDI, the Pulse Frame Overlap diffractometer at Paul Scherrer Institute. The method is based on the determination of several incomplete pole figures after splitting POLDI's diffraction detector, with an angular range of 30°, into several units of smaller angular coverage. This is done by time-focusing the neutrons arriving at all the detection elements of the new ‘virtual detector’ into a single diffractogram, performing a 2D-least squares fitting of the diffraction data and creating experimental pole figures from the Euler angles of the explored sample orientations and the refined peak areas corrected by the flight path of the neutrons inside the sample. From the incomplete experimental pole figures, the determination of the orientation distribution function of crystallites is accomplished using the MTEX toolbox. We will present demonstration experiments on a stainless steel additive manufacturing specimen and a hot-rolled and annealed Zircaloy-4 plate. • Non-destructive spatially resolved crystallographic texture methodology at POLDI. • POLTex: a crystallographic texture analysis toolbox for POLDI. • Texture characterization of engineering specimens.
Concurrent Operando Neutron Imaging and Diffraction Analysis Revealing Spatial Lithiation Phase Evolution in an Ultra-Thick Graphite Electrode Markus Strobl, Monica E. Baur, Stavros Samothrakitis, Florencia Malamud, Xiaolong Zhang, Patrick K.M. Tung, Søren Schmidt, Robin Woracek, Jongmin Lee, Ryoji Kiyanagi, Luise Theil Kuhn, Inbal Gavish Segev, Yair Ein‐Eli Advanced Energy Materials, 2025 Energy‐efficient, safe, and reliable Li‐ion batteries (LIBs) are required for a wide range of applications. The introduction of ultra‐thick graphite anodes, desired for high energy densities, meets limitations in internal electrode transport properties, leading to detrimental consequences. Yet, there is a lack of experimental tools capable of providing a complete view of local processes. Here, a multi‐modal operando measurement approach is introduced, enabling quantitative spatio‐temporal observations of Li concentrations and intercalation phases in ultra‐thick graphite electrodes. Neutron imaging and diffraction concurrently provide correlated multiscale information from the scale of the cell down to the crystallographic scale. In particular, the evolving formation of the solid electrolyte interphase (SEI), observation of gradients in total lithium content, as well as in the formation of ordered LixC6 phases and trapped lithium are mapped throughout the first charge–discharge cycle of the cell. Different lithiation stages co‐exist during charging and discharging; delayed lithiation and delithiation processes are observed in central regions of the electrode, while the SEI formation, potential plating, and dead lithium are predominantly found closer to the interface with the separator. The study emphasizes the potential to investigate Li‐ion diffusion and the kinetics of lithiation phase formation in thick electrodes.
Wavelength-resolved neutron transmission analyses of textured materials F. Malamud, M.A. Vicente Alvarez, J.R. Santisteban, M. Strobl Materials Characterization, 2025 Wavelength-resolved neutron imaging for diffraction contrast often referred to as Bragg edge imaging is a neutron-based technique that has gained attention in recent years due to its promising ability to characterize the microstructure of polycrystalline materials with spatial resolution. This method relies on spatially resolved analyses of diffraction induced features in transmission spectra within the thermal neutron range. Assessable characteristics are e.g. phase fractions, lattice strains, and crystallographic texture. For the latter forward modelling of transmission spectra from known orientation distribution functions (ODFs) has been demonstrated for various materials. However, solving the inverse problem—retrieving crystallographic texture from transmission spectra—presents a more complex challenge. In recent years, the authors have developed two theoretical approaches to model the relationship between transmission spectra and texture, either by decomposing the ODF into individual orientation fractions or by expanding it into a Fourier series. Both approaches have shown excellent predictive capability for materials with different crystal symmetries, including hexagonal, FCC, and BCC structures. Here we present the comparison between the proposed models, highlighting the advantages and disadvantages of the direct method based on different approaches for the analysis of wavelength-resolved neutron transmission experiments of textured materials. Finally, we present the future trends in the inversion method, i.e., the estimation of the ODFs from transmission spectra in tomography experiments. • Wavelength-resolved neutron imaging models for textured specimens. • Neutron transmission simulation of textured materials from known ODFs and comparison with experimental data. • Discussion of ODFs estimation from transmission spectra in tomography experiments.
Texture tomography with high angular resolution utilizing sparsity Mads Carlsen, Florencia Malamud, Peter Modregger, Anna Wildeis, Markus Hartmann, Robert Brandt, Andreas Menzel, Marianne Liebi Journal of Applied Crystallography, 2025 We demonstrate an approach to the reconstruction of scanning probe X-ray diffraction tomography data with anisotropic polycrystalline samples. The method involves reconstructing a voxel map containing an orientation distribution function in each voxel of a bulk 3D sample. By choosing a particular kind of basis functions, we can effectively utilize non-negativity in orientation space for samples with sparse texture. This enables us to achieve stable solutions at high angular resolutions where the problem would otherwise be underdetermined. This method differs from established approaches by not relying on a peak-finding step. It is therefore applicable to sample systems consisting of small and highly mosaic crystalline domains that are not handled well by these methods. We demonstrate the new approach using data from a shot-peened martensite sample where we are able to map the twinning microstructure in the interior of a bulk sample without resolving the individual lattice domains. We also demonstrate the approach on a piece of gastropod shell with a mosaic microstructure. The results suggest that, by utilizing the sparsity of the texture, the experiment can be carried out using only a single rotation axis, unlike previous demonstrations of texture and tensor tomography.
Evolution of texture and residual stresses in 2205 duplex stainless steel during laser powder bed fusion Steve Gaudez, Florencia Malamud, William Hearn, Shieren Sumarli, Markus Strobl, Steven Van Petegem Materials and Design, 2025 This study investigates the development of residual stresses in textured 2205 duplex stainless steel during laser powder bed fusion additive manufacturing (LPBF AM). In situ and operando neutron diffraction experiments were conducted to study the transient and real-time evolution of stresses and strains during processing, using an AM machine designed for neutron studies. Additionally, Bragg-edge imaging was employed to investigate the crystallographic texture. The results showed that residual stress redistribution primarily occurs in the first set of added layers when further layers are added on top. The cube texture observed in the sample significantly affects residual stress determination, leading to inaccuracies up to 96 MPa if not accounted for. This highlights the need for orientation-dependent diffraction elastic constants in residual stress calculations. Furthermore, variations in texture intensity across the sample dimensions were found to be driven by changes in the local temperature history, which were deciphered from real-time strain measurements. Finally, this study demonstrates the potential of combining LPBF with neutron diffraction to investigate the underlying mechanisms of AM in the bulk of the sample. • Utilize neutron diffraction to track transient and operando changes during LPBF. • Cube texture intensity varies across sample due to local thermal history. • Principal strain direction aligns with sample diagonal when using 90° rotation. • Residual stress redistribution primarily occurs during first set of added layers. • Outline potential of the novel n-SLM for analysing LPBF with neutron methods.
Image processing and software Anders Kaestner, Matteo Busi, Florencia Malamud Neutron Imaging from Applied Materials Science to Industry, 2024
Engineering Efthymios Polatidis, Florencia Malamud, Markus Strobl Neutron Imaging from Applied Materials Science to Industry, 2024
Manufacturing Efthymios Polatidis, Florencia Malamud, Pavel Trtik Neutron Imaging from Applied Materials Science to Industry, 2024
Natural heritage Eberhard Lehmann, David Mannes, Florencia Malamud Neutron Imaging from Applied Materials Science to Industry, 2024
Nuclear materials Pavel Trtik, Robert Zboray, Liliana I Duarte, Okan Yetik, Florencia Malamud Neutron Imaging from Applied Materials Science to Industry, 2024
Operando phase mapping in multi-material laser powder bed fusion Shieren Sumarli, Florencia Malamud, Steven Van Petegem, Steve Gaudez, Antonios Baganis, Matteo Busi, Efthymios Polatidis, Christian Leinenbach, Roland E. Logé, Markus Strobl Virtual and Physical Prototyping, 2024
Bragg edge tomography characterization of additively manufactured 316L steel Matteo Busi, Efthymios Polatidis, Florencia Malamud, Winfried Kockelmann, Manuel Morgano, Anders Kaestner, Anton Tremsin, Nikola Kalentics, Roland Logé, Christian Leinenbach, Takenao Shinohara, Markus Strobl Physical Review Materials, 2022