TY - CONF A1 - Bruno, Giovanni T1 - Redefining residual stress analysis to tackle the challenges posed by additively manufactured materials and structures N2 - Additively manufactured (and in particular laser powder bed fused) materials represent a manyfold challenge for the materials scientist and engineer because of their distinctive microstructure. If laser powder bed fusion is used to produce components, the complexity level increases because meso-structures (e.g., overhanging features, surface and internal defects) gain importance. Furthermore, if the main advantage of additive manufacturing, i.e., the freedom of design, is to be fully exploited, and geometrically complex structures, such as lattices, are manufactured, then such structures become meta-materials. This means that the geometry and the materials properties become equally important. This matryoshka-like (more literary than the dry “multi-scale”) complexity makes the characterization of the residual stress fields by means of diffraction methods so difficult with the current means, that new paradigms are necessary to tackle the challenge. Indeed, classic open problems acquire an extra layer of difficulty, such that new solutions need to be found and the sometimes-dormant debate needs to be re-opened. Examples include the determination of: a- the unstrained reference: this reference can become location-dependent and needs to be carefully determined; b- the so-called diffraction elastic constants, which becomes immensely challenging since even the single-crystal elastic constants are not known for additively manufactured materials. On top of this, other problems arise. The determination of the principal axes of stress becomes non-trivial because the hatching strategy sometimes dominates over the sample geometry. Even further, in complex structures, such as lattices, the textbook statement that the strain measurement in six independent directions uniquely identifies the strain tensor becomes simply invalid. The peculiar surface features of additively manufactured materials transform trivial tasks into formidable challenges: the precise alignment of a specimen in a beam or the determination of surface stresses with laboratory X-rays need to be thoroughly re-discussed and lay far from being routine tasks. In this paper, we will show a few examples of the cases mentioned above. We will demonstrate that sometimes the classic approach works very well, but other times surprising conclusions can be drawn from in-depth studies of the residual stress in additively manufactured materials. In short, we predicate that classic methods cannot be used on additively manufactured materials and structures without a critical evaluation of their validity and application range. T2 - ICRS11 CY - Nancy, France DA - 28.03.2022 KW - Neutron diffraction KW - Laser powder bed fusion KW - Diffraction elastic constants KW - Unstrained reference KW - Surface roughness KW - Porosity PY - 2022 AN - OPUS4-54642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Damage and stress evolution in multi-phase metal matrix composites N2 - While there is a extensive 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 and damage processes in such multi-phase composites, an Al alloy with 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 was used to investigate pre-strained samples, in order 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 the intermetallic network, it was observed that the second ceramic reinforcement changes the load transfer scenario only at very high applied load, when also intermetallic particles break. We rationalized the experimental results by means of a micromechanical model based on Maxwell’s homogenization scheme, and we could explain why no damage is observed in the ductile matrix under compression: the matrix finds itself in hydrostatic compression, and the Poisson’s tensile strain is totally carried by the reinforcement phases T2 - CIMTEC CY - Perugia, Italy DA - 20.06.2022 KW - Load transfer KW - Neutron Diffraction KW - Michromechanical modeling KW - Computed Tomography KW - Machine Learning PY - 2022 AN - OPUS4-55404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Schaupp, Thomas A1 - Griesche, Axel A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Hannemann, Andreas A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - Quantitative analysis of hydrogen-assisted microcracking in duplex stainless steel through X-ray refraction 3D imaging N2 - While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture. KW - 2101 duplex stainless steel KW - Hydrogen embrittlement KW - Synchrotron radiation KW - X-ray refraction KW - Computed tomography KW - Microcracking PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542811 DO - https://doi.org/10.1002/adem.202101287 SN - 1438-1656 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silveira, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Longo, E. A1 - Greving, I. A1 - Lasch, P. A1 - Shahar, R A1 - Zaslansky, P. T1 - Water flow through bone: Neutron tomography reveals differences in water permeability between osteocytic and anosteocytic bone material N2 - Vertebrate bones are made of a nanocomposite consisting of water, mineral and organics. Water helps bone material withstand mechanical stress and participates in sensation of external loads. Water diffusion across vertebrae of medaka (bone material lacking osteocytes) and zebrafish (bone material containing osteocytes) was compared using neutron tomography. Samples were measured both wet and following immersion in deuterated-water (D2O). By quantifying H+ exchange and mutual alignment with X-ray lCT scans, the amount of water expelled from complete vertebra was determined. The findings revealed that anosteocytic bone material is almost twice as amenable to D2O diffusion and H2O exchange, and that unexpectedly, far more water is retained in osteocytic zebrafish bone. Diffusion in osteocytic bones (only 33 % – 39 % water expelled) is therefore restricted as compared to anosteocytic bone (~ 60 % of water expelled), presumably because water flow is confined to the lacunar-canalicular network (LCN) open-pore system. Histology and Raman spectroscopy showed that anosteocytic bone contains less proteoglycans than osteocytic bone. These findings identify a previously unknown functional difference between the two bone materials. Therefore, this study proposes that osteocytic bone retains water, aided by non-collagenous proteins, which contribute to its poroelastic mechano-transduction of water flow confined inside the LCN porosity. KW - Bone porosity KW - Anosteocytic bone KW - Water permeability KW - Neutron tomography KW - Proteoglycans PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564563 DO - https://doi.org/10.1016/j.matdes.2022.111275 VL - 224 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Synchrotron X-Ray Refraction during in-situ heat treatments N2 - In this work, synchrotron X-ray refraction radiography (SXRR) was combined with in-situ heat treatment to monitor microstructure and porosity evolution as a function of temperature. The investigated material was a laser powder bed fusion (LPBF) manufactured AlSi10Mg, where the initial eutectic Si network is known to break down into larger particles with increasing temperature. Such alloy is also prone to thermally induced porosity (TIP). We show that SXRR allows detecting the changes in the Si-phase morphology upon heating, while this is currently possible only using scanning electron microscopy. SXRR also allows observing the growth of pores, usually studied via X-ray computed tomography, but on much smaller fields-of-view. Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes. T2 - MSE 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - Si network KW - Al alloys KW - PBF-LB KW - X-ray refraction radiography KW - Pore nucleation PY - 2022 AN - OPUS4-56161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Laquai, René A1 - Wieder, Frank A1 - Kupsch, Andreas A1 - Müller, Bernd R. T1 - The combined use of X-ray refraction and transmission radiography and computed tomography N2 - Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements. T2 - 11th Conference on Industrial Computed Tomography CY - Online meeting DA - 08.02.2022 KW - X-ray refraction radiography KW - Computed Tomography KW - Synchrotron radiation KW - Additive manufacturing KW - Damage evolution PY - 2022 UR - https://www.ndt.net/article/ctc2022/papers/ICT2022_paper_id268.pdf SP - 1 EP - 7 AN - OPUS4-54324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Bruno, Giovanni T1 - Micro Non-Destructive Testing and Evaluation N2 - What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue. At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation. In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration. Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress. The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity. Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation. The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E. KW - Neutron Diffraction KW - Ultrasound KW - Eddy Currents KW - X-ray Computed Tomography KW - Mechanical Properties KW - Residual Stress KW - Defects PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570321 SN - 978-3-0365-6180-6 DO - https://doi.org/10.3390/books978-3-0365-6180-6 SN - 1996-1944 SP - 1 EP - 304 PB - MDPI CY - Basel AN - OPUS4-57032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Climent Terol, Estela A1 - Gojani, Ardian A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Generalized Analysis Approach of the Profile Roughness by Electron Microscopy with the Example of Hierarchically Grown Polystyrene–Iron Oxide–Silica Core–Shell–Shell Particles N2 - The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained. KW - Core–shell particles KW - Image analysis KW - Nanoparticles KW - Roughness KW - SEM KW - transmission mode PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542576 DO - https://doi.org/10.1002/adem.202101344 SP - 1 EP - 9 PB - Wiley-VCH AN - OPUS4-54257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Gojani, Ardian B. A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - From 2D and Single Particle to 3D and Batch Analysis as a Routine Quality Check Procedure for the Morphological Characterization of Core-Shell Microparticles N2 - CS particles show unique properties by merging individual characteristics of the core and the shell materials. An alteration particularly in their surface roughness affects the final performance of the particles in the targeted application. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task employing microscopic techniques being scarce and showing large differences in terms of methodology and results. In our previous work, we have reported a systematic study with a reliable analysis tool, which evaluates profile roughness quantitatively, for individual core-shell microparticles using electron microscopy (EM) images of both types, Scanning Electron Microscopy (SEM) and transmission mode SEM (or TSEM). The SEM images contain two-dimensional (2D) information, therefore, provide profile roughness data only from the projection in the horizontal plane (in other words, from the “belly”) of a spherical particle. The present study offers a practical procedure to give access to more information by tilting the sample holder and hence allowing images of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, extended information on surface roughness of the particle can be extracted. Thus, instead of obtaining 2D information from a single SEM image, three-dimensional (3D) information is obtained from 2D projections recorded at different particle orientations. T2 - Microscopy and Microanalysis 2022 CY - Oregon, Portland, USA DA - 31.07.2022 KW - Core-shell particles KW - Image processing KW - Roughness KW - Scanning electron microscopy KW - Tilting PY - 2022 DO - https://doi.org/10.1017/S1431927622002094 SN - 1431-9276 VL - 28 IS - S1 SP - 332 EP - 334 PB - Cambridge University Press AN - OPUS4-55373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Jungnickel, H. A1 - Tentschert, J. A1 - Luch, A. A1 - Sogne, V. A1 - Maier, F. A1 - Burr, L. A1 - Schmid, D. A1 - Yoon, T.-H. A1 - Petters, R. A1 - Briffa, S.M. A1 - Valsami-Jones, E. T1 - Automation and Standardization—A Coupled Approach Towards Reproducible Sample Preparation Protocols for Nanomaterial Analysis N2 - Whereas the characterization of nanomaterials using different analytical techniques is often highly automated and standardized, the sample preparation that precedes it causes a bottleneck in nanomaterial analysis as it is performed manually. Usually, this pretreatment depends on the skills and experience of the analysts. Furthermore, adequate reporting of the sample preparation is often missing. In this overview, some solutions for techniques widely used in nano-analytics to overcome this problem are discussed. Two examples of sample preparation optimization by au-tomation are presented, which demonstrate that this approach is leading to increased analytical confidence. Our first example is motivated by the need to exclude human bias and focuses on the development of automation in sample introduction. To this end, a robotic system has been de-veloped, which can prepare stable and homogeneous nanomaterial suspensions amenable to a variety of well-established analytical methods, such as dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), field-flow fractionation (FFF) or single-particle inductively coupled mass spectrometry (sp-ICP-MS). Our second example addresses biological samples, such as cells exposed to nanomaterials, which are still challenging for reliable analysis. An air–liquid interface has been developed for the exposure of biological samples to nanomaterial-containing aerosols. The system exposes transmission electron microscopy (TEM) grids under reproducible conditions, whilst also allowing characterization of aerosol composition with mass spectrometry. Such an approach enables correlative measurements combining biological with physicochemical analysis. These case studies demonstrate that standardization and automation of sample preparation setups, combined with appropriate measurement processes and data reduction are crucial steps towards more reliable and reproducible data. KW - Sample preparation KW - Automation KW - Nanomaterial analysis KW - Standardization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543988 DO - https://doi.org/10.3390/molecules27030985 VL - 27 IS - 3 SP - 1 EP - 22 PB - MDPI AN - OPUS4-54398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine (TMB) in Amperometric Assays N2 - Electrochemical methods make great promise to meet the demand for user-friendly on-site devices for monitoring important parameters. Food industry often runs own lab procedures, e.g. for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with miniaturized technologies. Enzyme-linked immunosorbent assays, with photometric detection of the horseradish peroxidase (HRP) substrate, 3,3’,5,5’-tetramethylbenzidine (TMB), form a good basis for sensitive detection. To provide a straight-forward approach for the miniaturization of the detection step, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry it was found that the TMB electrochemistry is strongly dependent on the pH and the electrode material. It was found that screen-printed gold electrodes and a highly acidic pH value (pH 1) are well-suited to perform the electrochemical detection of TMB, due to the reversible character of the redox reaction under these conditions. This set-up provides a good signal stability over several measuring cycles, providing the basis for analysing multiple samples. In contrast to this, for carbon screen-printed electrodes, it was found that the signal response has changed after the electrochemical reaction with TMB at pH 1. At a weakly acidic pH value (pH 4), neither with carbon nor with gold electrodes a reproducible electrochemical detection of TMB could be achieved [1]. Based on these findings we created a smartphone-based, electrochemical, immunomagnetic assay for the detection of ochratoxin A and ergometrine in real samples. Therefore, a competitive assay was performed on magnetic beads using HRP and TMB/H2O2 to generate the signal. Enzymatically oxidized TMB was quantified after addition of H2SO4 by amperometry with screen-printed gold electrodes in a custom-made wall-jet flow cell. The results are in good correlation with the established photometric detection method, providing a solid basis for sensing of further analytes in HRP-based assays using the newly developed miniaturized smartphone-based, electrochemical, immunomagnetic assay. T2 - Electrochemistry 2022 CY - Berlin, Germany DA - 28.09.2022 KW - Cylic Voltammetry KW - Immunoassay KW - TMB KW - Amperometry PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-55876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Hanke, T. A1 - Muth, Thilo A1 - Riedel, Jens A1 - Schilling, Markus A1 - Schweizer, C. A1 - Skrotzki, Birgit A1 - Todor, A. A1 - Moreno Torres, Benjami A1 - Unger, Jörg F. A1 - Völker, Christoph A1 - Olbricht, Jürgen T1 - A Perspective on Digital Knowledge Representation in Materials Science and Engineering N2 - The amount of data generated worldwide is constantly increasing. These data come from a wide variety of sources and systems, are processed differently, have a multitude of formats, and are stored in an untraceable and unstructured manner, predominantly in natural language in data silos. This problem can be equally applied to the heterogeneous research data from materials science and engineering. In this domain, ways and solutions are increasingly being generated to smartly link material data together with their contextual information in a uniform and well-structured manner on platforms, thus making them discoverable, retrievable, and reusable for research and industry. Ontologies play a key role in this context. They enable the sustainable representation of expert knowledge and the semantically structured filling of databases with computer-processable data triples. In this perspective article, we present the project initiative Materials-open-Laboratory (Mat-o-Lab) that aims to provide a collaborative environment for domain experts to digitize their research results and processes and make them fit for data-driven materials research and development. The overarching challenge is to generate connection points to further link data from other domains to harness the promised potential of big materials data and harvest new knowledge. KW - Data infrastructures KW - Digital representations KW - Digital workflows KW - Knowledge graphs KW - Materials informatics KW - Ontologies KW - Vocabulary providers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546729 DO - https://doi.org/10.1002/adem.202101176 SN - 1438-1656 SP - 1 EP - 14 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-54672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tengattini, A A1 - Kardjilov, N A1 - Helfen, L A1 - Douissard, P A A1 - Lenoir, N A1 - Markötter, Henning A1 - Hilger, A A1 - Arlt, T A1 - Paulisch, M A1 - Turek, T A1 - Manke, Ingo T1 - Compact and versatile neutron imaging detector with sub-4μm spatial resolution based on a single-crystal thin-film scintillator N2 - A large and increasing number of scientific domains pushes for high neutron imaging resolution achieved in reasonable times. Here we present the principle, design and performance of a detector based on infinity corrected optics combined with a crystalline Gd3Ga5O12 : Eu scintillator, which provides an isotropic sub-4 μm true resolution. The exposure times are only of a few minutes per image. This is made possible also by the uniquely intense cold neutron flux available at the imaging beamline NeXT-Grenoble. These comparatively rapid acquisitions are compatible with multiple high quality tomographic acquisitions, opening new venues for in-operando testing, as briefly exemplified here. KW - Neutron imaging KW - Scintillator KW - Resolution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549836 DO - https://doi.org/10.1364/oe.448932 VL - 30 IS - 9 SP - 14461 EP - 14477 PB - Optica CY - Washington, DC AN - OPUS4-54983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mani, Deepak A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Diffraction Enhanced Imaging Analysis with Pseudo-Voigt Fit Function N2 - Diffraction enhanced imaging (DEI) is an advanced digital radiographic imaging technique employing the refraction of X-rays to contrast internal interfaces. This study aims at qualitatively and quantitatively evaluating images acquired using this technique and to assess how different fitting functions to the typical rocking curves (RCs) influence the quality of images. RCs are obtained for every image pixel. This allows the separate determination of the absorption and the refraction properties of the material in a position-sensitive manner. Comparison of various types of fitting functions reveals that the Pseudo-Voigt (PsdV) function is best suited to fit typical RCs. A robust algorithm was developed in the Python programming language, which reliably extracts the physically meaningful information from each pixel of the image. We demonstrate the potential of the algorithm with two specimens: a silicone gel specimen that has well-defined interfaces, and an additively manufactured polycarbonate specimen. KW - Diffraction Enhanced Imaging KW - Analyzer-Based Imaging KW - X-ray refraction KW - Non-Destructive Evaluation KW - Pseudo-Voigt fit function KW - Python PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553791 DO - https://doi.org/10.3390/jimaging8080206 SN - 2313-433X VL - 8 IS - 8 SP - 1 EP - 13 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A M A1 - Kardjilov, N A1 - Woracek, R A1 - Boin, M A1 - Markötter, Henning A1 - Kuhn, L T A1 - Makowska, M A1 - Strobl, M A1 - Pfretzschner, B A1 - Banhart, J A1 - Manke, I T1 - Temperature dependence in Bragg edge neutron transmission measurements N2 - A systematic study has been carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength-dependent neutron attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data. A theoretical description that includes the Debye–Waller factor in order to describe the temperature influence on the neutron cross sections was implemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying temperatures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher temperatures, the inelastically scattered intensities increase, and the two can be separated from each other by analysing unique sharp features in the form of Bragg edges. This study presents the first systematic approach to quantify this effect and can serve as a basis , for example, to correct measurements taken during in situ heat treatments, in many cases being a prerequisite for obtaining quantifiable results. KW - Neutron Bragg edge imaging KW - Debye–Waller factor KW - Temperature-dependent neutron transmission KW - Super martensitic stainless steel PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556896 DO - https://doi.org/10.1107/S1600576722006549 VL - 55 IS - Pt 4 SP - 919 EP - 928 PB - International Union of Crystallography AN - OPUS4-55689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Sintschuk, Michael A1 - Britzke, Ralf A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - Upgraded imaging capabilities at the BAMline (BESSY II) N2 - The BAMline at the BESSY II synchrotron X-ray source has enabled research for more than 20 years in widely spread research fields such as materials science, biology, cultural heritage and medicine. As a nondestructive characterization method, synchrotron X-ray imaging, especially tomography, plays a particularly important role in structural characterization. A recent upgrade of key equipment of the BAMline widens its imaging capabilities: shorter scan acquisition times are now possible, in situ and operando studies can now be routinely performed, and different energy spectra can easily be set up. In fact, the upgraded double-multilayer monochromator brings full flexibility by yielding different energy spectra to optimize flux and energy resolution as desired. The upgraded detector (based on an sCMOS camera) also allows exploiting the higher flux with reduced readout times. Furthermore, an installed slip ring allows the sample stage to continuously rotate. The latter feature enables tomographic observation of processes occurring in the time scale of a few seconds. KW - Synchrotron radiation KW - Computed tomography KW - Double-multilayer monochromators KW - Pink beams KW - X-ray optics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556907 DO - https://doi.org/10.1107/S1600577522007342 SN - 1600-5775 VL - 29 IS - Pt 5 SP - 1292 EP - 1298 PB - International Union of Crystallography CY - Chester AN - OPUS4-55690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Stegemann, R. A1 - Lyamkin, V. A1 - Cabeza, S. A1 - Evsevleev, S. A1 - Pelkner, Matthias A1 - Bruno, Giovanni T1 - Subsurface and Bulk Residual Stress Analysis of S235JRC + C Steel TIG Weld by Diffraction and Magnetic Stray Field Measurements N2 - Background Due to physical coupling between mechanical stress and magnetization in ferromagnetic materials, it is assumed in the literature that the distribution of the magnetic stray field corresponds to the internal (residual) stress of the specimen. The correlation is, however, not trivial, since the magnetic stray field is also influenced by the microstructure and the geometry of component. The understanding of the correlation between residual stress and magnetic stray field could help to evaluate the integrity of welded components. Objective This study aims at understanding the possible correlation of subsurface and bulk residual stress with magnetic stray field in a low carbon steel weld. Methods The residual stress was determined by synchrotron X-ray diffraction (SXRD, subsurface region) and by neutron diffraction (ND, bulk region). SXRD possesses a higher spatial resolution than ND. Magnetic stray fields were mapped by utilizing high-spatial-resolution giant magneto resistance (GMR) sensors. Results The subsurface residual stress overall correlates better with the magnetic stray field distribution than the bulk stress. This correlation is especially visible in the regions outside the heat affected zone, where the influence of the microstructural features is less pronounced but steep residual stress gradients are present. Conclusions It was demonstrated that the localized stray field sources without any obvious microstructural variations are associated with steep stress gradients. The good correlation between subsurface residual stress and magnetic signal indicates that the source of the magnetic stray fields is to be found in the range of the penetration depth of the SXRD measurements. KW - Residual stress KW - Magnetic stray field KW - Synchrotron X-ray diffraction KW - Neutron diffraction KW - TIG welding PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547419 DO - https://doi.org/10.1007/s11340-022-00841-x VL - 62 IS - 6 SP - 1017 EP - 1025 PB - Springer AN - OPUS4-54741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni T1 - Micro Non-Destructive Testing and Evaluation N2 - What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue. At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation. In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration. Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress. The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity. Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation. The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E. KW - Ultrasound KW - Materials Characterization KW - Residual Stress KW - Thermography Computed KW - Tomography KW - Non-destructive Testing KW - Magnetic Methods PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556849 DO - https://doi.org/10.3390/ma15175923 VL - 15 IS - 17 SP - 1 EP - 3 PB - MDPI CY - Basel, Schweiz AN - OPUS4-55684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Microstructure characterization of materials using X-ray refraction techniques N2 - X-ray refraction is an excellent tool for the characterization of the microstructure of materials. However, there are only a few (synchrotron) laboratories in the world that use this technique for material characterisation. Therefore, the seminar will first explain the basic principles of X-ray refraction and the measurement techniques installed at the hard X-ray beamline BAMline at BESSY II (Berlin, Germany). This is followed by examples of investigations on fibre-reinforced plastic composites (CFRP) as well as ceramic (Cordierite, ZrO2-SiO2) and metallic materials (Ti-6Al-4V, Inconel). Some of the investigations were carried out both ex-situ and in-situ under mechanical and thermal load. The results are correlated with the mechanical properties of the materials. T2 - LNLS Users Group Seminar Series CY - Campinas, Brasil DA - 25.10.2022 KW - X-ray refraction KW - Analyzer-Based Imaging KW - BAMline PY - 2022 AN - OPUS4-56117 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -