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- Zeitschriftenartikel (39) (entfernen)
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- Neutron imaging (11)
- Neutron tomography (7)
- Neutron radiography (5)
- Tomography (5)
- Fuel cell (4)
- Bragg-edge imaging (3)
- Computed tomography (3)
- Debye–Waller factor (3)
- Phase distribution (3)
- Austenite-to-martensite transformation (2)
Organisationseinheit der BAM
Ein effektives Wassermanagement ist ein wichtiger Aspekt in der Entwicklung von Brennstoffzellen hinsichtlich Langzeitstabilität und Optimierung der Leistungsfähigkeit. Eine zentrale Rolle spielt dabei die Gasdiffusionslage, die für die gleichmäßige Verteilung der Reaktionsgase auf die elektrochemisch aktive Schicht (Katalysator) sorgen soll. In diesem Beitrag werden gemeinsame Forschungsaktivitäten des Helmholtz-Zentrums Berlin für Materialien und Energie (Entwicklung bildgebender Verfahren) sowie des Zentrums für Sonnenenergie- und Wasserstoff-Forschung (ZSW, Entwicklung von Brennstoffzellen) vorgestellt. Im Rahmen dieser Kooperation werden die Entstehung, die Verteilung und der Transport von flüssigem Wasser, kurz das Wassermanagement, unter Betriebsbedingungen untersucht. Mittels Synchrotronradiografie und -tomografie werden kleinste Wassercluster in der Gasdiffusionslage detektiert. Die gewonnenen Erkenntnisse dienen der Modifikation und einer gezielten Auswahl der eingesetzten Materialien.
Die Aufklärung spezifischer Fragestellungen zur Funktionalität von PEM(polymer electrolyte membrane)- und DMFC(Direct Methanol)-Brennstoffzellen bedarf der 3D-Abbildung der spezifischen Komponenten mit unterschiedlichen Strahlungsarten: des Wassergehalts in den Flow Fields mit Neutronen, der Katalysator-Alterung in der MEA (membrane electrode assembly) mit Synchrotronstrahlung und der freien (reaktiven) Katalysator-Oberfläche von Nano-Partikeln mit TEM-Elektronen-Tomografie. Diese Messungen im Bereich der mm- bis nm-Skala unterliegen dabei erheblichen Restriktionen: einer ortsabhängigen Verschmierung der Neutronenradiogramme, Manipulatorinstabilitäten der Synchrotronmessungen sowie einer Kombination von Limited-View-Datensätzen, wenigen Projektionswinkeln und teilweiser Nichtdurchstrahlbarkeit in der Elektronen-CT. Die Vorteile eines fortentwickelten Directt-Algorithmus für die Bewältigung dieser Randbedingungen gegenüber gefilterten Rückprojektionen werden aufgezeigt.
In-situ-Neutronenradiografie wird erfolgreich eingesetzt, um flüssiges Wasser in Niedertemperatur-PEM-Brennstoffzellen während des Betriebs zerstörungsfrei abzubilden und das sogenannte Wassermanagement eine der größten Herausforderungen der Entwicklung durch Anpassung der Materialeigenschaften zu optimieren. Dabei werden die besonderen Eigenschaften der Neutronen genutzt, die metallische Bauteile relativ leicht durchdringen, während selbst kleine Wassermengen durch ihre starke Streuung leicht nachweisbar sind. Die relativ langen Messzeiten für die Neutronentomografie werden durch den Betrieb der Zelle im angehaltenen Zustand realisierbar, sodass die dreidimensionale Wasserverteilung darstellbar wird.
Magnetic domains have been the subject of much scientific investigation since their theoretical existence was first postulated by P.-E. Weiss over a century ago. Up to now, the three-dimensional (3D) domain structure of bulk magnets has never been observed owing to the lack of appropriate experimental methods. Domain analysis in bulk matter thus remains one of the most challenging tasks in research on magnetic materials. All current domain observation methods are limited to studying surface domains or thin magnetic films. As the properties of magnetic materials are strongly affected by their domain structure, the development of a technique capable of investigating the shape, size and distribution of individual domains in three dimensions is of great importance. Here, we show that the novel technique of Talbot-Lau neutron tomography with inverted geometry enables direct imaging of the 3D network of magnetic domains within the bulk of FeSi crystals.
Water transport in an operating PEM fuel cell was investigated with synchrotron X-ray radiography with a spatial resolution of 3 µm and a temporal resolution of 5 s. This method allows for the detection of water accumulations with less than 10 µm diameter. We demonstrate that synchrotron X-ray imaging can dramatically expand the possibilities of imaging with high spatial and time resolution, especially as a complement to neutron radiography. Water transport processes from the first appearance of small water accumulations in the gas diffusion layer to their transport into the channel system were analysed in situ. Correlations between local effects such as water formation and operating conditions of the whole system, e.g. power variations, were found. A recently described eruptive water transport mechanism is analysed in detail.
This paper gives a brief overview on3D imaging of magnetic domains with shearing grating neutron tomography. We investigated the three-dimensional distribution of magnetic domain walls in the bulk of a wedge-shaped FeSi single crystal. The width of the magnetic domains wasanalyzed at different locations within the crystal. Magnetic domains close to the tip of the wedge are much smaller than in the bulk. Furthermore, the three-dimensional shape of individual domains wasinvestigated. We discuss prospects and limitations of the applied measurement technique.
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.
Die Computer-gestützte Laminografie (CL) wurde als komplementäre Methode zur Computertomografie für die dreidimensionale Bildgebung von lateral ausgedehnten Objekten entwickelt. Ursprünglich für medizinische Zwecke verwendet, wurde diese Methode kürzlich als zerstörungsfreie nicht-invasive Methode nicht nur in der Materialforschung, sondern auch mit steigendem Interesse für kunsthandwerkliche und historische Objekte eingesetzt. Hier wird die Computer-gestützten Laminografie mit polychromatischer Neutronenstrahlung an einer historischen Tsuba eingesetzt, einem Stichblatt eines japanischen Schwerts. Eine Analyse der Lötstellen gibt Rückschlüsse auf das Herstellungsverfahren. Zudem wurden unterschiedliche Materialsysteme gefunden, vermutlich um dem Tsuba lokal eine höhere Stabilität zu verleihen. Die Messungen wurden an der Imaging-Beamline CONRAD-2 an der Neutronenquelle BER 2 des Helmholtz-Zentrums Berlins (HZB) durchgeführt.
We investigated the hydrogen distribution spatially and temporally in technical iron at room temperature. Samples were charged electrochemically and subsequently analysed by means of neutron radiography and tomography. The radiographic images allowed for a time-resolved analysis of hydrogen fluxes. The three-dimensional distribution of hydrogen measured by neutron tomography delivered valuable information for the damage analysis of hydrogen-induced cracks. For the first time hydrogen concentration gradients inside the material could be detect directly together with the cracks. The neutron radiography and tomography results were gained at the Research Reactor BER II of the HZB in Berlin.
We investigated hydrogen embrittlement and blistering in electrochemically hydrogen-charged technical iron samples at room temperature. Hydrogen-stimulated cracks and blisters and the corresponding hydrogen distributions were observed by neutron tomography. Cold neutrons were provided by the research reactor BER II to picture the sample with a spatial resolution in the reconstructed three-dimensional model of ~25 µm. We made the unique observation that cracks were filled with molecular hydrogen and that cracks were surrounded by a 50 µm wide zone with a high hydrogen concentration. The zone contains up to ten times more hydrogen than the bulk material. The hydrogen enriched zone can be ascribed to a region of increased local defect density. Hydrogen also accumulated at the sample surface having the highest concentration at blistered areas. The surfaces of the brittle fractured cracks showed micropores visualized by scanning electron microscopy. The micropores were located at grain boundaries and were surrounded by stress fields detected by electron backscattered diffraction. The cracks clearly originated from the micropores.
Neutron tomography has been applied to investigate the mechanism of hydrogen assisted cracking in technical iron and supermartensitic steel. Rectangular technical iron block samples showed blistering due to intense hydrogen charging and the tomographic method revealed in situ the spatial distribution of hydrogen and cracks. Hydrogen accumulated in a small region around cracks and the cracks are filled with hydrogen gas. Cracks close to the surface contained no hydrogen. Hydrogenous tensile test samples of supermartensitic steel were pulled until rupture and showed hydrogen accumulations at the notch base and in the plastically deformed region around the fracture surface.
A new high-resolution detector setup for neutron imaging has been developed based on infinity-corrected optics with high light collection, combined with customized mounting hardware. The system can easily be installed, handled and fitted to any existing facility, avoiding the necessity of complex optical systems or further improved electronics (CCD). This is the first time optical magnification higher than 1:1 has been used with scintillator-based neutron detectors, as well as the first implementation of infinity corrected optics for neutron imaging, achieving the smallest yet reported effective pixel size of 3.375 µm. A novel transparent crystal scintillator (GGG crystal) has been implemented with neutrons for the first time to overcome limitations of traditional powder scintillators (Li6/ZnS, Gadox). The standardized procedure for resolution measurements with the Modulation Transfer Function (MTF) is summarized to facilitate comparison between instruments and facilities. Using this new detector setup, a resolution of 14.8 µm with a field of view of 6 mm × 6 mm has been achieved while maintaining reasonable count times. These advances open a wide range of new possible research applications and allow the potential for additional future developments.
CT (computed tomography) reconstructions of fuel cell components of a yet unrivaled spatial resolution and quality are presented. This is achieved by application of the novel DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm. We focus on two different key issues which essentially rule the fuel cell's durability on different length scales and physical interactions. On the resolution scale of some 100 µm agglomerations of condensed water in flow-field channels are detected by means of quasi-in situ neutron CT (after operation). Five orders of magnitude below nanometer sized Ru catalyst particles on carbon black support are visualized by electron tomography. Both types of experiments are especially adapted to the type of material involved but they are accompanied by severe deviations from ideal CT measuring conditions, as well. In order to overcome the tremendous reconstruction artifacts of standard algorithms, we employ DIRECTT which is described in detail. Comparisons of DIRECTT reconstructions to the conventional filtered back projection, prove the significant improvements in both experimental methods.
In recent years, low-temperature polymer electrolyte fuel cells have become an increasingly important pillar in a zero-carbon strategy for curbing climate change, with their potential to power multiscale stationary and mobile applications. The performance improvement is a particular focus of research and engineering roadmaps, with water management being one of the major areas of interest for development. Appropriate characterisation tools for mapping the evolution, motion and removal of water are of high importance to tackle shortcomings.
This article demonstrates the development of a 4D high-speed neutron imaging technique, which enables a quantitative analysis of the local water evolution. 4D visualisation allows the time-resolved studies of droplet formation in the flow fields and water quantification in various cell parts. Performance parameters for water management are identified that offer a method of cell classification, which will, in turn, support computer modelling and the engineering of next-generation flow field designs.
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.
In various kinds of radiography, deficient transmission imaging may occur due to backlighting inside the detector itself arising from light or radiation scattering. The related intensity mismatches barely disturb the high resolution contrast, but its long range nature results in reduced attenuation levels which are often disregarded. Based on X-ray observations and an empirical formalism, a procedure is developed for a first order correction of detector backlighting. A backlighting factor is modeled as a function of the relative detector coverage by the sample projection. Different cases of sample transmission are regarded at different backlight factors and detector coverage. The additional intensity of backlighting may strongly affect the values of materials’ attenuation up to a few 10%. The presented scenario provides a comfortable procedure for corrections of X-ray or neutron transmission imaging data.
The ability to track electrode degradation, both spatially and temporally, is fundamental to understand performance loss during operation of lithium batteries. X-ray computed tomography can be used to follow structural and morphological changes in electrodes; however, the direct detection of electrochemical processes related to metallic lithium is difficult due to the low sensitivity to the element. In this work, 4-dimensional neutron computed tomography, which shows high contrast for lithium, is used to directly quantify the lithium diffusion process in spirally wound Li/SOCl2 primary cells. The neutron dataset enables the quantification of the lithium transport from the anode and the accumulation inside the SOCl2 cathode to be locally resolved. Complementarity between the collected neutron and X-ray computed tomographies is shown and by applying both methods in concert we have observed lithium diffusion blocking by the LiCl protection layer and identified all cell components which are difficult to distinguish using one of the methods alone.
The understanding of dynamic processes in Li-metal batteries is an important consideration to enable the full capacity of cells to be utilised. These processes, however, are generally not directly observable using X-ray techniques due to the low attenuation of Li; and are challenging to visualise using neutron imaging due to the low temporal resolution of the technique. In this work, complementary X-ray and neutron imaging are combined to track the dynamics of Li within a primary Li/SOCl2 cell. The temporal challenges posed by neutron imaging are overcome using the golden ratio imaging method which enables the identification of Li diffusion in operando. This combination of techniques has enabled an improved understanding of the processes which limit rate performance in Li/SOCl2 cells and may be applied beyond this chemistry to other Li-metal cells.
This work describes the effects of catalyst layers (CLs) consisting of hydrophobic PTFE on the performance and water management of PEM fuel cells. Catalyst inks with various PTFE contents were coated on Nafion membranes and characterized using contact angle measurements, SEX-EDX, and mercury porosimetry. Fuel cell tests and electrochemical impedance spectroscopy (EIS) were conducted under varying operating conditions for the prepared materials. At dry conditions, CLs with 5 wt.% PTFE were advantageous for cell performance due to improved membrane hydration, whereas under humid conditions and high air flow rates CLs with 10 wt.% PTFE improved the performance in high current density region. Higher PTFE contents (⩾20 wt.%) increased the mass transport resistance due to reduced porosity of the CLs structure. Operando neutron radiography was utilized to study the effects of hydrophobicity gradients within CLs and cathode microporous layer (MPLC) on liquid water distribution. More hydrophobic CLs increased the water content in adjacent layers and improved performance, especially at dry conditions. MPLC with higher PTFE contents increased the overall liquid water within the CLs and GDLs and escalated the water transfer to the anode side. Furthermore, the role of back-diffusion transport mechanism on water distribution was identified for the investigated cells.
Spectral neutron tomography
(2021)
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.