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In this investigation, synchrotron X-ray imaging was used to investigate the water distribution inside newly developed gas diffusion media in polymer electrolyte membrane fuel cells. In-situ radiography was used to reveal the relationship between the structure of the microporous layer (MPL) and the water flow in a newly developed MPL equipped with randomly arranged holes. A strong influence of these holes on the overall water transport was found. This contribution provides a brief overview to some of our recent activities on this research field.
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.
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.
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.
While X-ray based darkfield imaging with grating interferometers is already widely used, darkfield imaging with neutrons has still a relatively small user community focused mostly on magnetic materials. Here, we demonstrate the application of neutron darkfield imaging byTalbot-Lau type grating interferometry to fiber reinforced plastics. Common carbon and glass fiber composites have been investigated including characteristic damage structures. The darkfield images show a strong signal response caused by fiber delamination, suitable fiber direction, particles, pores and cracks. The basic principles of neutron darkfield imaging applied to fiber composites are highlighted.
Metal-based gas diffusion electrodes are utilized in chlor-alkali electrolysis or electrochemical reduction of carbon dioxide, allowing the reaction to proceed at high current densities. In contrast to planar electrodes and predominantly 2D designs, the industrially required high current densities can be achieved by intense contact between the gas and liquid phase with the catalytically active surfaces. An essential asset for the knowledge-based design of tailored electrodes is therefore in-depth information on electrolyte distribution and intrusion into the electrode’s porous structure. Lab-based and synchrotron radiography allow for monitoring this process operando. Herein, we describe the development of a cell design that can be modularly adapted and successfully used to monitor both the oxygen reduction reaction and the electrochemical reduction of CO2 as exemplary and currently very relevant examples of gas-liquid reactions by only minor modifications to the cell set-up. With the reported cell design, we were able to observe the electrolyte distribution within the gas diffusion electrode during cell operation in realistic
conditions.
The neutron imaging instrument CONRAD was operated as a part of the user program of the research reactor BER‐II at Helmholtz‐Zentrum Berlin (HZB) from 2005 to 2020. The Instrument was designed to use the neutron flux from the cold source of the reactor, transported by a curved neutron guide. The pure cold neutron spectrum provided a great advantage in the use of different neutron optical components such as focusing lenses and guides, solid‐state polarizers, Monochromators and phase gratings. The flexible setup of the instrument allowed for implementation of new methods including wavelength‐selective, dark‐field, phase‐contrast and imaging with polarized neutrons. In summary, these developments helped to attract a large number of scientists and industrial customers, who were introduced to neutron imaging and subsequently contributed to the Expansion of the neutron imaging community.
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.
The potentials of incoherent X-ray scattering (Compton) computed tomography (CT) are investigated. The imaging of materials of very different atomic number or density at once is generally a perpetual challenge for X-ray tomography or radiography. In a basic laboratory set-up for simultaneous perpendicular Compton scattering and direct beam attenuation tomography are conducted by single channel photon counting line scans. This results in asymmetric distortions of the projection profiles of the scattering CT data set. In a first approach, corrections of Compton scattering data by taking advantage of rotational symmetry yield tomograms without major geometric artefacts. A cylindrical sample composed of PE, PA, PVC, glass and wood demonstrates similar Compton contrast for all the substances, while the conventional absorption tomogram only reveals the two high order materials. Comparison to neutron tomography
reveals astonishing similarities except for the glass component (without hydrogen). Therefore, Compton CT offers the potential to replace neutron tomography, which requires much more efforts.