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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.
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.
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.
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.
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.
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.
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.
The mechanical compression of metal foam flow-field based polymer electrolyte fuel cells (PEFCs) is critical in determining the interfacial contact resistance with gas diffusion layers (GDLs), reactant flow and water management.
The distinct scale between the pore structure of metal foams and the entire flow-field warrant a multilength scale characterization that combines ex-situ tests of compressed metal foam samples and in-operando analysis of operating PEFCs using X-ray computed tomography (CT) and neutron radiography. An optimal ‘medium’ compression was found to deliver a peak power density of 853 mW/cm². The X-ray CT data indicates that the compression process significantly decreases the mean pore size and narrows the pore size distribution of metal foams. Simulation results suggest compressing metal foam increases the pressure drop and gas velocity, improving the convective liquid water removal. This is in agreement with the neutron imaging results that demonstrates an increase in the mass of accumulated liquid water with minimum compression compared to the medium and maximum compression cases. The results show that a balance between Ohmic resistance, water removal capacity and parasitic power is imperative for the optimal performance of metal foam based PEFCs.
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.
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.