The morphology of the electrolyte‐filled pore space in lithium‐ion batteries is determined by the solid microstructure formed by μm‐sized active material particles and the smaller‐featured carbon binder domain (CBD). Tomographic reconstructions have largely neglected the CBD, resulting in inadequately defined pore space morphologies at odds with experimental ionic tortuosity values. We present a three‐phase reconstruction of a LiCoO2 composite cathode by focused ion‐beam scanning electron microscopy tomography. Morphological analysis proves that the reconstruction, which combines an unprecedented volume (20 μm minimum edge length) with the hitherto highest resolution (13.9×13.9×20 nm3 voxel size), represents the cathode's pore space morphology. Pore‐scale diffusion simulations show consideration of the resolved CBD as indispensable to reproduce ionic tortuosity values from electrochemical impedance spectroscopy. Our results reveal the CBD as a convoluted network that dominates the pore space morphology and limits Li+ transport through tortuous and constricted diffusion pathways.
A laser‐based procedure for the preparation of metallic hierarchical porous materials is introduced and exemplified on tin, copper, silicon, titanium, and tungsten surfaces to demonstrate its general applicability. The impact of suitably tuned nanosecond laser pulses triggers a process in which laser‐induced metal ablation and instantaneous recondensation of partially oxidized metals lead to cauliflower‐like superstructures comprising a hybrid micro‐/nanopatterning. Repeated scanning with the intense focused beam over the surface creates microstructures of hierarchically tunable porosity in a layer‐by‐layer design. The 3D morphology of these superstructures is analyzed using tomographic data based on focused ion‐beam scanning electron microscopy to return a fractal dimension of Df = 2.79—practically identical to a natural cauliflower (Df ≈ 2.8), even though the plant is four orders of magnitude larger than the superstructures generated through the laser process. The high Df value signifies a complex morphology that boasts a huge external surface. The introduced concept enables convenient access to a variety of metallic hierarchical porous materials, which are key to performance in environmentally and technologically relevant areas like energy generation, storage, and conversion, as well as sensing and catalysis.
This study explores three unique approaches for closing valves and channels within microfluidic systems, specifically multilayer, centrifugally driven polymeric devices. Precise control over the cessation of liquid movement is achieved through either the introduction of expanding polyurethane foam, the application of direct contact heating, or the redeposition of xerographic toner via chloroform solvation and evaporation. Each of these techniques modifies the substrate of the microdevice in a different way. All three are effective at closing a previously open fluidic pathway after a desired unit operation has taken place, i.e., sample metering, chemical reaction, or analytical measurement. Closing previously open valves and channels imparts stringent fluidic control—preventing backflow, maintaining pressurized chambers within the microdevice, and facilitating sample fractionation without cross-contamination. As such, a variety of microfluidic bioanalytical systems would benefit from the integration of these valving approaches.
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