Abstract
Vast quantities of powder leave production lines each day, often with strict control measures. For quality checks to provide the most value, they must be capable of screening individual particles in 3D and at high throughput. Conceptually, X‐ray computed tomography (CT) is capable of this; however, achieving lab‐based reconstructions of individual particles has, until now, relied upon scan‐times on the order of tens of hours, or even days, and although synchrotron facilities are potentially capable of faster scanning times, availability is limited, making in‐line product analysis impractical. This work describes a preparation method and high‐throughput scanning procedure for the 3D characterization of powder samples in minutes using nano‐CT by full‐filed transmission X‐ray microscopy with zone‐plate focusing optics. This is demonstrated on various particle morphologies from two next‐generation lithium‐ion battery cathodes: LiNi0.8Mn0.1Co0.1O2 and LiNi0.6Mn0.2Co0.2O2; namely, NMC811 and NMC622. Internal voids are detected which limit energy density and promote degradation, potentially impacting commercial application such as the drivable range of an electric vehicle.
Highlights
Vast quantities of powder leave production lines each day, often with strict morphology and performance, many industries are required to produce very control measures
Powder is dispersed over an adhesive-covered surface of Kapton tape and the excess powder is removed by tapping the tape perpendicular to a surface to disperse and settle the powder layer
An X-ray radiograph mosaic was collected without angular rotation, regions of interest (ROIs) were chosen for 3D analysis
Summary
The two NMC samples were assessed using the optimized preparation and data acquisition methods for maximum image quality, with minimal acquisition time. This preparation involves the production of an approximately monolayer dispersion of particles onto an X-ray transparent mechanical support. Powder is dispersed over an adhesive-covered surface of Kapton tape and the excess powder is removed by tapping the tape perpendicular to a surface to disperse and settle the powder layer. The NMC811 ROIs were chosen because they appeared to contain particles of various sizes, i.e., would provide sufficient tests for the versatility of the technique. For an exposure time of 1 s and scan duration of approximately 5 min (Figures S4, S5, Supporting Information), the average signal to noise (SNR) for the particles resolved within these tomograms was found to be 10.4, sufficient for the analysis (Figure S6, Supporting Information)
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