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Correlative microscopy approaches are attracting considerable interest in several research fields such as materials and battery research. Recent developments regarding X-ray computer tomography have made this technique available in a compact module for scanning electron microscopes (SEMs). Nano-computed tomography (nanoCT) allows morphological analysis of samples in a nondestructive way and to generate 2D and 3D overviews. However, morphological analysis alone is not sufficient for advanced studies, and to draw conclusions beyond morphology, chemical analysis is needed. While conventional SEM-based chemical analysis techniques such as energy-dispersive X-ray spectroscopy (EDS) are adequate in many cases, they are not well suited for the analysis of trace elements and low-Z elements such as hydrogen or lithium. Furthermore, the large information depth in typical SEM-EDS imaging conditions limits the lateral resolution to micrometer length scales. In contrast, secondary ion mass spectrometry (SIMS) can perform elemental mapping with good surface sensitivity, nanoscale lateral resolution, and the possibility to analyze even low-Z elements and isotopes. In this study, we demonstrate the feasibility and compatibility of a novel FIB-SEM-based correlative nanoCT-SIMS imaging approach to correlate morphological and chemical data of the exact same sample volume, using a cathode material of a commercial lithium battery as an example.
A method for rapid quantitative imaging of dopant distribution using secondary ion mass spectrometry (SIMS) is described. The method is based on SIMS imaging of the cross-section of a reference sample with a known concentration profile. It is demonstrated for the case of boron quantification in silicon in a SIMS imaging mode. A nonlinear relationship between the secondary ion intensity and the concentration is observed. A detection limit of 3 (±2) × 1017 at./cm3 (~6 ppm) is determined with 39 nm pixel-size for the used experimental conditions. As an application example, a boron concentration profile in a passivating contact deposited on a textured Si surface is analyzed.