Development of innovative characterization tools is of paramount importance to advance the frontiers of science and technology in nearly all areas of research. In order to overcome the limitations of individual techniques, correlative microscopy has been recognized as a powerful approach to obtain complementary information about the investigated materials. High-resolution imaging techniques such as Transmission Electron Microscopy (TEM) or Helium Ion Microscopy (HIM) offer excellent spatial resolution. However, the analytical techniques associated with TEM such as Energy Dispersive X-ray spectroscopy (EDX) or Electron Energy-Loss Spectroscopy (EELS) are inadequate for the analysis of (i) isotopes, (ii) trace concentrations (< 0.1 at. % or < 1000 ppm) and (iii) light elements (H, Li, B). Secondary Ion Mass Spectrometry (SIMS), on the other hand, has several advantages such as the possibility to analyse elements and isotopes of all elements of the periodic table while also providing high-sensitivity to detect even trace concentrations. However, the main drawbacks of SIMS are (i) difficulty in quantification and (ii) lateral resolution of SIMS imaging is fundamentally limited by ion-solid interaction volume to ~10 nm. Owing to the complementary strengths of SIMS imaging, we developed new in-situ and operando instrumentations for correlative microscopy combining electron microscopy and SIMS imaging. In this presentation, we will discuss the instrumentation development aspects of correlative microscopy techniques based on SIMS imaging. With a range of examples from energy materials, we will show the powerful correlative microscopy possibilities that emerge due to these new in-situ and operando methods and compare with ex-situ correlation. Our recent work in the application of these methods in hydrogen containing materials and Li ion batteries will be reviewed.
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