Focused-Ion-Beam Artifacts and Evidence Reliability in Advanced Microscopy of Energy Materials

Focused-ion-beam scanning electron microscopy (FIB-SEM) provides site-specific access to buried interfaces, particle interiors, porous electrode architectures, and localized degradation regions in energy materials. This capability is particularly valuable for rechargeable batteries, solid-state ion conductors, alkali-metal electrodes, and reactive solid–liquid interfaces, where the structures governing transport and failure are rarely exposed at a free surface. However, the preparation and imaging steps that reveal these regions may also alter them. Ion milling, environmental transfer, vacuum exposure, scanning electron microscopy (SEM), cryogenic handling, transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDS), electron energy-loss spectroscopy (EELS), and atom probe tomography (APT) can each modify local morphology, chemistry, or phase state. These effects are especially important when the intended evidence involves light elements, metastable phases, nanoscale coatings, reactive interphases, volatile species, or ion-conducting materials. This perspective develops a claim-specific framework for evaluating such results. Preparation- and imaging-induced changes are related to the material feature being interpreted and to the minimum control needed to distinguish the two origins. For porous electrodes, the relevant outputs include pore volume, connectivity, tortuosity, crack geometry, phase fraction, and active surface area. For reactive interfaces and solid electrolytes, the critical questions concern alkali-metal redistribution, surface amorphization, light-element contrast, implanted-species chemistry, and beam-induced phase formation. The discussion further compares conventional Ga-FIB, cryogenic FIB, Xe plasma FIB, low-energy Ar+ polishing, broad-ion-beam preparation, ultramicrotomy, and repeated particle-oriented FIB workflows. Reliable interpretation requires the preparation route, transfer conditions, imaging dose, analytical acquisition, and claim-specific controls to be reported together with the final microscopy result.