Laser preparation for large‐scale FIB‐SEM tomography: Extended abstract

Abstract

Focused Ion Beam‐Scanning Electron Microscopy (FIB‐SEM) combined with Energy‐Dispersive X‐ray Spectroscopy (EDX) is a powerful tool for high‐resolution 3D characterization of cement‐based materials. However, conventional in‐bulk serial sectioning suffers from shadowing, material redeposition, and charging artifacts due to geometric constraints, while alternative lift‐out methods are highly time‐consuming. To address these limitations, this study utilizes femtosecond (fs) laser ablation for initial specimen preparation. Laser ablation rapidly creates large, deep trenches (e.g., 0.6 × 1.0 mm, >100 μm deep), significantly reducing geometric constraints, reducing artifacts, and enabling large‐scale analysis, such as the Interfacial Transition Zone. Although the laser induces an amorphous layer of up to 2 μm, this is easily removed via a final FIB polish. By coupling this rapid pre‐preparation with optimized low‐damage EDX acquisition, this workflow enables the efficient, artifact‐minimized acquisition of large‐scale, high‐resolution 3D datasets, overcoming the severe volumetric limitations of the traditional lift‐out approach.