The thin scanning transmission electron microscopy foil restricts scattering to a much smaller projected specimen volume than bulk SEM at . It reveals the nanoscale shape and continuity of the gold/NiP interface, the narrow low-density opening and the fine heterogeneous region underneath the gold, which the larger SEM interaction volume and surface-sensitive collection obscure.
The enlarged view resolves structure on the tens-of-nanometres scale: local interface roughness, small bright and dark domains and the relationship of the gold layer to the damaged or porous-looking NiP region. This helps distinguish an interface-associated defect from merely a change between nominal alloy layers. It still does not identify a crystalline phase or quantify composition without diffraction or spectroscopic analysis. Since the SEM surface and focused ion beam milling lamella need not cut precisely the same volume, correlations should allow for section position.
The conspicuous approximately vertical streaks are focused ion beam milling curtaining: different sputtering rates beneath the rough, compositionally varying cap and interfaces leave stripes of different foil thickness. The uneven lower foil edge, contrast gradient and locally thinned regions are also consistent with nonuniform milling; redeposition can add material to other regions.
A dark gap or pull-out may have been enlarged or created during milling, so its original dimensions cannot be inferred securely from this one image. ion implantation and an amorphized surface layer are additional possible focused ion beam milling effects, but they are not independently demonstrated by these intensity variations. A lower-energy final polish, improved protective cap and examination of another lamella could test the preparation contribution.
Use high-resolution transmission electron microscopy with a coherent, well-aligned beam and an objective aperture admitting the direct beam and the spatial frequencies required at the interface. Orient a crystalline region near a suitable zone axis so that useful lattice fringes are excited; minimize drift, vibration and astigmatism. Choose defocus and aberration correction to transfer the target frequencies, rather than treating the image as a direct map of atoms at arbitrary defocus.
An aberration-corrected scanning transmission electron microscopy probe with high-angle annular dark-field imaging can instead resolve an interface with more directly interpretable atomic-number contrast. A nominal thickness may be too great for clean atomic-resolution interpretation: thin the interface further if necessary, finish focused ion beam milling at lower ion energy to reduce damaged surface layers, and check for curtaining and implantation. The best mode depends on crystallinity and damage sensitivity; an amorphous interface calls for resolving its boundary and composition rather than inventing lattice fringes.