Transmission electron microscopy (TEM) is a useful tool in process evaluation and failure analysis for semiconductor industries. A common focus of semiconductor TEM analyses is metalization vias (plugs) and it is often desirable to cross-section through a particular one. If the cross-sectional plane deviates away from the center of the plug, then the thin adhesion layer around the plug will be blurred by surrounding materials such as the inter-layer dielectric and the plug material. The importance of these constraints, along with the difficulty of precision sample preparation, has risen sharply as feature sizes have fallen to 0.25 μm and below. The suitability of common sample preparation techniques for these samples is evaluated.