In thermal oxidation studies, the structure of the oxide-metal interface and the near-surface region is of great importance. A technique has been developed for constructing cross-sectional samples of oxidized aluminum alloys, which reveal these regions. The specimen preparation procedure is as follows: An ultra-sonic drill is used to cut a 3mm diameter disc from a 1.0mm thick sheet of the material. The disc is mounted on a brass block with low-melting wax, and a 1.0mm hole is drilled in the disc using a #60 drill bit. The drill is positioned so that the edge of the hole is tangent to the center of the disc (Fig. 1) . The disc is removed from the mount and cleaned with acetone to remove any traces of wax. To remove the cold-worked layer from the surface of the hole, the disc is placed in a standard sample holder for a Tenupol electropolisher so that the hole is in the center of the area to be polished.