This paper describes a novel method of sample preparation for Transmission Electron Microscope (TEM) analysis, particularly a technique for photoresist sample preparation for TEM analysis. In the analysis of an ultra large scale integrated (ULSI) circuit, the profile images of a ULSI circuit sample are crucial. In order to identify the tiny features of modern semiconductor devices clearly, TEMs are used because of their high spatial resolution. However, the TEM analysis is not available for photoresist materia, especially for a patterned photoresist layer, due to the difficulty in specimen preparation and its susceptibility to electron beam damage during TEM analysis. A critical step in preparing this type of TEM specimens is to deposit a conductive layer and a dielectric layer upon the patterned phototresist by a physical vapor deposition process at room temperature first, then followed by a focus ion beam (FIB) process. The exact profile of the patterned photoresist is kept, during specimen preparation and TEM analysis, by this modified method. Precise dimension measurements are then possible.