Sample preparation is very important for crystal structure analysis of novel nano-structured materials in electron microscopy. Generally, a grid dispersion method has been used as transmission electron microscope (TEM) sampling method of nano-powder samples. However, it is diff cult to obtain the cross-sectional information for the tabular-structured materials. In order to solve this problem, we have attempted a new sample preparation method using focused ion beam. Base on this approach, it was possible to successfully obtain the electron diffraction patterns and high-resolution TEM images of the cross-section of tabular structure. Finally, we were able to obtain three-dimensional crystallographic information of novel zeolite nano-crystal of the tabular morphology by applying the new sample preparation technique.