Three-dimensional transmission electron microscopy (3D-TEM), effectuated by multiple imaging of a sample combined with image analysis, offers a new approach in materials science to obtain 3D information of complex solid materials. Here we report first-of-its-kind results that have been obtained with zeolite materials. Virtual cross-sections and volume rendering of the 3D reconstruction of a metal/zeolite crystal (Ag/NaY) give unequivocal information on the location of the silver particles (10-40 nm in diameter). Virtual cross-sections of the 3D reconstruction of an acid-leached mordenite show the three-dimensional mesoporous channel system (3-20 nm in diameter) with a clarity and definition not seen before.Nano-structured inorganic materials, such as solid catalysts, 1 photonic crystals, 2 and electronic devices, 3 are of growing importance in various fields. To gain precision in synthesis and assembly of solids, knowledge of their three-dimensional (3D) structure is required. Electron microscopy is the only technique available to obtain structural information on these types of materials at nanometer scale resolution. However, scanning electron microscopy (SEM) provides surface information with limited information about the internal structure, whereas transmission electron microscopy (TEM) provides only 2D projections of the solid structure. Here we show that 3D-TEM offers a new approach in materials science to obtain 3D information, at nanometer scale resolution, of complex solid materials. 3D-TEM, with its high potential as a unique tool to study biological structures, has rapidly developed during the past few years, which resulted in a first international workshop dedicated to the technique in 1997. 4 Since then, a first generation of automated 3D-TEM data collection systems has become available to the scientific community to study macromolecular structures 5-7 as well as large cellular structures and organelles. 8 So far, it was not recognized that 3D-TEM is also for materials science a unique and powerful tool in the investigation of individual samples of inorganic solids several hundred nanometers in size. With 3D-TEM one can study architecture and composition of individual samples with nanometer scale resolution. 3D-TEM complements other techniques generally used in the characterization of materials such as XRD, XPS, and highresolution TEM. In this paper we describe the principles of 3D-TEM followed by two examples using zeolite materials. The first example involves establishing the location of metal particles in a metal-zeolite crystal (Ag/NaY); the second one involves imaging of mesopores in an acid-leached mordenite crystal.Principles of 3D-TEM. With conventional TEM, images are acquired that are, to a first approximation, 2D projections of a 3D object. Electron tomography, 9 here referred to as 3D-TEM, is a technique where a series of 2D projections (scattering contrast) is recorded that is subsequently used to compute a 3D image (3D reconstruction) of the object under investigation. These projections...