SINOPSIS

Recent breakthroughs have enabled the synthesis of engineered 3D microstructures in materials used, for example, in energy storage and conversion, telecommunications, medicine, and electronics. The direct measurement of material properties, especially in 3D, of such materials has been particularly challenging. Synchrotron-based transmission X-ray microscopy, a microscope constructed to utilize a high brilliance, tunable synchrotron X-ray source, provides detailed 3D microstructural images at nanoscale resolution with the ability to obtain 3D elemental speciation and chemical bonding information. In this chapter, transmission X-ray microscopy is described along with techniques such as X-ray nanoto-mography, differential X-ray absorption contrast imaging, and XANES nanotomography, which are used to obtain structural, elemental, and chemical bonding information of material structures in 3D. A discussion of tomographic reconstruction and imaging processing techniques used to prepare data for analysis is also included. Examples for calculation of structural properties such as void fraction, connectivity, tortuosity, interfacial contact area, triple-phase boundary length, and curvature are also presented. This chapter concludes with a discussion on the use of imaged data sets for numerical simulation of transport phenomena, chemical/electrochemical reactions, and microstructural evolution. These 3D property measurement methods are envisioned to enable the advancement of next-generation 3D engineered materials.