This expanded, updated, third edition features many new color illustrations, timely practical examples, and experimental and computational tools introduced in the past ten years, while retaining its excellent introduction to structural characterization and crystallography. The book is written for those interested in a fundamental conceptual understanding powder diffraction and structural characterization of materials as well as in practical skills in examining phase composition and structure of materials using modern experimental powder diffraction tools. Special attention is given to proper collection of powder diffraction data using laboratory x-ray, synchrotron, and neutron radiation. Exemplary data sets serve as a springboard for readers to develop knowledge about modern approaches, algorithms, and software, as well as to gain proficiency in extracting precise structural information about crystalline materials from powder diffraction data. The book requires nospecialized knowledge, so it is useful to beginners. Suitable for upper level undergraduate, and graduate students, as well as practitioners in the research labs and the field, the authors' in-depth treatment helps readers from various disciplines, including crystallography, materials science, solid state chemistry and physics, geology and mineralogy, become experts on this subject.