This chapter explains how to measure the shape, size, microstructure, and composition of powders as well as their flowability and crystallization behavior. It presents detailed workflows and calculations based on SEM, TEM, FESEM, and STEM imaging, x-ray diffraction, differential scanning calorimetry, EDS and EELS spectroscopy, and powder sieving. It also discusses the measurement of crystallite size, lattice mismatch, and crystallinity and the relationship between surface area and flowability.

This chapter describes some of the most effective tools for investigating boiler tube failures, including scanning electron microscopy, optical emission spectroscopy, atomic absorption spectroscopy, x-ray fluorescence spectroscopy, x-ray diffraction, and x-ray photoelectron spectroscopy. It explains how the tools work and what they reveal. It also covers the topic of image analysis and its application in the measurement of grain size, phase/volume fraction, delta ferrite and retained austenite, inclusion rating, depth of carburization/decarburization, scale thickness, pearlite banding, microhardness, and hardness profiles. The chapter concludes with a brief discussion on the effect of scaling and deposition and how to measure it.

This chapter covers the early studies and various discoveries by metals researchers to study the internal structure of metals. The topics covered include light microscopy, phase diagrams, X-ray diffraction, principles of precipitation hardening, and dislocation theory.

This appendix provides a detailed overview of the crystal structure of metals. It describes primary bonding mechanisms, space lattices and crystal systems, unit cell parameters, slip systems, and crystallographic planes and directions as well as plastic deformation mechanisms, crystalline imperfections, and the formation of surface or planar defects. It also discusses the use of X-ray diffraction for determining crystal structure.

This article introduces procedures an engineer or materials scientist can use to investigate failures. It provides a brief survey of polymer systems and key properties that need to be measured during failure analysis. The article begins with an overview of the problem-solving approach pertinent to structure analysis. This is followed by a review of the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy. The article then provides information on the distribution of molecular weight of an engineering plastic. It further discusses the methods used in thermal analysis, namely differential thermal analysis, thermogravimetric analysis, thermal-mechanical analysis, and dynamic mechanical analysis. The following sections provide details on X-ray diffraction for analyzing crystalline phases and on a minimal scheme for polymer analysis and characterization to assist the design engineer. The article ends with a discussion on the thermal-analytical scheme for analyzing the milligram quantities of polymer samples.

Several specialized instruments are available for the metallographer to use as tools to gather key information on the characteristics of the microstructure being analyzed. These include microscopes that use electrons as a source of illumination instead of light and x-ray diffraction equipment. This chapter describes how these instruments can be used to gather important information about a microstructure. The instruments covered include image analyzers, transmission electron microscopes, scanning electron microscopes, electron probe microanalyzers, scanning transmission electron microscopes, x-ray diffractometers, microhardness testers, and hot microhardness testers. A list of other instruments that are usually located in a research laboratory or specialized testing laboratory is also provided.