This chapter discusses the practices and procedures used to reveal and record macrostructural features such as hardening depth, weld thickness, crack size, porosity, hot folds, and machining and tooling marks. It provides information on sectioning, sample location, orientation, surface grinding, and etching. It describes macrographic etchants and the features they reveal along with common etching problems and how to avoid them. It explains how to evaluate etching results and how they can be improved using remedial processes such as light grinding. It also discusses photographic reproduction, lighting, and image enhancement techniques.

The analysis of composite materials using optical microscopy is a process that can be made easy and efficient with only a few contrast methods and preparation techniques. This chapter is intended to provide information that will help an investigator select the appropriate microscopy technique for the specific analysis objectives with a given composite material. The chapter opens with a discussion of macrophotography and microscope alignment, and then goes on to describe various illumination techniques that are useful for specific analysis requirements. These techniques include bright-field illumination, dark-field illumination, polarized-light microscopy, interference and contrast microscopy, and fluorescence microscopy. The chapter also provides a discussion of sample preparation materials such as dyes, etchants, and stains for the analysis of composite materials using optical microscopy.

This chapter describes several macroscopic examination techniques, including macroetching, contact printing, fracturing, and lead exudation. It explains how each method is implemented, why it is used, and what it reveals about manufacturing processes, defects, imperfections, and failure mechanisms.

This chapter explains how to prepare metallographic samples for light microscopy and how to anticipate and avoid related problems. It describes standard practices and procedures for sectioning, mounting, grinding, and polishing and identifies common defects along with their causes and cures. It also provides recommendations for handling specific materials and addresses safety concerns.

This chapter explains how to achieve accurate, sharp delineation of the microstructure of metals using appropriate etching and contrasting techniques. It covers a variety of methods, including chemical etching, heat tinting, gas contrasting, vapor deposition, magnetic etching, ion bombardment, and dislocation etch pitting.

This chapter discusses the tools and techniques of light microscopy and how they are used in the study of materials. It reviews the basic physics of light, the inner workings of light microscopes, and the relationship between resolution and depth of field. It explains the difference between amplitude and optical-phase features and how they are revealed using appropriate illumination methods. It compares images obtained using bright field and dark field illumination, polarized and cross-polarized light, and interference-contrast techniques. It also discusses the use of photometers, provides best practices and recommendations for photographing structures and features of interest, and describes the capabilities of hot-stage and hot-cell microscopes.

Hardness tests provide valuable information about the quality of materials and how they are likely to perform in different types of service. This chapter covers some of the most widely used hardness testing methods, including Vickers, Rockwell, and Brinell tests, Shore scleroscope and Equotip hardness tests, and microindentation tests. It describes the equipment and procedures used, discusses the factors that influence accuracy, and provides hardness conversion equations for different types of materials. It also explains how hardness testing sheds light on anisotropy, machinability, wear, fracture toughness, and tensile strength as well as temperature effects, residual stress, and quality control.

This chapter covers the emerging practice of quantitative microscopy and its application in the study of the microstructure of metals. It describes the methods used to quantify structural gradients, volume fraction, grain size and distribution, and other features of interest. It provides examples showing how the various features appear, how they are measured, and how the resulting data are converted into usable form. The chapter also discusses the quantification of fracture morphology and its correlation with material properties and behaviors.

This appendix provides a list of etch compositions and procedures that reveal the macrostructure of aluminum, beryllium, bismuth, antimony, cobalt, copper, lead, magnesium, nickel, tin, titanium, zinc, and their respective alloys as well as iron, steel, noble metals, refractory metals, silicon, zirconium, and hafnium.

This appendix lists copper-containing macroetchants that are used on iron and steel.

This appendix lists etch compositions and procedures that reveal strain patterns in aluminum and nickel-base superalloys.

This appendix lists plating solutions and procedures used in metallographic edge preparation.

This appendix contains recipes of the electrolytic solutions in which various metals are polished in preparation for metallographic examination.

This appendix lists attack-polishing solutions and procedures used in metallographic sample preparation.

This appendix lists chemical polishing solutions and procedures used in metallographic sample preparation.

This appendix provides detailed information on the processes and procedures used in electrolytic polishing. It lists important process parameters, including time, temperature, voltage, and current density, as well as the recipes of electrolytic solutions used. The information is presented in tabular form, corresponding to specific metals and their alloys.

This appendix contains tables that list the composition and capabilities of etchants that reveal the microstructure of metals and alloys, including aluminum, chromium, cobalt, copper, lead, magnesium, molybdenum, nickel, niobium, palladium, platinum, radioactive metals, rare earth metals, rhenium, rhodium, selenium, tellurium, silicon, silver, tantalum, tin, titanium, tungsten, vanadium, and zinc, as well as carbides, oxides, and nitrides.

This appendix is a list of etchants that are used to reveal dislocations in various metals, alloys, and compounds.