The reflected light microscope is the most commonly used tool to study the microstructure of metals, composites, ceramics, minerals, and polymers. For the study of the microstructure of metals and alloys, light microscopy is employed in the reflected-light mode using either bright-field illumination, dark-field illumination, polarized light illumination, or differential interference contract, generally by the Nomarski technique. This article concentrates on how to reveal microstructure properly to enable the proper identification of the phases and constituents and, if needed, measuring the amount, size, and spacing of constituents, using the light optical microscope. The discussion covers the examination of microstructures using different illumination methods and includes a comparison between light optical images and scanning electron microscopy images of microstructure.

This article describes the methods and equipments involved in the preparation of specimens for examination by light optical microscopy, scanning electron microscopy, electron microprobe analysis for microindentation hardness testing, and for quantification of microstructural parameters, either manually or by the use of image analyzers. Preparation of metallographic specimens generally requires five major operations: sectioning, mounting, grinding, chemical polishing, and etching. The article provides information on the principles of technique selection in mechanical polishing, and describes the procedures, advantages, and disadvantages of electrolytic and chemical polishing. It also provides a detailed account of procedures, precautions, and composition for preparation and handling of etchants.

Quantitative image analysis has expanded the capabilities of surface analysis significantly with the use of computer technology. This article provides an overview of the quantitative image analysis and optical microscopy. It describes the various steps involved in surface preparation of samples prone to abrasion damage and artifacts for quantitative image analysis.

Measuring the thickness of thin films can be accomplished in many ways. This article focuses on the optical method of single-wavelength ellipsometry, two multiple-wavelength methods of reflectometry and spectroscopic ellipsometry for measuring the thickness of thin films. The general capabilities, principles and applications of ellipsometry and reflectometry are discussed in terms of nondestructive methods.

The application of transmission electron microscope to the study of fracture surfaces and related phenomena has made it possible to obtain magnifications and depths of field much greater than those possible with light (optical) microscopes. This article reviews the methods for preparing single-stage, double-stage, and extraction replicas of fracture surfaces. It discusses the types of artifacts and their effects on these replicas, and provides information on shadowing of replicas. The article concludes with a comparison of the transmission electron and scanning electron fractographs with illustrations.

The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.

Transmission electron microscopy (TEM) approach enables essentially simultaneous examination of microstructural features through imaging from lower magnifications to atomic resolution and the acquisition of chemical and crystallographic information from small regions of the thin specimen. This article discusses fundamentals of the technique, especially for solving materials problems. Background information is provided to help understand basic operations and principles, including instrumentation, the physics of signal generation and detection, image formation, electron diffraction, and spectrometry techniques with data analysis.

This article provides detailed information on the instrumentation and principles of the scanning electron microscope (SEM). It begins with a description of the primary components of a conventional SEM instrument. This is followed by a discussion on the advantages and disadvantages of the SEM compared with other common microscopy and microanalysis techniques. The following sections cover the critical issues regarding sample preparation, the physical principles regarding electron beam-sample interaction, and the mechanisms for many types of image contrast. The article also presents the details of SEM-based techniques and specialized SEM instruments. It ends with example applications of various SEM modes.

This article discusses the fundamentals and operating principles of the following acoustic microscopy methods: scanning laser acoustic microscopy, C-mode scanning acoustic microscopy, and scanning acoustic microscopy. It describes the applications of acoustic microscopy for detecting defects in metals, ceramics, glasses, polymers, and composites with examples.

This article provides an overview of scanning probe microscopes (scanning tunneling microscope and atomic force microscope (AFM)), covering the various operating modes and probes used in these instruments and providing information on AFM instrumentation, applications, and analyses.

This article focuses on laboratory atomic force microscopes (AFMs) used in ambient air and liquid environments. It begins with a discussion on the origin of AFM and development trends occurring in AFM. This is followed by a section on the general principles of AFM and a comprehensive list of AFM scanning modes. There is a brief description of how each mode works and what types of applications can be made with each mode. Some of the processes involved in preparation of samples (bulk materials and those placed on a substrate) scanned in an AFM are then presented. The article provides information on the factors applicable to the accuracy and precision of AFM measurements. It ends by discussing the applications for AFMs in the fields of science, technology, and engineering.

This article presents examples of the visual fracture examination that illustrate the procedure as it applies to failure analysis and quality determination. It describes the techniques and procedures for the visual and light microscopic examination of fracture surfaces with illustrations. The article also describes microscopic and macroscopic features of the different fracture mechanisms with illustrations with emphasis on visual and light microscopy examination. The types of fractures considered include ductile fractures, tensile-test fractures, brittle fractures, fatigue fractures, and high-temperature fractures.

Scanning electron microscopy (SEM) has unique capabilities for analyzing fracture surfaces. This article discusses the basic principles and practice of SEM, with an emphasis on its applications in fractography. The topics include an introduction to SEM instrumentation, imaging and analytical capabilities, specimen preparation, and the interpretation of fracture features. SEM can be subdivided into four systems, namely, illuminating/imaging, information, display, and vacuum systems. The article also describes the major criteria and techniques of SEM specimen preparation, and the general features of ductile and brittle fracture modes.

This article briefly discusses popular techniques for metals characterization. It begins with a description of the most common techniques for determining chemical composition of metals, namely X-ray fluorescence, optical emission spectroscopy, inductively coupled plasma optical emission spectroscopy, high-temperature combustion, and inert gas fusion. This is followed by a section on techniques for determining the atomic structure of crystals, namely X-ray diffraction, neutron diffraction, and electron diffraction. Types of electron microscopies most commonly used for microstructural analysis of metals, such as scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy, are then reviewed. The article contains tables listing analytical methods used for characterization of metals and alloys and surface analysis techniques. It ends by discussing the objective of metallography.

Fractography is the systematic study of fractures and fracture surfaces. It is a useful tool in failure analysis and provides a means for correlating the influence of microstructure on the fracture mode of a given material. This article discusses the preservation, preparation, and photography of fractured parts and surfaces, and describes some of the more common fractographic features revealed by light microscopy, including tensile-fracture surface marks in unnotched specimens, fatigue marks, and structural discontinuities within the metal. The article also explains how to interpret fracture information contained in optical and scanning-electron microscope fractographs.

Nanotechnology and smart-coating technologies have been reported to show great promise for improved performance in critical areas such as corrosion resistance, durability, and conductivity. This article exemplifies nanofilms and nanomaterials used in coatings applications, including carbon nanotubes, silica, metals/metal oxides, ceramics, clays, buckyballs, graphene, polymers, titanium dioxide, and waxes. These can be produced by a variety of methods, including chemical vapor deposition, plasma arcing, electrodeposition, sol-gel synthesis, and ball milling. The application of nanotechnology and the development of smart coatings have been dependent largely on the availability of analytical and imaging techniques such as Raman spectroscopy, scanning and transmission electron microscopy, atomic force microscopy, and scanning tunneling microscopy.

This article describes testing and characterization methods of ceramics for chemical analysis, phase analysis, microstructural analysis, macroscopic property characterization, strength and proof testing, thermophysical property testing, and nondestructive evaluation techniques. Chemical analysis is carried out by X-ray fluorescence spectrometry, atomic absorption spectrophotometry, and plasma-emission spectrophotometry. Phase analysis is done by X-ray diffraction, spectroscopic methods, thermal analysis, and quantitative analysis. Techniques used for microstructural analysis include reflected light microscopy using polarized light, scanning electron microscopy, transmission electron microscopy, energy dispersive analysis of X-rays, and wavelength dispersive analysis of X-rays. Macroscopic property characterization involves measurement of porosity, density, and surface area. The article describes testing methods such as room and high-temperature strength test methods, proof testing, fracture toughness measurement, and hardness and wear testing. It also explains methods for determining thermal expansion, thermal conductivity, heat capacity, and emissivity of ceramics and glass and measurement of these properties as a function of temperature.

This article focuses on the modes of operation, physical basis, sample requirements, properties characterized, advantages, and limitations of common characterization methods that are used to evaluate the physical morphology and chemical properties of component surfaces for medical devices. The methods include light microscopy, scanning electron microscopy, atomic force microscopy, energy-dispersive x-ray spectroscopy, Auger electron spectroscopy, secondary ion mass spectrometry, x-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy.

Metallographic examination is one of the most important procedures used by metallurgists in failure analysis. Typically, the light microscope (LM) is used to assess the nature of the material microstructure and its influence on the failure mechanism. Microstructural examination can be performed with the scanning electron microscope (SEM) over the same magnification range as the LM, but examination with the latter is more efficient. This article describes the major operations in the preparation of metallographic specimens, namely sectioning, mounting, grinding, polishing, and etching. The influence of microstructures on the failure of a material is discussed and examples of such work are given to illustrate the value of light microscopy. In addition, information on heat-treatment-related failures, fabrication-/machining-related failures, and service failures is provided, with examples created using light microscopy.

This article is intended to provide the reader with a good understanding of the underlying science, technology, and the most common applications of focused ion beam (FIB) instruments. It begins with a survey of the various types of FIB instruments and their configurations, discusses the essential components, and explains their function only to the extent that it helps the operator obtain the desired results. An explanation of how the components of ion optical column shape and steer the ion beam to the desired target locations is then provided. The article also reviews the many diverse accessories and options that enable the instrument to realize its full potential across all of the varied applications. This is followed by a detailed analysis of the physical processes associated with the ion beam interacting with the sample. Finally, a complete survey of the most prominent FIB applications is presented.