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.

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.

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.

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 is a detailed account of the principles of electron-excited X-ray microanalysis. It begins by discussing the physical basis of electron-excited X-ray microanalysis and the advantages and limitations of energy dispersive spectrometry (EDS) and wavelength dispersive spectrometry for electron probe microanalysis. Key concepts for performing qualitative analysis and quantitative analysis by electron-excited X-ray spectrometry are then presented. Several sources that lead to measurement uncertainties in the k-ratio/matrix corrections protocol are provided, along with the significance of the raw analytical total. Sections on accuracy of the standards-based k-ratio/matrix corrections protocol with EDS and processes of analysis when severe peak overlap occurs are also included. The article provides information on low-atomic-number elements, iterative qualitative-quantitative analysis for complex compositions, and significance of standardless analysis in the EDS software. It ends with a section on the processes involved in elemental mapping for major and minor constituents.

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.

The electron backscatter diffraction (EBSD) technique has proven to be very useful in the measurement of crystallographic textures, orientation relationships between phases, and both plastic and elastic strains. This article focuses on backscatter diffraction in a scanning electron microscope and describes transmission Kikuchi diffraction. It begins with a discussion on the origins of EBSD and the collection of EBSD patterns. This is followed by sections providing information on EBSD spatial resolution and system operation of EBSD. Various factors pertinent to perform an EBSD experiment are then covered. The article further describes the processes involved in sample preparation that are critical to the success or usefulness of an EBSD experiment. It also discusses the applications of EBSD to bulk samples and the development of EBSD indexing methods.

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 describes the operation and capabilities of surface analysis methods of metals, including scanning electron microscopy, electron probe microanalysis, transmission electron microscopy, secondary ion mass spectroscopy, and X-ray photoelectron spectroscopy. It provides information on the capabilities, typical uses, spatial resolution, elemental analysis detection threshold and precision, limitations, sample requirements, and operating principles of the scanning auger microprobe.

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.

Microstructural analysis is the combined characterization of the morphology, elemental composition, and crystallography of microstructural features through the use of a microscope. This article reviews three types of the most commonly used electron microscopies in metallurgical studies, namely scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy. It briefly describes the operating principles, instrumentation which includes energy dispersive X-ray detectors, spatial resolution, typical use of the techniques, elemental analysis detection threshold and precision, limitations, sample requirements, and the capabilities of related techniques.

This article is an overview of the division Surface Analysis of this volume. The division covers various developed surface-analysis techniques, such as scanning probe and atomic force microscopy. The division focuses on the analysis of surface layers that are less than 100 nm. A quick reference summary of surface-analysis methods is presented in this article.

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 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.

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 provides an overview of the characteristics of Rayleigh waves plus methods for generation and detection of waves, including using piezoelectric transducers or noncontact techniques such as lasers, electromagnetic acoustic transducers, or air-coupled ultrasonics. It reviews the methods for using Rayleigh waves for defect detection and materials characterization, alongside nonlinear ultrasonic inspection and surface acoustic wave (SAW) microscopy. The article concludes with information on the standards that use Rayleigh waves for nondestructive evaluation (NDE) of different structures.

Nondestructive testing (NDT), also known as nondestructive evaluation (NDE), includes various techniques to characterize materials without damage. This article focuses on the typical NDE techniques that may be considered when conducting a failure investigation. The article begins with discussion about the concept of the probability of detection (POD), on which the statistical reliability of crack detection is based. The coverage includes the various methods of surface inspection, including visual-examination tools, scanning technology in dimensional metrology, and the common methods of detecting surface discontinuities by magnetic-particle inspection, liquid penetrant inspection, and eddy-current testing. The major NDE methods for internal (volumetric) inspection in failure analysis also are described.

Computed tomography (CT) is an imaging technique that generates a three-dimensional (3-D) volumetric image of a test piece. This article illustrates the basic principles of CT and provides information on the types, applications, and capabilities of CT systems. A comparison of performance characteristics for film radiography, real-time radiography, and X-ray computed tomography is presented in a table. A functional block diagram of a typical computed tomography system is provided. The article discusses CT scanning geometry that is used to acquire the necessary transmission data. It also provides information on digital radiography, image processing and analysis, dual-energy imaging, and partial angle imaging, of a CT system.

This article introduces various techniques commonly used in the characterization of semiconductors, namely single-crystal, polycrystalline, amorphous, oxide, organic, and low-dimensional semiconductors and semiconductor devices. The discussion covers material classification, fabrication methods, sample preparation, bulk/elemental characterization methods, microstructural characterization methods, surface characterization methods, and electronic characterization methods.

Ceramics are used widely in a number of different clinical applications in the human body. This article provides a brief history of the bioceramics field and information on the classification of the different types of bioceramics. These include bioinert ceramics, bioactive ceramics, and bioresorbable ceramics. The article describes the third-generation bioceramics, classified by Hench and Polak, such as silicate-substituted hydroxyapatite and bone morphogenic protein-carrying calcium phosphate coatings. It reviews several examination methods that are used to test the biocompatibility of ceramics, namely, biosafety testing, biofunctionality testing, bioactivity testing, and bioresorbability testing.