This article covers the three most popular techniques used to characterize the very outermost layers of solid surfaces: Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Some of the more important attributes are listed for preliminary insight into the strengths and limitations of these techniques for chemical characterization of surfaces. The article describes the basic theory behind each of the different techniques, the types of data produced from each, and some typical applications. Also discussed are the different types of samples that can be analyzed and the special sample-handling procedures that must be implemented when preparing to do failure analysis using these surface-sensitive techniques. Data obtained from different material defects are presented for each of the techniques. The examples presented highlight the typical data sets and strengths of each technique.

This article discusses several purposes and types of materials characterization techniques. Some of the factors to be considered when selecting appropriate characterization methods are described. The article also presents the scope and organization of this volume.

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.

The characterization, testing, and nondestructive evaluation of ceramics and glasses are vital to manufacturing control, property improvement, failure prevention, and quality assurance. This article provides a broad overview of characterization methods and their relationship to property control, both in the production and use of ceramics and glasses. Important aspects covered include the means for characterizing ceramics and glasses, the corresponding rationale behind them, and relationship of chemistry, phases, and microconstituents to engineering properties. The article also describes the effects that the structure of raw ceramic materials and green products and processing parameters have on the ultimate structure and properties of the processed piece. The effects that trace chemistry and processing parameters have on glass properties are discussed. The article describes mechanical tests and failure analysis techniques used for ceramics.

This article introduces various analytical techniques commonly used in the characterization of organic solids and liquids and discusses the challenges in performing the analysis, with examples. Some general advice in approaching a material analysis is also provided.

This article uses metal and alloy powders as examples to briefly discuss how to perform the characterization of powders. It begins by reviewing some of the techniques involved in the sampling of powders to ensure accurate characterization. This is followed by a discussion on the important properties to characterize powders, namely the particle size, surface area, density, porosity, particle hardness, compressibility, green strength, and flowability. For characterization of powders, both individual particles and bulk powders are used to evaluate their physical and chemical properties. The article also discusses the important characteristics and compositions of powder as well as impurities that directly affect powder properties. It ends with a description of the ignition and dust-explosion characteristics of organic and metal powders.

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.

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.

This article is a detailed account of optical emission spectroscopy (OES) for elemental analysis. It begins with a discussion on the historical background of OES and development trends in OES methods. This is followed by a description of the general principles and optical systems of OES, along with various types of emission sources commonly used for OES. Some of the processes involved in calibration and quantification of OES for direct solids analysis by the ratio method are then described. The article ends with a discussion on the applications of each type of emission sources.

This article focuses on some of the factors pertinent to atomic absorption spectroscopy (AAS). It begins by describing the working principle, critical components, and construction of flame atomic absorption instrumentation. This is followed by sections discussing various types of interferences in AAS, namely vaporization, ionization, matrix interferences, and background correction. Some of the methods for the analysis of microliter-sized samples and methods of standard additions to the sample solution for generating calibration standards are then reviewed. The article concludes with a section on processes involved in matrix matching.

This article provides a clear but nonexhaustive description of the general principle of atomic emission, with a particular focus on instrumentation, and summarizes the main characteristics of the inductively coupled plasma optical emission spectrometer technique. Basic atomic theory as well as the instrument characteristics and their influence on the instrument performances are presented. The advantages, drawbacks, and developments of this technique are discussed, and, finally, alternative techniques and examples of applications are provided.

Infrared (IR) spectra have been produced by transmission, that is, transmitting light through the sample, measuring the light intensity at the detector, and comparing it to the intensity obtained with no sample in the beam, all as a function of the infrared wavelength. This article discusses the sampling techniques and applications of IR spectra as well as the molecular structure information it can provide. The discussion begins with a description of the general principle of IR spectroscopy. This is followed by a section on commercial IR instruments. Sampling techniques and accessories necessary in obtaining the infrared spectrum of a material are then discussed. The article presents various techniques and methods involved in IR qualitative analysis and quantitative analysis. It ends with a few examples of the applications of IR spectroscopy.

This article introduces the principles of Raman spectroscopy and the representative materials characterization applications to which Raman spectroscopy has been applied. A discussion on light-scattering fundamentals and a description of the experimental aspects of the technique are included. Emphasis is placed on the different instrument approaches that have been developed for performing Raman analyses on various materials. The applications presented reflect the breadth of materials characterization uses for Raman spectroscopy and highlight the analysis of bulk material and of surface and near-surface species.

This article focuses on the application of solid-state nuclear magnetic resonance (NMR) spectroscopy in materials science, especially for inorganic and organic polymer solids. It begins with a discussion on the general principles of NMR, providing information on nuclear spin descriptions and line narrowing and spectral resolution and describing the impact of magnetic field on nuclear spins and the factors determining resonance frequency. This is followed by a description of various systems and equipment necessary for NMR spectroscopy. A discussion on general sampling for solid-state NMR, sample-spinning requirements, and extraneous signals is then included. Various factors pertinent to accurate calibration of the NMR spectrum are also described. The article provides information on some of the parameters both beneficial and problematic for processing NMR data. It ends with a description of the applications of NMR in glass science and ceramics.

This article endeavors to familiarize the reader with a selection of different ionization designs and instrument components to provide knowledge for sorting the various analytical strategies in the field of solid analysis by mass spectrometry (MS). It begins with a description of the general principles of MS. This is followed by sections providing a basic understanding of instrumentation and discussing the operating requirements as well as practical considerations related to solid sample analysis by MS. Instrumentation discussed include the triple quadrupole mass spectrometer and the time-of-flight mass spectrometer. Inductively coupled plasma and thermal ionization MS provide atomic information, and direct analysis in real-time and matrix-assisted laser-desorption ionization MS are used to analyze molecular compositions. The article describes various factors pertinent to ionization methods, namely glow discharge mass spectrometry and secondary ion mass spectrometry. It concludes with a section on various examples of applications and interpretation of MS for various materials.

Gas analysis by mass spectrometry, or gas mass spectrometry, is a general technique using a family of instrumentation that creates a charged ion from a gas phase chemical species and measures the mass-to-charge ratio. This article covers gas analysis applications that do not use chromatographic separation to physically isolate components of the sample prior to analysis. It is intended to provide an understanding of gas analysis instrumentation and terminology that will help make informed decisions in choosing an instrument and methodology appropriate for the data needed. Mass-analyzer technologies for gas mass spectrometry, namely quadrupole mass filters, magnetic sector mass filters, and time-of-flight mass analyzers are covered. Common factors to consider in choosing an analyzer for static or continuous gas measurement are also described. In addition, the article presents some examples of applications of gas mass spectrometry.

This article provides a brief account of glow discharge mass spectrometry (GDMS) for direct determination of trace elements in solid samples and for fast depth profiling in a great variety of innovative materials. It begins by describing the general principles of GDMS. This is followed by a discussion on the various components of a GDMS system as well as commercial GDMS instruments. A description of processes involved in specimen preparation and cleaning in GDMS is then presented. Various problems pertinent to multielemental calibrations in GDMS are discussed along with measures to overcome them. The article further provides information on the processes involved in the analytical setup of parameters in GDMS, covering the steps involved in the analysis of GDMS data. It ends with a section on the application and interpretation of GDMS in the metals industry.

This article discusses the basic principles of inductively coupled plasma mass spectrometry (ICP-MS), covering different instruments used for performing ICP-MS analysis. The instruments covered include the sample-introduction system, ICP ion source, mass analyzer, and ion detector. Emphasis is placed on ICP-MS applications in the semiconductor, photovoltaic, materials science, and other electronics and high-technology areas.

This article provides a detailed account of the basic concepts of Rutherford backscattering spectrometry (RBS). It begins with a description of the principles of RBS, as well as the effect of channeling in conjunction with backscattering measurements and the effect of energy loss under this condition. This is followed by a section on equipment used in RBS analysis. Channel-energy conversion, energy-depth conversion, and separation of the dechanneling background are then discussed as the main steps of RBS data analysis. The article also discusses the applications of RBS—including composition of bulk samples, thin-film composition and layer thickness, impurity profiles, damage depth profile, and surface peak—as well as the various codes developed to simulate it.

This article is a brief account of low-energy ion-scattering spectroscopy (LEIS) for determining the atomic structure of solid surfaces. It begins with a description of the general principles of LEIS. This is followed by a section providing information on the equipment used for LEIS. Various steps involved in the sample preparation, calibration, and data analysis are then discussed. The article concludes with a section on the applications and interpretation of LEIS in material analysis, including discussion on surface structural analysis, layer-by-layer (Frank-van der Merwe) growth, and low-energy atom-scattering spectroscopy.