Archaeometallurgists use metallography to reveal and interpret the microstructures of objects, in conjunction with the results of their chemical analyses and microanalyses. This article describes a number of special problems that occur while performing metallographic analyses on archaeological materials. It also presents case studies, with examples that illustrate situations where metallography has contributed to archaeometallurgical studies.

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 provides a summary of the concepts discussed in the articles under the Section “Failure Analysis” in ASM Handbook, Volume 21: Composites. Most of the information in this Section is geared toward organic-matrix composites, although there is some information on failure analysis and fractography of ceramic- and metal-matrix composites.

X-ray diffraction (XRD) is the most extensively used method for identifying and characterizing various aspects of metals related to the arrangements and spacings of their atoms for bulk structural analysis. XRD techniques are also applicable to ceramics, geologic materials, and most inorganic chemical compounds. This article describes the operating principles and types of XRD analyses, along with information about the threshold sensitivity and precision, limitations, sample requirements, and capabilities of related techniques. The necessary instrumentation for XRD analyses include the Debye-Scherrer camera and the X-ray diffractometer. The article also describes the uses of XRD analyses, such as the identification of phases or compounds in metals and ceramics; detection of order and disorder transformation; determination of lattice parameters and changes in lattice parameters due to alloying and temperature effects; measurement of residual stresses; characterization of crystallite size and perfection; characterization of preferred orientations; and determination of single crystal orientations.

This article discusses the basic principles of and chemical effects in Auger electron spectroscopy (AES), covering various factors affecting the quantitative analyses of AES. The discussion covers instrumentation and sophisticated electronics typically used in AES for data acquisition and manipulation and various limitations of AES. Various examples highlighting the capabilities of the technique are also included.

This article discusses the production process, testing methods, quality control, and common defects found in heavy-section ductile iron (DI) castings, along with analyses of industrial examples. The common defects include shrinkage defects, graphite-particle-related defects, and chunk graphite defects. The recommended chemical compositions for certain section thicknesses in ductile iron grades are presented in a table. The article illustrates the relationship between microstructure and mechanical properties of DI by using either industrial examples or castings produced under laboratory conditions.

This article provides a background to the biological evaluation of medical devices. It discusses what the ISO 10993 standards require for polymeric biomaterials and presents examples of qualitative and quantitative tests that can be used to satisfy these requirements. The article describes infrared (IR) and thermal analyses that are used extensively to fingerprint polymeric materials. It also presents a discussion on the chemical characterization and risk assessment of extracts. Background information on risk assessments of extracts is also included. The four basic steps that are commonly used in the risk assessment process are discussed. These include hazard identification, dose-response assessment, and exposure assessment, and risk characterization.

The overall chemical composition of metals and alloys is most commonly determined by X-ray fluorescence (XRF) and optical emission spectroscopy (OES), and combustion and inert gas fusion analysis. This article provides information on the capabilities, uses, detection threshold and precision methods, and sample requirements. The amount of material that needs to be sampled, operating principles, and limitations of the stated methods are also discussed.

Identification of alloys using quantitative chemical analysis is an essential step during a metallurgical failure analysis process. There are several methods available for quantitative analysis of metal alloys, and the analyst should carefully approach selection of the method used. The choice of appropriate analytical techniques is determined by the specific chemical information required, the condition of the sample, and any limitations imposed by interested parties. This article discusses some of the commonly used quantitative chemical analysis techniques for metals. The discussion covers the operating principles, applications, advantages, and disadvantages of optical emission spectroscopy (OES), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray spectroscopy, and ion chromatography (IC). In addition, information on combustion analysis and inert gas fusion analysis is provided.

This article describes some of the common elemental composition analysis methods and explains the concept of referee and economy test methods in failure analysis. It discusses different types of microchemical analyses, including backscattered electron imaging, energy-dispersive spectrometry, and wavelength-dispersive spectrometry. The article concludes with information on specimen handling.

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.

Field ion microscopy (FIM) can be used to study the three-dimensional structure of materials, such as metals and semiconductors, because successive atom layers can be ionized and removed from the surface by field evaporation. The ions removed from the surface by field evaporation can be analyzed chemically by coupling to the microscope a time-of-flight mass spectrometer of single-particle sensitivity, known as the atom probe (AP). This article describes the principles, sample preparation, and quantitative analysis of FIM. It also provides information on the principles, instrument design and operation, mass spectra and their interpretation, and applications of AP microanalysis.

The electronic microcircuit industry has placed severe demands on metal suppliers to provide metals of the highest reproducible purity attainable as a result of the constant quest for the true values of physical and chemical properties of metals. This article describes the commonly used methods for ultrapurification of metals produced by electrolytic processes, including fractional crystallization, zone refining, vacuum melting, distillation, chemical vapor deposition, and solid state refining techniques. In addition, it describes the trace element analysis and resistance-ratio test methods used to characterize purity. Tables list the values for resistance ratios of zone-refined metals and their corresponding chemical compositions, and provide an example of the detection of impurities to concentrations in the parts per billion range, utilizing a combination of the glow discharge mass spectroscopy method and Leco combustion methods.

As a failure investigation progresses, the time arrives when the data and results of the various testing and analyses are compiled, compared, and interpreted. Data interpretation should be relatively straightforward for results that align well. However, interpretation can be challenging when results from various tests seem contradictory or inconclusive. Regardless, conclusions must eventually be drawn from the data. This article discusses the processes involved in reviewing data, formulating conclusions, failure analysis report preparation and writing, and providing recommendations and follow-up with appropriate personnel to prevent future failures.

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 is a compilation of property data for standard grades of cast copper alloys. Data are provided for mechanical, physical, thermal, electrical, chemical, nuclear, optical, and magnetic properties. The list for each alloy includes its common name, chemical composition, applications, mass characteristics, and fabrication characteristics.

Atomic absorption spectrometry (AAS) is generally used for measuring relatively low concentrations of approximately 70 metallic or semimetallic elements in solution samples. This article describes several features that are common to three techniques, namely, AAS, atomic emission spectrometry (AES), and atomic fluorescence spectrometry (AFS). It discusses the reasons for the extreme differences in AAS sensitivities that affect AFS and AES. The article provides information on the advantages and disadvantages of the Smith/Hieftje system and two types of background correction systems, namely, the continuum-source background correction and Zeeman background correction. It also provides a list of applications of conventional AAS equipment, which includes most of the types of samples brought to laboratories for elemental analyses.

This article provides information on the development of finite element analysis (FEA) and describes the general-purpose applications of FEA software programs in structural and thermal, static and transient, and linear and nonlinear analyses. It discusses special-purpose finite element applications in piping and pressure vessel analysis, impact analysis, and microelectronics. The article describes the steps involved in the design process using the FEA. It concludes with two case histories that involve the use of FEA in failure analysis.

The inclusion of damage tolerance design and a systematic review of design procedures allow the U.S. Air Force to design, manufacture, and maintain systems that are structurally safe and economically prudent. After a brief introduction of fracture mechanics, this article describes the particular aspects that relate to damage tolerance in aircraft design. It discusses the use of fracture mechanics as a method of predicting failure, understanding failure mechanisms, and suggesting inspection methods to protect against failure in pressure vessels. Various programs of U.S. Air Force to design aircraft structure, namely, airframe structural integrity programs, engine structural integrity program, and mechanical subsystems structural integrity program are also discussed.