This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.

X-ray diffraction (XRD) residual-stress analysis is an essential tool for failure analysis. This article focuses primarily on what the analyst should know about applying XRD residual-stress measurement techniques to failure analysis. Discussions are extended to the description of ways in which XRD can be applied to the characterization of residual stresses in a component or assembly and to the subsequent evaluation of corrective actions that alter the residual-stress state of a component for the purposes of preventing, minimizing, or eradicating the contribution of residual stress to premature failures. The article presents a practical approach to sample selection and specimen preparation, measurement location selection, and measurement depth selection; measurement validation is outlined as well. A number of case studies and examples are cited. The article also briefly summarizes the theory of XRD analysis and describes advances in equipment capability.

This article describes the methods of X-ray diffraction analysis, the types of information that can be obtained, and its interpretation. The discussion covers the basic theories of X-rays and various types of diffraction experiments, namely single-crystal methods for polychromatic and monochromatic beams, powder diffraction methods, and the Rietveld method.

X-ray powder diffraction (XRPD) techniques are used to characterize samples in the form of loose powders, aggregates of finely divided material or polycrystalline specimens. This article provides a detailed account of XRPD. It begins with a discussion on XRPD instrumentation and the techniques used to characterize samples. The article then describes the principles, advantages, and disadvantages of various types of powder diffractometers. A section on the Rietveld method of diffraction analysis is then presented. The article discusses various methods and procedures for qualifying and quantifying phase mixtures in powder samples. It provides information on typical sensitivity and experimental limits on precision of XRPD analysis and other systematic sources of errors that affect accuracy. Some of the factors pertinent to the estimation of crystallite size and defects are also presented. The article ends with a few application examples of XRPD.

This article provides a detailed account of the concepts of single-crystal x-ray diffraction (XRD). It begins with a historical review of XRD methods, followed by a description of the various factors involved in crystal symmetry. The article then focuses on the phase problem in x-ray structural analysis and validation of the structural model. Some of the factors to be considered for performing experimental procedure are provided. The article presents several examples of applications of single-crystal XRD. The following sections cover the crystallographic problem in terms of structural analysis, software programs for crystal structure solution and refinement, and visualization of crystal structures. The article ends with a discussion on various databases available for single-crystal XRD analysis.

This article discusses various concepts of micro x-ray diffraction (XRD) used for the examination of materials in situ. The discussion covers the principles, equipment used, sample preparation procedure, considerations for calibrating a detector, steps for performing data analysis, and applications and interpretation of micro-XRD.

This article provides a detailed account of x-ray diffraction (XRD) residual-stress techniques. It begins by describing the principles of XRD stress measurement, followed by a discussion on the most common methods of XRD residual-stress measurement. Some of the procedures required for XRD residual-stress measurement are then presented. The article provides information on measurement of subsurface stress gradients and stress relaxation caused by layer removal. The article concludes with a section on examples of applications of XRD residual-stress measurement that are typical of industrial metallurgical, process development, and failure analysis investigations undertaken at Lambda Research.

This article discusses the techniques and applications of synchrotron x-ray diffraction, providing information on x-ray generation, monochromation, and crystallography. X-ray diffraction techniques covered include single-crystal and powder diffraction. Some of the factors involved in the construction and development of macromolecular x-ray crystallography are also described.

This article discusses the capabilities and limitations of various material characterization methods that assist in the selection of a proper analytical tool for analyzing particulate materials. Commonly used methods are microanalysis, surface analysis, and bulk analysis. The techniques used for performing microanalysis include scanning electron microscopy and electron probe X-ray microanalysis. The article describes surface analysis techniques, including Auger electron spectroscopy, X-ray photoelectron spectroscopy, and ion-scattering spectroscopy. Bulk analysis techniques, such as X-ray powder diffraction, inductively coupled plasma atomic emission spectroscopy, atomic absorption spectroscopy, and atomic fluorescence spectrometry, are also discussed.

The raw materials used in thermal spray processes are a critical parameter in the finished coating because the variations in their size, morphology, chemistry, and phase composition can significantly impact coating properties. Therefore, it is important to test and characterize the raw materials. This article discusses various characterization methods for powders. Topics discussed include: methods for determining particle size and/or size distribution; powder and coating stoichiometry; particle chemistry; and phase analysis by x-ray diffraction. This article discusses the characterization of thermal spray powders which involves the determination of particle size and/or size distribution and phase analysis by x-ray diffraction. It provides information on preferential volatilization and rapid solidification that influence compositional differences. Wet chemical methods, spectographic analysis, and atomic absorption spectrometry are also discussed.

This article discusses the central aspect of anisotropy modeling, namely, texture measurement and analysis. It provides an overview of the methods available for characterizing crystallographic preferred orientation, or texture, in polycrystalline materials. These methods include pole figure measurement and electron backscatter diffraction (EBSD). The article describes the process considerations for pole figure measurement, including X-ray diffraction, neutron diffraction, stereographic projection, equal area projection, graphing pole figures, typical textures, and orientation distribution. It also deals with the limitations and challenges associated with the EBSD, and applications of the diffraction.

This article focuses primarily on what an analyst should know about applying X-ray diffraction (XRD) residual stress measurement techniques to failure analysis. Discussions are extended to the description of ways in which XRD can be applied to the characterization of residual stresses in a component or assembly. The article describes the steps required to calibrate instrumentation and to validate stress measurement results. It presents a practical approach to sample selection and specimen preparation, measurement location selection, and measurement depth selection, as well as an outline on measurement validation. The article also provides information on stress-corrosion cracking and corrosion fatigue. The importance of residual stress in fatigue is described with examples. The article explains the effects of heat treatment and manufacturing processes on residual stress. It concludes with a section on the XRD stress measurements in multiphase materials and composites and in locations of stress concentration.

This article outlines the basic steps to be followed and the range of techniques available for failure analysis, namely, background data assembling, visual examination, microfractography, chemical analysis, metallographic examination, electron microscopy, electron microprobe analysis, X-ray techniques, and simulations. It also describes the steps for analyzing the data, preparing the report, preservation of evidence, and follow-up on recommendations.

This article focuses on the visual or macroscopic examination of damaged materials and interpretation of damage and fracture features. Analytical tools available for evaluations of corrosion and wear damage features include energy dispersive spectroscopy, electron probe microanalysis, Auger electron spectroscopy, secondary ion mass spectroscopy, and X-ray powder diffraction. The article discusses the analysis and interpretation of base material composition and microstructures. Preparation and examination of metallographic specimens in failure analysis are also discussed. The article concludes with a review of the evaluation of polymers and ceramic materials in failure analysis.

This article discusses the need of and the strain basis for residual stress measurements and describes the nature of residual stress fields. A generic destructive stress relief procedure is described along with the issues generally involved in each procedural step. The article presents the stress reconstruction equations to be used for computational reconstruction of the stress fields from the measured strains for the destructive methods. It provides information on the sectioning, material removal, strain measurement, and chemical methods of residual stress measurement. The article reviews the semidestructive methods of residual stress measurement: blind hole drilling and ring coring, spot annealing, and X-ray diffraction techniques. Nondestructive methods such as neutron diffraction, ultrasonic velocity, and magnetic Barkhausen noise techniques, are also discussed.

This article discusses the standard test methods that can be applied to many types of welds: tension, bending, impact, and toughness testing. It provides information on four qualification stages, namely, the weld material qualification, base material qualification, the weld procedure qualification, and the weld service assessment. The article describes two general types of measurements for residual stress in welds: locally destructive techniques and nondestructive techniques. Locally destructive techniques include hole drilling, chip machining, and block sectioning. Nondestructive techniques include X-ray diffraction, neutron diffraction, Barkhausen noise analysis, and ultrasonic propagation analysis. The article concludes with an overview of weldability testing.

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 describes the test techniques that are available for monitoring crack initiation and crack growth and for obtaining information on fatigue damage in test specimens. These techniques include optical methods, the compliance method, electric potential measurement, and gel electrode imaging methods. The article discusses the magnetic techniques that are primarily used as inspection techniques for detecting fatigue cracks in structural components. It details the principles and operation procedures of the liquid penetrant methods, positron annihilation techniques, acoustic emission techniques, ultrasonic methods, eddy current techniques, infrared techniques, exoelectron methods, and gamma radiography. The article explains the microscopy methods used to determine fatigue crack initiation and propagation. These include electron microscopy, scanning tunneling microscopy, atomic force microscopy, and scanning acoustic microscopy. The article also reviews the X-ray diffraction technique used for determining the compositional changes, strain changes, and residual stress evaluation during the fatigue process.

This article describes the structure of coatings produced by plasma spraying, vapor deposition, and electrodeposition processes. The main techniques used for microstructure assessment are introduced. The relationship between the microstructure and property is also discussed. The experimental techniques for microstructural characterization include metallographic technique, X-ray diffraction, electron, microscopies, and porosimetry.