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.

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.

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 discusses the principles and limitations of micromagnetic techniques, namely, magnetic Barkhausen noise (MBN) and magnetoacoustic emission (MAE). It also discusses various factors limiting the establishment of acceptance criteria for test components as they pertain to the successful application of MBN measurement and signal interpretation. The article provides an overview of basic magnetic phenomena and dynamics in ferromagnetic materials that underlie the origin of MBN emissions. It describes the changes in the domain structure of the ferromagnetic material under an applied external field. The relationship between uniaxial stress and angular-dependent strain is also discussed. The influence of stress on domain walls, and therefore, the generation of Barkhausen noise are described. The article also describes the directional and angular MBN measurements and provides information on detection, angular dependence, and advanced analysis methods of MBN emissions.

In high-iron-tonnage operations, the cupola remains the most efficient source of continuous high volumes of iron needed to satisfy high production foundries or the multiple casting machines of centrifugal pipe producers. This article explores successful improvement technologies in cupola equipment, including preheated air blast, recuperative hot blast systems, and duplex electric holders. It discusses the shell, intermittent or continuous tapping, tuyere and blower systems, refractory lining, water-cooled cupolas, emission-control systems, and storage and handling of the charge materials. The article provides a discussion on control tests for cupola, including the chill test and mechanical test. It concludes with information on specialized cupolas such as cokeless cupola and plasma-fired cupola.

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.

Additive manufacturing (AM) is the process of joining materials to make parts from three-dimensional (3D) model data, usually layer upon layer, as opposed to subtractive manufacturing and formative manufacturing methodologies. This article discusses various defects in AM components, such as porosity, inclusions, cracking, and residual stress, that can be avoided by using vendor recommended process parameters and approved materials. It describes the development of process-structure-property-performance modeling. The article explains the practical considerations in nondestructive evaluation for additively manufactured metallic parts. It also examines nondestructive testing (NDT) inspection and characterization methods for each of the manufacturing stages in their natural order. The article provides information on various inspection techniques for completed AM manufactured parts. The various electromagnetic and eddy current techniques that can be used to detect changes to nearsurface geometric anomalies or other defects are also discussed. These include ultrasonic techniques, radiographic techniques, and neutron imaging.

This article discusses the inspection/reference standards that are absolutely critical for proper application of ultrasonic inspection systems. Many of the standards and specifications for ultrasonic inspection require the use of standard reference blocks. The article lists the variables that should be considered when selecting standard reference blocks and describes the three types of standard blocks ordinarily used for calibration or reference: area-amplitude blocks, distance-amplitude blocks, and blocks of the type sanctioned by the International Institute of Welding. It reviews the determination of area-amplitude and distance-amplitude curves of a straight-beam pulse-echo ultrasonic inspection system. The article discusses the three principal conventional manual ultrasonic sizing techniques: 6 dB drop technique, maximum-amplitude technique, and 20 dB drop technique. It provides information on the dimension-measurement applications of ultrasonic inspection methods.

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.

Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.

The potential for introducing defects during processing becomes greater as the relative density of pressed and sintered powder metallurgy (PM) parts increases and more multilevel parts with complex geometric shapes are produced. This article discusses the potential defects in pressed and sintered PM parts: density variations, compaction and ejection cracks, microlaminations, poor degree of sintering, and voids from prior lubricant agglomerates. It describes the various methods applicable to green compacts: direct-current resistivity testing, radiographic techniques, computed tomography, and gamma-ray density determination. The article also discusses the methods for automated nondestructive testing of pressed and sintered PM parts: acoustic methods-resonance testing, eddy current testing, magnetic bridge comparator testing, ultrasonic techniques, radiographic techniques, gamma-ray density determination, and visual inspection.

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.

Mechanical testing is an evaluative tool used by the failure analyst to collect data regarding the macro- and micromechanical properties of the materials being examined. This article provides information on a few important considerations regarding mechanical testing that the failure analyst must keep in mind. These considerations include the test location and orientation, the use of raw material certifications, the certifications potentially not representing the hardware, and the determination of valid test results. The article introduces the concepts of various mechanical testing techniques and discusses the advantages and limitations of each technique when used in failure analysis. The focus is on various types of static load testing, hardness testing, and impact testing. The testing types covered include uniaxial tension testing, uniaxial compression testing, bend testing, hardness testing, macroindentation hardness, microindentation hardness, and the impact toughness test.

Adhesive-bonded joints are extensively used in aircraft components and assemblies where structural integrity is critical. This article addresses the problem of how to inspect bonded assemblies so that all discrepancies are identified. It describes several inspection techniques and presents drawbacks and limitations of these techniques. Generic flaw types and flaw-producing mechanisms are listed in a table. The article discusses metal-to-metal defects, adherend defects, honeycomb sandwich defects, repair defects, and in-service defects. It reviews the methods applicable to the inspection of bonded structures, including visual inspection, ultrasonic inspection, X-ray radiography, and neutron radiography. The evaluation and correlation of inspection results are also discussed. The article concludes with information on the effects of ultrasonic wave interference in the ultrasonic inspection of adhesive-bonded joints.

Both nondestructive testing (NDT) and nondestructive evaluation (NDE) use noninvasive measurement techniques to gain information about defects and various properties of materials, components, and structures. This article begins with a discussion on the historical development of quantitative measurement techniques, evaluation reliability, and quantitative interpretation of nondestructive inspection methods. The common nondestructive evaluation methods, along with their uses and limitations, are summarized in a table. The article conceptually illustrates the interplay of NDE and fracture mechanics in the damage tolerant approach. It concludes with information on pressure vessel applications that can be separated into three protocols used by military nuclear power, commercial nuclear power, and non-nuclear pressure vessels and/or fired boilers.

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.

This article considers the two primary methods used for ultrasonic inspection: pulse-echo and the transmission methods. Pulse-echo inspection can be accomplished with longitudinal, shear, surface (Rayleigh), or Lamb (plate) waves using a diverse range of transducers. The article discusses the principles of each of these inspection methods. It describes the applications and the basic data formats for single-element transducer-based systems, including A-scans, B-scans, and C-scans. The article provides information on electronic equipment used for ultrasonic inspection. It also describes how specific material conditions produce and modify A-scan indications. The article provides information on the controls and their functions for the display unit of the electronic equipment. It describes the techniques used for the identification and characterization of flaws, namely, surface (Rayleigh) wave and ultrasonic polar scan techniques.

Thermomechanical fatigue (TMF) is the general term given to the material damage accumulation process that occurs with simultaneous changes in temperature and mechanical loading. TMF may couple cyclic inelastic deformation accumulation, temperature-assisted diffusion within the material, temperature-assisted grain-boundary evolution, and temperature-driven surface oxidation, among other things. This article discusses some of the major aspects and challenges of dealing with TMF life prediction. It describes the damage mechanisms of TMF and covers various experimental techniques to promote TMF damage mechanisms and elucidate mechanism coupling interactions. In addition, life modeling in TMF conditions and a practical application of TMF life prediction are presented.

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.

Probability of detection (POD) assesses the performance of a non-destructive evaluation (NDE)-based inspection, which is a method used to determine the capability of an inspection as a function of defect type and defect size. This article provides an overview of the concept of POD, why it is needed, the history behind the development of POD, how POD assessments are performed, and how modeling and simulation can be integrated into the execution of a POD assessment. It describes the methods by which POD is determined. This includes detail on the experimental process to acquire the needed data, the mathematical methods to obtain a POD curve, and techniques to assess uncertainty in the POD curve as it is obtained from a limited data set. The concept of model-assisted POD (MAPOD) is introduced, with additional details and representative examples of MAPOD.