Several specialized instruments are available for the metallographer to use as tools to gather key information on the characteristics of the microstructure being analyzed. These include microscopes that use electrons as a source of illumination instead of light and x-ray diffraction equipment. This chapter describes how these instruments can be used to gather important information about a microstructure. The instruments covered include image analyzers, transmission electron microscopes, scanning electron microscopes, electron probe microanalyzers, scanning transmission electron microscopes, x-ray diffractometers, microhardness testers, and hot microhardness testers. A list of other instruments that are usually located in a research laboratory or specialized testing laboratory is also provided.

This chapter discusses the use of electron microscopy in metallographic analysis. It explains how electrons interact with metals and how these interactions can be harnessed to produce two- and three-dimensional images of metal surfaces and generate crystallographic and compositional data as well. It discusses the basic design and operating principles of scanning electron microscopes, transmission electron microscopes, and scanning transmission electron microscopes and how they are typically used. It describes the additional information contained in backscattered electrons and emitted x-rays and the methods used to access it, namely wavelength and energy dispersive spectroscopy and electron backscattering diffraction techniques. It also describes the role of focused ion beam milling in sample preparation and provides information on atom probes, atomic force microscopes, and laser scanning microscopes.

This article presents methods that enable one to consistently, uniformly and quickly remove substrate silicon from units without imparting damage to the structure of interest. It provides examples of electron beam probing and backside nano-probing techniques. The electron beam probing techniques are E-beam Logic State Imaging, Electron-beam Signal Image Mapping, and E-beam Device Perturbation. Backside nano-probing techniques discussed include: Electron Beam Absorbed Current, Electron Beam Induced Resistance Change, four terminal resistance measurements, resistive gate defect identification, and circuit editing. The article also presents methods to prepare electron beam probing samples where some remaining silicon is required for the transistor functions and transmission electron microscope samples from units where the substrate silicon has been partially or completely removed.

This article provides an overview of the most common micro-analytical technique in the failure analysis laboratory: energy dispersive X-ray spectroscopy (EDS). It discusses the general characteristics, advantages, and disadvantages of some of the X-ray detectors attached to the scanning electron microscope chamber including the lithium-drifted EDS detector, silicon drift detector (SDD), and wavelength dispersive X-ray detector. The article then provides information on qualitative and quantitative X-ray analysis programs followed by a discussion on EDS elemental mapping. The discussion includes a comparison of scanning transmission electron microscope-EDS elemental mapping and mapping with an SDD. A brief section is devoted to the discussion on the artifacts that occur during X-ray mapping.

There are several analytical methods available that can be used in-line on whole wafers as well as off-line on de-processed products that are returned from the field. These techniques are surface analytical techniques that can be used to characterize the bulk of the material. The main six methods used in semiconductor industry are: Auger spectroscopy, dynamic secondary ion mass spectroscopy, time of flight static secondary ion mass spectroscopy (ToF-SIMS), X-ray photoelectron spectroscopy, scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX), and transmission electron microscope-EDX. This review specifically addresses ToF-SIMS and describes some typical examples of the application of Auger and SEM-EDX.

This article provides an overview of how to use the scanning electron microscope (SEM) for imaging integrated circuits. The discussion covers the principles of operation and practical techniques of the SEM. The techniques include sample mounting, sample preparation, sputter coating, sample tilt and image composition, focus and astigmatism correction, dynamic focus and image correction, raster alignment, and adjusting brightness and contrast. The article also provides information on achieving ultra-high resolution in the SEM. It concludes with information on the general characteristics and applications of environmental SEM.

This chapter discusses the setup and use of a transmission electron detector in a typical scanning electron microscope (SEM). It describes the arrangement and function of the primary components in the detector, following the signal path from the sample to a micromirror array where it is directed by the user to either a CMOS sensor (to record diffraction patterns) or a photomultiplier tube (to observe real-space images). The chapter discusses some of the nuances of digital imaging and diffraction and includes examples in which transmission electron detectors are used to analyze gold films, carbon nanotubes, zeolite sheets, and monolayer graphene. It also describes emerging techniques, including four-dimensional STEM, thermal diffuse scattering, energy filtering, aberration correction, and atomic resolution imaging.

This chapter discusses the principles of scanning transmission electron microscopy (STEM) as implemented using conventional scanning electron microscopes (SEMs). It describes the pros and cons of low-energy imaging and diffraction, addresses basic hardware requirements, and provides information on imaging modes, detector positioning and alignment, and the effect of contrast reversal. It also discusses beam convergence and angular selectivity, the use of application-specific masks, and how to generate grain orientation maps for different material systems.

After several failed attempts to lower their starboard wheels for landing, pilots engaged the help of gravity through g-force maneuvers and managed to coax the wheels into place. An inspection following the incident revealed a broken universal joint in one of the linkages that opens and closes the doors to the undercarriage compartment. The failed component was removed from the aircraft and examined using optical and electron microscopes. Under low magnification, the fracture surface appeared jagged except for one corner that was relatively smooth. SEM fractography revealed the presence of fatigue striations in the smooth region and dimpling elsewhere. Based on their findings, investigators concluded that fatigue loading initiated a crack in the universal joint that progressed with time and that the final fracture occurred due to bending tensile overload.

The quill shaft in an aircraft engine was found in two pieces following a flameout. One piece was short, straight, and otherwise undamaged; the other piece was bent in several places as was the sleeve that covered it. The facture surface, as viewed under optical and scanning electron microscopes, was flat and shiny with deformation marks and dimples, typical of torsional overload, and signs of severe rubbing on the periphery. Based on their observations, investigators concluded that the quill shaft failed by torsional overload, the source of which could not be determined.

During a routine preflight inspection of a piston aircraft engine, part of a cooling fin was found that had broken off the cylinder. The piece, made of aluminum-silicon alloy, was cleaned and examined. Based on the fracture characteristics revealed by an electron microscope, it was concluded that the fin failed in a brittle manner by overload.

A pair of bolts on a connecting rod failed during a test run for a prototype engine. They were replaced by bolts made from a stronger material that also failed, one due to fatigue, the other by tensile overload. The fracture surfaces on all four bolts were examined using optical and electron microscopes, indicating that the operating loads on the bolts far exceeded the design loads. Based on their observations, which are summarized in the report, failure analysts concluded that the design of the connecting rod system needs to be reassessed.

This article briefly reviews abrasive and adhesive wear failure of reinforced polymers and polymer composites, namely particulate-filled polymers, short-fiber-reinforced polymers, polymers with continuous fibers, and mixed reinforcements and fabrics. It includes scanning electron microscope micrographs of abraded surfaces of composites against 80-grade SiC paper and under 14 N load, and worn surfaces of abraded polyether-imide composites and polyamide 66 unidirectional composites and 66 hybrid composites.

This article addresses the ancillary issues regarding the nanoprobing and characterization of transistors, probing copper metallization layers, and the various imaging techniques. The discussion includes several characterization examples of known transistor failure types, namely four probe transistor characterization, two probe transistor characterization, and probing and characterizing metallization issues. The imaging techniques discussed are those that are specific to atomic force nanoprober or scanning electron microscope based tools. They are current contrast imaging, scanning capacitance imaging, e-beam absorbed current imaging, e-beam induced current imaging, e-beam induced resistance change imaging, and active voltage contrast imaging.

The mechanical properties of steel are strongly influenced by the underlying microstructure, which is readily observed using optical microscopy. This chapter describes common room-temperature steel microstructures and how they are achieved via heat treatment. It discusses the production of hypo- and hypereutectoid steels and the effect of cooling rate on microstructure. It also examines quenched steels and the phase transformations associated with rapid cooling. It describes the development of lath and plate martensite, retained austenite, and bainite and how to identify the various phases. The chapter concludes with a brief review of spheroidized microstructures.

This chapter provides perspective on the physical dimensions associated with the microstructure of steel and the instruments that reveal grain size, morphology, phase distributions, crystal defects, and chemical composition, from which properties and behaviors derive. The chapter also reviews the definitions and classifications used to identify and differentiate commercial steels, including the AISI/SAE and UNS designation systems.

This article covers common techniques for surface characterization, including the modern scanning electron microscopy and methods for the chemical characterization of surfaces by Auger electron spectroscopy, X-ray photoelectron spectroscopy, and time-of-flight secondary ion mass spectrometry. The principles of surface analysis and some of the applications of the technique in polymer failure studies are also provided.

The ultimate goal of the failure analysis process is to find physical evidence that can identify the root cause of the failure. Transmission electron microscopy (TEM) has emerged as a powerful tool to characterize subtle defects. This article discusses the sample preparation procedures based on focused ion beam milling used for TEM sample preparation. It describes the principles behind commonly used imaging modes in semiconductor failure analysis and how these operation modes can be utilized to selectively maximize signal from specific beam-specimen interactions to generate useful information about the defect. Various elemental analysis techniques, namely energy dispersive spectroscopy, electron energy loss spectroscopy, and energy-filtered TEM, are described using examples encountered in failure analysis. The origin of different image contrast mechanisms, their interpretation, and analytical techniques for composition analysis are discussed. The article also provides information on the use of off-axis electron holography technique in failure analysis.

Ductile fracture results from the application of an excessive stress to a metal that has the ability to deform permanently, or plastically, prior to fracture. Careful examination and knowledge of the metal, its thermal history, and its hardness are important in determining the correct nature of the fracture features. This chapter is a detailed account of the general characteristics and microstructural aspects of ductile fracture with suitable illustrations. It describes some of the complicating factors extraneous to the fracture itself.

This chapter provides an overview of the tools and techniques used to examine failure specimens and the wealth of information that can be obtained from fracture surfaces, cracks, wear patterns, and other such features. It discusses the use of metallography, fractography, and optical and electron microscopy. It presents a number of images recorded using these methods and explains what they reveal about the mode of fracture and the state of the component prior to failure.