X-ray spectroscopy is generally accepted as the most useful ancillary technique that can be added to any scanning electron microscope (SEM), even to the point of being considered a necessity by most operators. While “stand-alone” x-ray detection systems are used less frequently in failure analysis than the more exact instrumentation employed in SEMs, the technology is advancing and is worthy of note due to its capability for nondestructive analysis and application in the field. This article begins with information on the basis of the x-ray signal. This is followed by information on the operating principles and applications of detectors for x-ray spectroscopy, namely energy-dispersive spectrometers, wavelength-dispersive spectrometers, and handheld x-ray fluorescence systems. The processes involved in x-ray analysis in the SEM and handheld x-ray fluorescence analysis are then covered. The article ends with a discussion on the applications of x-ray spectroscopy in failure analysis.

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.

An Incoloy 800H (UNS N08810) transfer line on the outlet of an ethane-cracking furnace failed during decoking of the furnace tubes after nine years in service. A metallographic examination using optical and scanning electron microscopy as well as energy-dispersive x-ray spectroscopy revealed that the failure was due to sulfidation. The source of the sulfur in the furnace effluent was either dimethyl disulfide, injected into the furnace feed to prevent coke formation and carburization of the furnace tubes, or contamination of the feed with sulfur bearing oil.

Suspension lugs fabricated from AISI 4340 steel used to facilitate loading of bombs onto the underside of military aircraft could not sustain required loads during routine proof load testing. Three failed lugs underwent visual examination, chemical analysis, metallography, hardness testing, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. It was determined that the failures were due to forging defects. Both forging laps and seams acted as stress concentrators when the lugs were loaded during proof testing.

A component of a water filtration unit failed while being used in service for approximately eight months. The filter system had been installed in a commercial laboratory, where it was stated to have been used exclusively in conjunction with deionized water. The failed part had been injection molded from a 30% glass-fiber and mineral-reinforced nylon 12 resin. Investigation, including visual inspection, 118x SEM images, 9x micrographs, energy-dispersive x-ray spectroscopy, micro-FTIR in the ATR mode, and TGA, supported the conclusion that the filter component failed as a result of molecular degradation caused by the service conditions. Specifically, the part material had undergone severe chemical attack, including oxidation and hydrolysis, through contact with silver chloride. The source of the silver chloride was not established, but one potential source was photographic silver recovery.

Six cases of failure attributed to microbiologically influenced corrosion (MIC) were analyzed to determine if any of the failures could have been avoided or at least predicted. The failures represent a diversity of applications involving typical materials, primarily stainless steel and copper alloys, in contact with a variety of liquids, chemistries, and substances. Analytical techniques employed include stereoscopic examination, energy dispersive x-ray spectroscopy (EDS), temperature and pH testing, and metallographic analysis. The findings indicate that MIC is frequently the result of poor operations or improper materials selection, and thus often preventable.

On 15 March 2000, a National Railroad Passenger Corporation (Amtrak) train traveling from Chicago to Los Angeles derailed in Carbondale, KS. After the initial on-scene investigation, 12 pieces of rail were sent to the materials laboratory for examination. Ten of them were from the point of derailment (POD). A vertical crack was observed in the head of the rail (vertical split head). The crack was at least 233 in. (591 cm) long, continuing through the entire lengths of most pieces recovered from the POD. The vertical fracture surface had features consistent with overstress fracture with short-term exposure to an oxygen-rich environment. Fracture features emanated from longitudinally-aligned inclusions rich in aluminum.

An investigation of a Stirling engine after an aborted test run revealed that the regenerator screens had suffered substantial damage. During the run, the individual screens oscillated as the helium working fluid was shuttled through the regenerator. In localized areas, the 41 mu m (1600 mu in.) diam type 304 stainless steel wire screening had been torn and pieces were missing. Scanning electron microscope revealed that the fracture had occurred at wire crossover locations by a fatigue mechanism. The problem was solved by sintering the individual screens into a single unit.

This article provides information on the chemical characterization of surfaces by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). It describes the basic theory behind each of these techniques, the types of data produced from each, and some typical applications. The article explains the strengths of AES, XPS, and TOF-SIMS based on data obtained from the surface of a slightly corroded stainless steel sheet.