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.

Some 99.90 pure tin tubes (0.15 mm thick) used for packaging a chemical compound cracked on bending and underwent brittle fracture prior to filling, while others remained ductile and showed no sign of failure. Examination showed that specimens prepared by mechanical methods such as electrolytic and hand polishing and the vibration method resulted in poor edge and crack edge definition due to material thickness. Etching experiments involved a grain surface attack and hence produced a rather strong surface relief from which the grain boundary cracks could again not clearly be differentiated. The sections were therefore examined unetched in polarized light. The microstructure of the cracked tubes was shown to have much smaller grains than the ductile and showed cracks from the surface down along the grain boundaries. Material hardness also differed between the unusable tubes and the ductile, and chemical analysis showed a higher level of aluminum in the brittle specimens. Failure obviously occurred due to the high material aluminum content that increased hardness which then caused embrittlement at the surface which led to cracks or fracture on bending. Since no explanation of how the aluminum entered the tin was available, no recommendations could be made.

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 provides a discussion on the metallographic techniques used for failure analysis, and on fracture examination in materials, with illustrations. It discusses various metallographic specimen preparation techniques, namely, sectioning, mounting, grinding, polishing, and electrolytic polishing. The article also describes the microstructure examination of various materials, with emphasis on failure analysis, and concludes with information on the examination of replicas with light microscopy.

Several torsion bars had failed in a projectile weaving machine and were analyzed to determine the cause. Specimens prepared from the damaged components were subjected to visual inspection, hardness testing, chemical analysis, and metallurgical evaluations. The failed torsion bars had been fabricated from spring steel which, according to stress calculations, did not have sufficient torsional strength. Examination of the damaged parts confirmed the finding, revealing that all fractures started at a shoulder radius in an area of high stress concentration. Based on the investigation, the shoulder radius should be increased to alleviate stress and the working torsion angle of the bar should be decreased to improve safety factors.

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.

Metallographic examination is one of the most important procedures used by metallurgists in failure analysis. Typically, the light microscope (LM) is used to assess the nature of the material microstructure and its influence on the failure mechanism. Microstructural examination can be performed with the scanning electron microscope (SEM) over the same magnification range as the LM, but examination with the latter is more efficient. This article describes the major operations in the preparation of metallographic specimens, namely sectioning, mounting, grinding, polishing, and etching. The influence of microstructures on the failure of a material is discussed and examples of such work are given to illustrate the value of light microscopy. In addition, information on heat-treatment-related failures, fabrication-/machining-related failures, and service failures is provided, with examples created using light microscopy.

Several fuses made of nickel silver (57 to 61% Cu, 11 to 13% Ni, bal Zn) exposed to air containing ammonium and nitrate ions failed by SCC. Test solutions of 1 N ammonium nitrate (NH4NO3) and a 1:1 mixture of 1 N sodium nitrate (NaNO3) and 1 N calcium nitrate (Ca(NO3) 2) were prepared. In addition, stressed fuses made of nickel silver and of cupro-nickel (80Cu-20Ni) were exposed to a drop of corrosive solution in the stressed area. All nickel silver specimens failed after two days of exposure to NH4NO3 solution. However, 17% of them failed and 67% showed crack initiation but no failure after 42 days of exposure to NaNO3 + Ca(NO3)2 solution. None of the cupro-nickel specimens failed, but among those exposed to NH4NO3, 17% displayed crack initiation and 83% showed partial dealloying after 42 days. Based on the test results, the fuse material was changed from nickel silver to cupro-nickel, solving the SCC problem.

Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.

During a hydraulic test on one of the boilers in a range, leakage occurred from the lower surface of a horizontal S bend in the main steam pipe between the drum connector box and the junction valve. The pipe in question was 15 in. bore and had been in service for about 50 years. Specimens were prepared for microscopical examination to include the defective zone and a section through a circumferential crack. The defective zone was found to contain numerous inclusions of slag and oxides of globular form. Regions surrounding the inclusions were decarburized, the indications being that this region of the plate had been heated to an excessively high temperature. A corrosion-fatigue fissure was at one location, this having originated at the internal surface of the pipe and run into an inclusion in the defective zone. The failure resulted from the development of corrosion-fatigue fissures which originated at a zone containing defects introduced at the time of manufacture. These may have had their origin in the ingot from which the plate was rolled or, alternatively, be indicative of a zone which suffered overheating and local burning at the time the forge weld was made.

The Pandia digester is a long cylindrical vessel which uses alkaline sulfite liquor to cook sawdust for pulping. The inlet cone was fabricated from AISI 304L stainless steel with E308 welds. Typical liquor concentration was approximately 80% NaOH, 20% Na2SO3 with chloride concentrations at 2 grams per liter. The operating pressures in the inlet cone were up to 1.2 MN/sq m (170 psig). The inlet cone had developed leaks within a year of service. Liquid penetrant inspection showed significant through-wall cracking near the fillet welds joining the bottom flange and side wall and the butt welds. Metallographic specimens were prepared from the welds to examine the microstructure and nature of the cracks. The cooking liquor at the inlet cone contained over ppm chlorides and was aggressive to 304 stainless steel. The cracking was identified as chloride-induced SCC. The inlet cone was replaced with an Inconel clad carbon steel inlet cone to combat the SCC.

An air bottle, machined from a solid block of aluminum alloy 2219-T852, displayed liquid-penetrant crack indications after assembly welding. The air bottle was machined to rough shape, a 3.8 mm (0.15 in.) wall thickness cylindrical cup with a 19 mm (3/4 in.) wall thickness integral boss on one side. After annealing, hot spinning, annealing a second time, and tack welding a port fitting, the assembly was torch preheated to 120 to 150 deg C (250 to 300 deg F). The port fitting was then welded in place. Final full heat treatment to the T62 temper was followed by machining, testing, and inspection. The crack indications were found only on one side of the boss and on the lower portion of the hot-spun dome region. The metallographic specimens revealed triangular voids and severe intergranular cracks. The cracks displayed the glossy surfaces typical of melted and resolidified material. The localized cracks in the air bottle were from grain-boundary eutectic melting caused by local torch overheating used in preparation for assembly welding of a port fitting. A change in design was scheduled to semiautomatic welding without the use of preheating for the joining of the port fitting for the dome opening.

Countersunk riveted joints in aluminum sheet are widely employed in the aircraft industry. The preparation of the sheet for the riveting process consists either of countersinking where the sheet is sufficiently thick or of dimpling. Metallographic assessment of dimple defects is described in specimens made of clad aluminum sheet of alloy type AlZnMgCu1.5. Addressed are a dimple with partially missing stamped surface (bell-mouth), a cylindrical prominence because the dimpling force was too great and the stamping cylinder force too low, and a dimple with flashes at the top surfaces of the sheet as a result of play between the stamping cylinder and the anvil head (ringed dimple). Frequently, overlapping of several defects occurs, especially with steel or titanium sheet, with the result that it is difficult to identify the defects.

A Lynx helicopter from the Royal Netherlands Navy lost a rotor blade during preparation for take-off. The blade loss was due to failure of a rotor hub arm by fatigue. The arm was integral to the titanium alloy rotor hub. An extensive material based failure analysis covered the hub manufacture, service damage, and estimates of service stresses. There was no evidence for failure due to poor material properties. However, fractographic and fracture mechanics analyses of the service failure, a full scale test failure, and specimen test failures indicated that the service fatigue stress history could have been more severe than anticipated. This possibility was subsequently supported by a separate investigation of the assumed and actual fatigue loads and stresses.

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.

The gun mount used in two types of self-propelled artillery consists of an oil-filled recoil cylinder and a sand-cast (MIL-I-11466, grade D7003) ductile-iron piston that connects to the gun tube through a threaded rod. The piston contains several orifices through which oil is forced as a means of absorbing recoil energy. During operation, the piston is stressed in tension, pulled by oil pressure on one end and the opposing force of the gun tube on the other. The casting specification stipulated that the graphite be substantially nodular and that metallographic test results be provided for each lot. Investigation (visual inspection, fatigue testing, 0.25x/0.35x/50x magnifications, 2% nital etched 60x/65x magnifications, and SEM views) showed that most of the service fractures occurred in pistons containing vermicular graphite. Recommendations included ultrasonic testing of pistons already in the field to identify and reject those containing vermicular graphite. In addition, metallographic control standards were suggested for future production lots.

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.

During a routine start-up exercise of a standby service water pump, a threaded coupling that joined sections of a 41.5 ft (12.7 m) long pump shaft experienced fracture. The pump was taken out of service and examined to determine the cause of fracture. It was apparent early in the examination that the fracture involved hydrogen stress cracking. However, the nature of the corrosive attack suggested an interaction between the threaded coupling and biological organisms living in the freshwater environment of the pump shaft. The organisms had colonized on the coupling, changing the local environment and creating conditions favorable to hydrogen stress cracking. This paper describes the analysis of the fracture of the coupling and provides an example of how biologically induced corrosion can result in unexpected fracture of a relatively basic machine part.