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.

A steel spring used in an automotive application suddenly began to fail in the field, although “nothing had changed” in the fabrication process. Fatigue tests using springs fabricated prior to field failures lasted 500,000 cycles to failure, whereas fatigue tests performed on springs fabricated after field failures lasted only 50,000 cycles to failure. It was discovered that the percent coverage of shot peening prior and subsequent to the increase in failure incidence was much less than 100%, with a shot peening time of 12 min. The residual-stress state of “as fabricated” springs in three conditions were evaluated using XRD: springs manufactured prior to failure incidence increase, 12 min peen; springs manufactured following failure incidence increase, 12 min peen; and 60 min peen. The conclusion was that the failure occurred because low peening time significantly decreased the compressive residual-stress levels in the springs. Recommendation was made to increase the time the spring was shot peened from 12 to 60 min.

Severe pitting corrosion of a carbon steel tube was observed in the air preheater of a power plant, which runs on rice straw firing. Approximately 1450 tubes were removed from Stage 3 of the preheater (air inlet and flue gas outlet) due to corrosion and local bursting. Samples from Stage 2 (where corrosion was low) and Stage 3 (severe corrosion) were taken and subjected to visual inspection, SEM, x-ray diffraction, microhardness measurement, and chemical and microstructural analysis. It was determined that extended non-operation of the plant resulted in the settlement of corrosive species on the tubes in Stage 3. The complete failure of the tube occurred due to diffusion of these elements into the base metal and precipitation of potassium and chlorine compounds along the grain boundaries, with subsequent dislodging of grains. The nonmetallic inclusions acted as nucleating sites for local pitting bursting. Nonuniform heat transfer in Stage 3 operation accelerated the selective corrosion of front-end tubes. The relatively high heat transfer in this stage resulted in condensation of some corrosive gases and consequent corrosion. Continuous operation of the plant with some precautions during assembly of the tubes reduced the corrosion problem.

An arsenical admiralty brass (UNS C44300) finned tube in a generator air cooler unit at a hydroelectric power station failed. The unit had been in operation for approximately 49,000 h. The cooling medium for the tubes was water from a river. Air flowed over the finned exterior of the tubes, while water circulated through the tubes. Investigation (visual inspection, leak testing, history review, 100X micrographs etched in potassium dichromate, chemical analysis, and EDS and XRD analysis of internal tube deposits) supported the conclusion that the cause of the tube leaks was ammonia-induced SCC. Because the cracks initiated on the inside surfaces of the tubes and because the river water was not treated before it entered the coolers, the ammonia was likely present in the river water and probably concentrated under the internal deposits. Recommendations included either eliminating the ammonia (prohibitively expensive in cost and time) or using an alternate material (such as a 70Cu-30Ni alloy or a more expensive titanium alloy) that is resistant to ammonia corrosion as well as to chlorides and sulfur species.

The shaft-and-bearing assembly in a freon compressor was subjected to severe pounding and vibration after six years of service. After about one year of service, the compressor had been shut down to replace a bearing seal. One month before the shaft failed, a second seal failure occurred, requiring the collar, spacer sleeve, seal, roller bearing, and lock washer to be replaced. The shaft was made of 4140 steel, heat treated to a hardness of 20 to 26 HRC. The seal, bearing, and lock washer were commercial components. Investigation (visual inspection, 4.5x images, x-ray diffraction, hardness testing, and microscopic exam) supported the conclusion that shaft failure was initiated by fretting between the bearing race and the bearing surface on the shaft because of improper bearing installation. Once clearance was established between the bearing and the shaft, the shaft began pounding on the inner bearing race, causing final failure of the shaft surface. Recommendations included proper fitting of the shaft and bearing race to preventing movement of the bearing on the shaft. Also, the lock washer and locknut must be installed properly.

Cracks initiating from the tip of the cloverleaf pattern in steel cargo tiedown sockets were observed by the builder following installation aboard several cargo vessels in various stages of construction. Testing of finite element models and measurements performed in the field on cargo ships with the cracking problem supported the conclusion that the failure was caused by overload. Additional testing showed that the overload failure and the transition from ductile to brittle fracture were facilitated by a combination of high brittleness due to flame cutting, increased hardness due to the cold-working coining process, and high residual stresses created by welding. Recommendations included the removal of the brittle, carbon-rich transformed martensite layer introduced by flame cutting and the application of a localized stress-relief heat treatment process. X-ray diffraction residual-stress measurements were then performed on heat treated tiedown sockets to verify the effectiveness of the localized heat treatment process applied.

Immediately after installation, leakage was observed at the mounting surface of several rebuilt hydraulic actuators that had been in storage for up to three years. At each joint, there was an aluminum alloy spacer and a vellum gasket. The mounting flanges of the steel actuators had been nickel plated. During assembly of the actuators a lubricant containing molybdenum disulfide had been applied to the gaskets as a sealant. The vellum gasket was found to be electrically conductive, and analysis (visual inspection, 500x unetched micrographs, galvanic action testing, and x-ray diffraction) supported the conclusions that leakage was the result of galvanic corrosion of the aluminum alloy spacers while in storage. The molybdenum disulfide was apparently suspended in a volatile water-containing vehicle that acted as an electrolyte between the aluminum alloy spacer and the nickel-plated steel actuator housing. Initially, the vellum gasket acted as an insulator, but the water-containing lubricant gradually impregnated the vellum gasket, establishing a galvanic couple. Recommendations included discontinuing use of molybdenum disulfide lubricant as a gasket sealer, and assembling the actuators using dry vellum gaskets.

Accelerated aging tests on detonator assemblies, to verify the compatibility of gold bridgewire and Pd-In-Sn solder with the intended explosives, revealed an unusual form of corrosion. The tests, conducted at 74 deg C (165 deg F) and 54 deg C (130 deg F), indicated a preferential attack of the gold. To investigate the problem, a matrix of test units was produced and analyzed. Scanning electron microscopy, EDX analysis, and x-ray diffraction techniques were used to determine the extent of the corrosion and identify the corrosion products. The results indicated that the preferential attack of the gold was due to HCN formed by decomposition of the explosive powder at high temperatures. Other associated reactions were also observed including the subsequent attack of the solder by the gold corrosion product and degradation of the plastic header.

Military aircraft use a cartridge ignition system for emergency engine starts. Analysis of premature failures of steel (AISI 4340) breech chambers in which the solid propellant cartridges were burned identified corrosion as one problem with an indication that stress-corrosion cracking may have occurred. A study was made for stress-corrosion cracking susceptibility of 4340 steel in a paste made of the residues collected from used breech chambers. The constant extension rate test (CERT) technique was employed and SCC susceptibility was demonstrated. The residues, which contained both combustion products from the cartridges and corrosion products from the chamber, were analyzed using elemental analysis and x-ray diffraction techniques. Electrochemical polarization techniques were also utilized to estimate corrosion rates.

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.