A batch of bimetal foil/epoxy laminates was rejected because of poor peel strength. The laminates were manufactured by sintering a nickel/phosphorus powder layer to a copper foil, cleaning, then chromate conversion coating the nickel-phosphorus surface, and laminating the nickel-phosphorus side of the clad bimetal onto an epoxy film, so that the end product contained nickel-phosphorus sandwiched between copper and epoxy, with a chromate conversion layer on the epoxy side of the nickel-phosphorus. Peel testing showed abnormally low adhesion strength for the bad batch of peel test samples. Comparison with normal-strength samples using XPS indicated an 8.8% Na concentration on the surface of the bad sample; the good example contained less than 1% Na on the surface. After 15 min of argon ion etching, depth profiling showed high concentrations of sodium were still evident, indicating that the sodium was present before the chromate conversion treatment was performed. A review of the manufacturing procedures showed that sodium hydroxide was used as a cleaning agent before the chromate conversion coating. Failure cause was that apparently the sodium hydroxide had not been properly removed during water rinsing. Thus, recommendation was to modify that stage in the processing.

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 first-stage nozzles of a high-pressure turbine section of an industrial gas turbine exhibited leading and trailing-edge deterioration. The nozzles were made of X-40, a cobalt-base alloy, and were aluminide coated. Failure analysis determined that the deterioration was the result of hot corrosion caused by a combination of contaminants, cooling-hole blockage, and coating loss.

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.

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.

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.

A crane long-travel worm drive shaft was found to be chipped during unpacking after delivery. Chemical analysis showed that the steel (EN36A with a case depth of 1 mm, or 0.04 inch did not meet specifications. Magnetic particle inspection revealed a crack on the side of the shaft opposite the chip. Metallographic examination indicated that the case depth was approximately 2 mm (0.08 in.) and that a repair weld of an earlier chip had been made in the cracked area. The chipping was attributed to excessive case depth and rough handling. It was recommended that the shaft be returned to the manufacturer and a replacement requested.

A high-pressure steam pipe specified to be P22 low-alloy steel failed after 25 years of service. Located at the end of the steam line, the pipe reportedly received no steam flow during normal service. Visual examination of the failed pipe section revealed a window fracture that appeared brittle in nature. Specimens from the fracture area and from an area well away from the fracture were examined metallographically and chemically analyzed. Results indicated that the pipe had failed by hydrogen damage that resulted in brittle fracture. Chemical analysis indicated that the pipe material was 1020 carbon steel, not P22. The misapplication of pipe material was considered to be a contributing factor. Position of the pipe within the system caused the localized damage.

An ASTM A 504 carbon steel railway car wheel that was used on a train in a metropolitan railway system failed during service, causing derailment. The wheel was completely fractured from rim to hub. Macrofractography of the fracture surface showed road grime, indicating that the crack had existed for a considerable time prior to derailment and initiated in the flange. Failure propagated from the flange across the rim and down the plate to the bore of the hub. Two zones that exhibited definite signs of heating were observed. The fracture initiation site was typical of fatigue fracture. No defects were found that could have contributed to failure. The wheel conformed to the chemical, microstructural, and hardness requirements for class A wheels. Failure was attributed to repeated severe heating and cooling of the rim and flange due to brake locking or misapplication of the hand brake. It was recommended that the brake system on the car be examined and replaced if necessary.

A low-carbon steel (St35.8) tube in a phthalic anhydride reactor system failed. Visual and stereomicroscopic examination of fracture surfaces revealed heavy oxide/deposits on the outer surface of the tube, tube wall thinning in the area of the fracture, and discolorations and oxides/deposits on the inner surface. Cross sections from the fracture surface were metallographically examined, and the deposits were analyzed. It was determined that the tube had thinned from the inner surface because of a localized overheating condition (probably resulting from a runaway chemical reaction within the tube) and then fractured, which allowed molten salt to flow into the tube.

A type 430Ti stainless steel flue gas expansion joint cracked because of caustic-induced stress-corrosion cracking. Energy-dispersive X-ray spectroscope analysis of the fracture surface deposits revealed the presence of sodium and potassium—caustics in hydroxide form. Primary fracture surfaces were all similar in appearance, and a primary crack origin could not be identified. A secondary crack brought to fracture in the laboratory showed brittle, cleavage features rather than classic, tensile overload features. This suggested that the material was embrittled.

Compound bow handle risers that had failed in service and during assembly along with an unassembled riser were submitted for analysis. The risers were die cast from magnesium-base alloy AM60A. Inspection of the failed risers and metallurgical investigations conducted on the stock riser revealed the presence of cold shuts at the same site in all specimens. It was recommended that all risers be thoroughly inspected and that the bow company work with their die casting shop to design a mold with acceptable filling characteristics.

A segment from a premium-quality H13 tool steel die for die casting of aluminum failed after only 700 shots. The segment was subjected to visual, macroscopic, hardness, and metallographic testing. The investigation revealed that failure occurred as a result of fatigue at an electrical-discharge-machined surface where the resulting rehardened layer had not been removed. This rehardened layer had cracked, providing a source for fatigue initiation.

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.

An ASTM A193-83a grade B7 (AISI 4140) steel turbine impeller shaft fractured after 2 months of service. Failure had initiated at three separate points around the periphery of the shaft, each associated with one of three keyways. SEM fractography, metallography, and chemical analysis indicated that the mechanism of fracture initiation was torsional fatigue. Intermittent deceleration and acceleration resulting from power surges during operation of the turbine caused torsional vibration and was considered the most probable source of the required cyclic stress. Final failure took place by torsional shear.

Waterwall tube failure samples removed from a coal- and oil-fired boiler in service for 12 years exhibited localized underdeposit corrosion and hydrogen damage. EDS and XRD revealed that bulk internal deposits collected from the tubes contained metallic copper which can accelerate corrosion through galvanic effects and can promote hydrogen damage. Ultrasonic testing was recommended to locate tubes with severe gouging and corrosion, which are suspect locations for hydrogen damage. The source of the copper should be identified and future chemical cleaning of the boiler should address its presence in the waterwall tubes.

Field metallography and replication were performed on a type 316 stainless steel column in diglycol amine vacuum service to determine the cause of visible OD pitting on the column in several areas above the insulation support rings. The examination revealed transgranular stress-corrosion cracking beneath the pitted areas on the OD. The likely cause of the cracking was chloride stress corrosion, with chlorides deriving from the marine atmosphere and concentrating under the insulation around the support rings. A complete insulation evaluation, including repair or replacement, was recommended to prevent chloride buildup. Painting of the steel surface with an epoxy-phenolic or epoxy-coal tar was also suggested.

Cracking was discovered in an in-service, second-stage turbine impeller during a downtime inspection. The fabricated 4300 series low-alloy steel impeller was used in a compressor in an industrial petrochemical plant. It was also reported that a process upset had allowed a 10% NaOH solution to be ingested by the unit. Routine magnetic particle inspection revealed numerous cracks in the hub area and vane tips of the second-stage impeller Additionally, the outside surface of the backing plate showed a cyclic pattern of cracks. An overview of a conventional, systematic metallurgical approach to failure analysis to confirm that the cracking was caused by a caustic stress-corrosion cracking mechanism is presented.

Numerous cracks observed on the surface of a forged A470 Class 4 alloy steel steam turbine rotor disc from an air compressor in a nitric acid plant were found to be the result of caustic induced stress-corrosion cracking (SCC). No material defects or anomalies were observed in the disc sample that could have contributed to crack initiation or propagation or secondary crack propagation. Chlorides detected in the fracture surface deposits were likely the primary cause for the pitting observed on the disc surfaces and within the turbine blade attachment area. It was recommended that the potential for water carryover or feedwater induction into the turbine be addressed via an engineering evaluation of the plant's water treatment procedures, steam separation equipment, and start-up procedures.

The interior surface of a type 316L stainless steel trailer barrel used to haul various chemicals showed evidence of severe pitting after less than 1 year of service. Two sections were cut from the barrel and microscopically examined. Metallographic sections were also prepared at the weld areas and away from the weld zones. Terraced, near-surface pits with subsurface caverns and a high level of sulfur in the pit residue, both indicative of bacteria-induced corrosion, were found. No evidence of weld defects or defective material was present. Testing of the water used at the wash station and implementation of bacteria control measures (a special drying process after washing and use of a sanitizing rinse) were recommended.