Cracks, with no other damage, were observed in a niobium alloy (Nb-106) part when it was pulled from several months of protective storage for assembly into a rocket nozzle. SEM views showed the cracks to be intergranular, with contaminant particles on a large number of the grain facets. EDX analysis showed they consisted of niobium and fluorine. Plastic replicas, prepared by standard TEM techniques, were analyzed with selected-area electron diffraction, showing a pattern match for niobium tetrafluoride. Auger analyses showed electron spectra containing peaks representing carbon, oxygen, nitrogen, fluorine, and chlorine. Investigation into the processing history of the part showed the tenacious oxide film formed by the affinity of niobium for oxygen - even when heat treated in a vacuum – was removed with a combination of strong acids: nitric, hydrochloric, hydrofluoric, and lactic, resulting in the contaminants found on the surface. Thus, residues of the cleaning acid on the part had caused SCC during storage, with the tensile stresses necessary to generate SCC assumed to have been residual stresses from the heat treatment. Recommendation was made that more stringent cleaning procedures to remove any trace of the cleaning acids be used.

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.

A Ti-6Al-4V alloy pressure vessel failed during a proof-pressure test, fracturing along the center girth weld. The girth joints were welded with the automatic gas tungsten arc process utilizing an auxiliary trailing shield attached to the welding torch to provide inert-gas shielding for the exterior surface of the weld. A segmented backup ring with a gas channel was used inside the vessel to shield the weld root. The pressure vessel failed due to contamination of the fusion zone by oxygen, which resulted when the gas shielding the root face of the weld was diluted by air that leaked into the gas channel. Thermal stresses cracked the embrittled weld, exposing the crack surfaces to oxidation before cooling. One of these cracks caused a stress concentration so severe that failure of the vessel wall during the proof test was inevitable. A sealing system at the split-line region of the segmented backup ring was provided, and a fine-mesh stainless steel screen diffuser was incorporated in the channel section of the backup ring to prevent air from leaking in. A titanium alloy color chart was furnished to permit correlation of weld-zone discoloration with the degree of atmospheric contamination.

One inch diam Type 304 stainless steel piping was designed to carry containment atmosphere samples to an analyzer to monitor hydrogen and oxygen levels during operational and the design basis accident conditions that are postulated to occur in a boiling water reactor. Only one of six lines in the system had thru-wall cracks. Shallow incipient cracks were detected at the lowest elevations of one other line. The balance of the system had no signs of SCC attack. Chlorides and corrosion deposits in varying amounts were found throughout the system. The failure mechanism was transgranular, chloride, stress-corrosion cracking. Replacement decisions were based on the presence of SCC attack or heavy corrosion deposits indicative of extended exposure time to chloride-contaminated water. The existing uncracked pipe, about 75 percent of the piping in the system, was retained despite the presence of low level surface chlorides. Controls were implemented to insure that temperatures are kept below 150 deg F, or, walls of the pipe are moisture-free or the cumulative wetted period will never exceed 30 h.

An aluminum brass seawater surface condenser failed due to pitting after less than one year of service. Large pits filled with a green deposit were evidenced under the nonuniform black scale present over the entire inside surface of the tube. The black deposit was identified as primarily copper sulfide, with zinc and aluminum sulfides while the green deposit was revealed to be copper chloride. The combination of sulfide and chloride attack on the tubes was concluded to have resulted in the failure. Injection of ferrous sulfate upstream of the condenser which could aid the formation of protective oxide films was recommended.

An outer fan-duct assembly of titanium alloy Ti-5Al-2.5Sn (AMS 4910) for a gas-turbine fan section cracked 75 mm (3 in.) circumferentially through a repair weld in an arc weld in the front flange-duct segment. Examination of the crack with a binocular microscope revealed no evidence of fatigue. A blue etch-anodize inspection showed the presence of an alpha case along the edges of the repair weld. The alpha case, a brittle oxide-enriched layer, forms when welds are inadequately shielded from the atmosphere during deposition. The brittleness of this layer caused transgranular cracks to form and propagate in tension under the thermal stresses created by the repair-weld heat input. The crack resulted from contamination and embrittlement of a repair weld that had received inadequate gas shielding. Thermal stresses cracked the oxide-rich layer that formed. The gas-shielding accessories of the welding torch were overhauled to ensure that leak-in or entrainment of air was eliminated. Also, the purity of the shielding-gas supplies was rechecked to make certain that these had not become contaminated.

Numerous protective covers, used in conjunction with an electrical appliance, failed during assembly with the mating components. The failures were traced to a particular production lot of the covers and occurred during insertion of the screws into the corresponding bosses. The parts had been injection molded from an ABS resin to which regrind was routinely added. Inspection of both the failed covers and retained parts, which exhibited normal behavior during assembly, included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The FTIR results indicated the presence of contaminant material exclusively within the ABS resin used to mold the failed covers, and the thermograms suggested contamination with a PBT resin. Further TGA analysis showed the contamination was estimated to account for approximately 23% of the failed cover material. The conclusion was that the appliance covers failed via brittle fracture associated with stress overload. The failures, which occurred under normal assembly conditions, were attributed to embrittlement of the molded parts, due to contamination of the ABS resin with a high level of PBT. The source of the PBT resin was not positively identified, but a likely source appeared to be the use of improper regrind.

Within the first few months of operation of an 8 km (5 mile) long 455 mm (18 in.) diam high-pressure steam line between a coal-fired electricity-generating plant and a paper mill, several of the Inconel 600 bellows failed. The steam line operated at 6030 kPa (875 psi) and 420 deg C (790 deg F). Metallographic sections, energy-dispersive x-ray spectra, chemical analyses, tensile tests, and Auger microscope analyses showed the failed bellows met the specifications for the material. However, investigation also showed entire oxide thickness was contaminated with relatively large amounts of sodium, calcium, potassium, aluminum, and sulfur, alkali, alkali earth, and other contaminants that completely permeated even the thin oxides on the fracture surfaces. Additional investigation of the purity of the steam itself as reported by the power plant showed that corrosion and cracks were ultimately caused by the steam. While under normal operation, the steam's purity posed no problem to the material, during boiler cleaning operations, the generating plant had allowed contamination to get into the steam line.

Failure of three C22000 commercial bronze rupture discs was caused by mercury embrittlement. The discs were part of flammable gas cylinder safety devices designed to fail in a ductile mode when cylinders experience higher than design pressures. The subject discs failed prematurely below design pressure in a brittle manner. Fractographic examination using SEM indicated that failure occurred intergranularly from the cylinder side. EDS analysis indicated the presence of mercury on the fracture surface and mercury was also detected using scanning auger microprobe (SAM) analysis. The mercury was accidentally introduced into the cylinders during a gas-blending operation through a contaminated blending manifold. Replacement of the contaminated manifold was recommended along with discontinued use of mercury manometers, the original source of mercury contamination.

Following a freight train derailment, part of a fractured side frame was retained for study because a portion of its fracture surface exhibited a rock candy appearance and black scale. It was suspected of having failed, thereby precipitating the derailment. Metallography, scanning electron microscopy, EDXA, and x-ray mapping were used to study the steel in the vicinity of this part of the fracture surface. It was found to be contaminated with copper. Debye-Scherrer x-ray diffraction patterns obtained from the scale showed that it consisted of magnetite and hematite. It was concluded that some copper was accidentally left in the mold when the casting was poured. Liquid copper, carrying with it oxygen in solution, penetrated the austenite grain boundaries as the steel cooled. The oxygen reacted with the steel producing a network of scale outlining the austenite grain structure. When the casting fractured as a result of the derailment, the fracture followed the scale in the contaminated region thus creating the “rock candy” fracture.

An SB407 alloy 800H tube failed at a 100 deg bend shortly after startup of a new steam superheater. Three bends failed and one bend remote from the failure area was examined. Visual examination showed that the fracture started on the outside surface along the inside radius of the bend and propagated in a brittle, intergranular fashion. Chemical analysis revealed that lead contamination was a significant factor in the failure and phosphorus may have contributed. The localized nature of the cracks and minimum secondary cracking suggested a distinct, synergistic effect of applied tensile stress with the contamination. Stress analysis found that stress alone was not enough to cause failure; however the operating stresses in the 100 deg bends were higher than at most other locations in the superheater Reduced creep ductility may be another possible cause of failure. Remedial actions included reducing the tube temperature, replacing the Schedule 40 100 deg bends with Schedule 80 pipe, and solution annealing the pipe after bending.

Several type 304L stainless steel dished ends used in the fabrication of cylindrical vessels developed extensive cracking during storage. All of the dished ends had been procured from a single manufacturer and belonged to the same batch. When examined visually, several rust marks were observed, indicating contamination by rusted carbon steel particles. Liquid penetrant testing was used to determine the extent of the cracks, and in situ metallographic analysis was performed over the cracked region. The morphology of the cracks was indicative of transgranular stress-corrosion cracking (TGSCC). Conditions promoting the occurrence of the TGSCC included significant tensile stresses on the inside of the dished ends, the presence of surface contamination by iron due to poor handling practice using carbon steel implements, and storage in a coastal environment with an average temperature of 25 to 32 deg C (77 to 90 deg F), an average humidity ranging from 70 to 80%, and an atmospheric NaCl content ranging from 8 to 45 mg/m2 /day. Recommendations preventing further occurrence of the situation were strict avoidance of the use of carbon steel handling implements, strict avoidance of cleaning practices that cause long-term exposure to chlorine-containing cleaning fluid, and solution annealing of the dished ends at 1050 deg C (1920 deg F) for 1 h followed by water quenching to relieve residual stresses.

The contamination of lubrication with powdered stone resulted in progressive wear of the internal surfaces of a bearing. Because of the motion of rollers, the inner race exhibited an unusual cyclic washboard wear pattern. Because of a lack of bearing conformity, wear progressed into severe coarse-grain spalling.

This article considers the main characteristics of wear mechanisms and how they can be identified. Some identification examples are reported, with the warning that this task can be difficult because of the presence of disturbing factors such as contaminants or possible additional damage of the worn products after the tribological process. Then, the article describes some examples of wear processes, considering possible transitions and/or interactions of the mechanism of fretting wear, rolling-sliding wear, abrasive wear, and solid-particle erosion wear. The role of tribological parameters on the material response is presented using the wear map concept, which is very useful and informative in several respects. The article concludes with guidelines for the selection of suitable surface treatments to avoid wear failures.

This article discusses the classification of sliding bearings and describes the major groups of soft metal bearing materials: babbitts, copper-lead bearing alloys, bronze, and aluminum alloys. It provides a discussion on the methods for fluid-film lubrication in bearings. The article presents the variables of interest for a rotating shaft and the load-carrying capacity and surface roughness of bearings. Grooves and depressions are often provided in bearing surfaces to supply or feed lubricant to the load-carrying regions. The article explains the effect of contaminants in bearings and presents the steps for failure analysis of sliding bearings. It also reviews the factors responsible for bearing failure with examples.

Linear indications on the outer surface of a cross in a piping system were revealed by dye-penetrant examination. The cross was specified to be SA403 type WP 304 stainless steel. The cross had been subjected to induction-heating stress improvement. The linear indications on the cross were located in wide bands running circumferentially below the cross-to-cap weld and above the cap-to-discharge-pipe weld. The material was found to conform to the requirements both in terms of hardness and strength. Intergranular cracks filled with oxide were observed on metallographic analysis of a sectioned and oxalic acid etched sample. The grain size was found to exceed the ASTM standard. No indications of sensitization were observed during testing with practice A of ASTM A 262. Definitive evidence of contaminants to support SCC as the failure mechanism was not disclosed during analysis. It was concluded that overheating or burning of the forging, which classically results in large grain size, intergranular fractures, and fine oxide particles dispersed throughout the grains was the possible reason for the failure.

A nickel alloy cylinder plated with chromium along its inner liner, installed in a commercial ice cream freezer, showed gray discoloration along its OD surface. The discolored parts exhibited significantly reduced cooling efficiency as compared with new cylinders. During operation, the OD of the cylinder was exposed to liquid ammonia refrigerant containing lubricant from the compressor. The lubricant (mineral oil) was intended to separate from the ammonia and be recirculated through the compressor. Nondestructive portable optical microscopy, XRF, EDS, and XPS analyses showed that the discoloration on the cylinder was associated with metal oxidation products coated with a thin oil film. One of the recommendations was to plate the OD of the cylinder with hard chromium to increase its resistance to erosion. Another recommendation was to reduce the amounts of water contamination in the refrigerant.

Corrosion in a closed-loop cooling water system constructed of austenitic stainless steel occurred during an extended lay up of the system with biologically contaminated water. The characteristics of the failure were those of microbiologically influenced corrosion (MIC). The corrosion occurred at welds and consisted of large subsurface void formations with pinhole penetrations of the surfaces. Corrosive attack initiated in the heat affected zones of the welds, usually immediately adjacent to fusion lines. Stepwise grinding, polishing, and etching through the affected areas revealed that voids generally grew in the wrought material by uniform general corrosion. Tunneling or worm-holing was also observed, whereby void extension occurred by initiating daughter voids probably at flaws or other inhomogeneities. Selective attack occurred within the fusion zone, i.e., within the cast two-phase structure of the weld filler itself. The result was a void wall which consisted of a rough and porous ferritic material, a consequence of preferential attack of the austenitic phase and slightly lower rate of corrosive attack of the ferrite phase. The three-dimensional spongy surface was studied optically and with the scanning electron microscope.

New aircraft wing panels extruded from 7075-T6 aluminum exhibited an unusual pattern of circular black interrupted lines, which could not be removed by scouring or light sanding. The panels, subsequent to profiling and machining, were required to be penetrated inspected, shot peened, H2SO4 anodized, and coated with MIL-C-27725 integral fuel tank coating on the rib side. Scanning electron microscopy and microprobe analysis (both conventional energy-dispersive and Auger analyzers) showed that the anodic coating was applied over an improperly cleaned and contaminated surface. The expanding corrosion product had cracked and, in some places, had flaked away the anodized coating. The corrodent had penetrated the base aluminum in the form of subsurface intergranular attack to a depth of 0.035 mm (0.0014 in.). It was recommended that a vapor degreaser be used during cleaning prior to anodizing. A hot inhibited alkaline cleaner was also recommended during cleaning prior to anodizing. The panels should be dichromate sealed after anodizing. The use of deionized water was also recommended during the dichromate sealing operation. In addition, the use of an epoxy primer prior to shipment of the panels was endorsed. Most importantly, surveillance of the anodizing process itself was emphasized.

During an acceptance test of the Apollo spacecraft 101 service module prior to delivery, an SPS fuel pressure vessel (SN054) (titanium Ti-6Al-4V, approximately 1.2 m (4 ft) in diam and 3 m (10 ft) long) containing methanol developed cracks adjacent to the welds. The test was stopped. This acceptance test had been run 38 times on similar pressure vessels without problems. The methanol was a safe-fluid replacement for the storable hypergolic fuels (blend of 50% hydrazine and 50% unsymmetrical dimethyl hydrazine). Investigation (visual inspection and 65X images) showed similarities to stress-corrosion resulting from contamination during misprocessing of the vessels. However, another vessel underwent a more severe testing procedure and failed catastrophically. Further investigation supported the conclusion that the failure cause was SCC of titanium in methanol. Attack is promoted by crazing of the protective oxide film. It was learned that minor changes in the testing procedures could inhibit or accelerate the reaction. Recommendations included replacing the methanol with a suitable alternate fluid. Isopropyl alcohol was chosen after considerable testing. This incident further resulted in the imposition of a control specification (MF0004-018) for all fluids that contact titanium for existing and future space designs.