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.

In a housing made of cast steel GS 20MoV12 3, weighing 42 tons, precipitates were found on the austenitic grain boundaries during metallographic inspection. According to their shape and type they were recognized as carbides that precipitated during tempering. In addition, a much coarser network of rod-shaped and plate-shaped precipitates was found, that probably corresponded to the primary grain boundaries, or to the grain boundaries or twin planes of the austenite formed during solidification of the melt. These particles could have been aluminum nitride judging by their shape and order of precipitation. Tests showed that a subsequent removal of this defect by solutioning was impractical because the annealing temperature was too high. To avoid this defect in the future the sole recommendation is to accelerate the cooling rate through the critical region between 1200 to 900 deg C to such an extent as is practicable with respect to machinability.

Octagonal cast ingots weighing 6.5 tons and made of unalloyed heat treated steel CK 45 according to DIN 17200, and crankshafts forged from these ingots showed internal separations during ultrasonic testing. To determine the cause of defect, an ingot slice and a crank arm were examined metallographically. Investigation showed this was a case where flaky forgings were made from cast ingots with primary grain boundary cracks. This parallelity supports the often expressed opinion that both occurrences have the same origin, i.e. that hydrogen precipitation was the driving force in the formation of primary grain boundary cracks in cast ingots.

A microstructural analysis has been made of a burner nozzle removed from service in a coal gasification plant. The nozzle was a casting of a Co-29wt%Cr-19wt%Fe alloy. Extensive hot corrosion had occurred on the surface. There was penetration along grain boundaries, and corrosion products in these regions were particularly rich in S, and also contained Al, Si, O, and Cl. The grain boundaries contained Cr-rich particles which were probably Cr23-C6 type carbides. In the matrix, corrosion occurred between the Widmanstatten plates. Particles were found between these plates, most of which were rich in Cr and O, and probably were Cr2-O3 oxides. Other matrix particles were found which were rich in Al, O, and S. The corrosion was related to these grain boundary and matrix particles, which either produced a Cr-depleted zone around them or were themselves attacked.

Results of failure analyses of two aircraft crankshafts are described. These crankshafts were forged from AMS 6414 (similar composition to AISI 4340) vacuum arc remelted steels with sulfur contents of 0.003% (low sulfur) and 0.0005% (ultra-low sulfur). A grain boundary sulfide precipitate was caused by overheat of the low sulfur steel, and an incipient melting of grain boundary junctions was caused by overheat of the ultra-low sulfur steel. The precipitates and incipient melting in these two failed crankshafts were observed during the examination. As expected, impact fractures from the low sulfur steel crankshaft contained planar dimpled facets along separated grain boundaries with a small spherical manganese sulfide precipitates within each dimple. In contrast, planar dimpled facets along separated grain boundaries of impact fractures from the ultra-low sulfur crankshaft steel contained a majority of small spherical particles consisting of nitrogen, boron, iron, carbon, and a small amount of oxygen. Some other dimples contained manganese sulfide precipitates. Fatigue samples machined from the ultra-low sulfur steel crankshaft failed internally at planar grain boundary facets. Some of the facets were covered with nitrogen, boron, iron, and carbon film, while other facets were relatively free of such coverage. Results of experimental forging studies defined the times and temperatures required to produce incipient melting overheat and facets at grain boundary junctions of ultra-low sulfur AMS 6414 steels.

Two of four adjustable Moore pins, which had been used to stabilize a proximal femur fracture, were found to be broken and deformed at their threads. The pins were made from a cobalt-chromium alloy and were not in the same condition. Brittle precipitates in the grains and grain boundaries were seen in one of the pins and hence the fracture was revealed to have occurred along the grain boundaries. The other pin made from cold-worked cobalt-chromium alloy was observed to have randomly lines of primary inclusions. Intermingled dimples and fatigue striations were exhibited on the fracture surface of this pin. Thus, the effect of different conditions of cobalt-chromium alloys on failure behavior was demonstrated as a result of this study.

The failure of a boiler operating at 540 °C and 9.4 MPa was investigated by examining material samples from the near-failure region and by thermodynamic analysis. A scanning Auger microprobe, SEM, and commercial thermodynamic software codes were used in the investigation. Results indicated that the boiler failure was caused by grain-boundary segregation of phosphorous, tin, and nitrogen and the in-service formation of carbide films and granules on the grain boundaries.

Microstructural examinations on transverse cross sections of a steam reformer tube, showed the presence of large macrovoids elongated in the radial direction and emanating from the internal surface of the tube. The macrovoids were located at the interdendritic regions, and were partially filled by a Mn-Fe bearing chromium oxide film. The areas adjacent to the oxide film were chemically depleted in C, Cr and Mn and rich in Fe and Ni. Associated with this depletion were a large concentration of microvoids. It was suggested that the dissolution of carbides in areas surrounding the macrovoids and the concentration of stresses at their tips, caused extensive localized plastic deformation which led to the formation of microvoids and subsequently to the spalling of the oxide film. The non-protective character of the film induced a progressive deterioration of the grain boundaries properties. Grain boundary sliding and dislocation motion were enhanced, causing a local increase in the steady state strain rate and the premature failure of the tube.

A preflight inspection found a broken diaphragm from a side controller fabricated from 17-7 PH stainless steel in the RH 950 heat treatment condition. Failure occurred by cracking of the base of the flange-like diaphragm. The crack traveled 360 deg around the diaphragm. Scanning electron microscopy (SEM) revealed that the failure occurred by a brittle intergranular mechanism and stress-corrosion cracking (SCC), and indicated a failure mode of selective grain-boundary separation. The diaphragms were heat treated in batches of 25. An improper heat treatment could have resulted in the formation of grain boundary precipitates, including chromium carbides. It was concluded that failure of the diaphragm was due to a combination of sensitization caused by improper heat treatment and subsequent SCC. It was recommended that the remaining 24 sensor diaphragms from the affected batch be removed from service. In addition, a sample from each heat treat batch should be submitted to the Strauss test (ASTM A262, practice E) to determine susceptibility to intergranular corrosion. Also, it was recommended that a stress analysis be performed on the system to determine whether a different heat treatment (which would offer lower strength but higher toughness) could be used for this part.

In this article, we report the outcome of an investigation made to uncover the premature fracture of crusher jaws produced in a local foundry. A crusher jaw that had failed while in service was studied through metallographic techniques to determine the cause of the failure. Our investigation revealed that the reason for the fracture was the presence of large carbides at the grain boundaries and in the grain matrix. This led to the formation of microcracks that propagated along the grain boundaries under in-service working forces. It is also believed that the precipitation of carbides at the grain boundaries may have occurred because of improper heat treatment, but not because of a deficiency in composition.

A sleeve-shaped fire shield that operates inside one of two burner trains in an oil and gas processing unit ruptured after 15 y of service. A detailed analysis was conducted to determine how and why the sleeve failed. The investigation included visual inspection, chemical and gas analysis, mechanical property testing, stereomicroscopy, and metallographic examination. The fire sleeves are fabricated from 3-mm thick plate made of Incoloy 800 rolled into 540-mm diam sections welded along the seam. Three such sections are joined together by circumferential welds to form a single 2.8 m sleeve. The findings from the investigation indicated that internal oxidation corrosion, driven by high temperatures, was the primary cause of failure. Prolonged exposure to temperatures up to 760 °C resulted in sensitization of the material, making it vulnerable to grain boundary attack. This led to significant deterioration of the grain boundaries, causing extensive grain loss (grain dropping) and the subsequent thinning of sleeve walls. Prior to failure, some portions of the sleeve were only 1.6 mm thick, nearly half their original thickness.

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.

During microscopic examination of a number of cases of caustic cracking, a certain feature has been recognized that appeared to be associated only with caustic cracking. This was a preferential attack on the carbide envelopes and lamellae of the pearlite grains. Evidence suggests that the intergranular path of caustic cracks in steam boilers may be due largely to the presence, probably on a submicroscopic scale, of carbides at the grain boundaries, thus rendering these regions susceptible to preferential attack. It is known that some steels are more liable to develop caustic cracks than others, although their microstructures may not show any significant differences, and it seems probable that this behavior may be related to the amount and continuity of the grain-boundary carbides.

The causes of internal cracking that occurred in 9% Ni steel castings during manufacture were investigated using a series of eight laboratory castings containing varying amounts of molybdenum. The effect of mold thickness was also investigated. The laboratory castings were subjected to three-point bend testing, and fracture surfaces were examined using SEM fractography, metallography, and depth analysis (SIMS) of the fracture surface. The cracks were found to originate at austenitic grain boundaries that coincided with primary dendrite interfaces. The cracking was attributed to a decrease in grain-boundary cohesion resulting from sulfur segregation. Addition of molybdenum proved effective in preventing cracking. The molybdenum promoted MnS precipitation in the grain and preferentially segregated to the interfaces.

Two suction rolls at the first press section of a 25 ft. wide paper machine developed cracks within two years of service. The rolls were austenitic stainless steel castings made of ASTM A 351 Grade CF8M alloy containing molybdenum. The rolls were exposed to slightly acidic white water (pH approximately 4.7) containing chlorides (45 ppm). Visual and liquid penetrant inspections of the rolls revealed extensive cracking at the roll inside surface. The cracks penetrated more than 30 percent of the wall thickness and a few cracks were several inches long. The cracks were preferentially oriented along the roll length and primarily at the roll inside surface. Field metallographic examination showed significant grain boundary chromium-carbide precipitation and intergranular corrosion. The roll failures were attributed to chromium depletion along the grain boundaries (sensitization) resulting from slow cooling of the casting to avoid large residual stresses. The roll manufacturer recommended a proprietary ferritic/austenitic stainless steel as the replacement material for the rolls.

This article describes the visual, fractographic, and metallographic evidence typically encountered when analyzing stress rupture of turbine airfoils. Stress-rupture fractures are generally heavily oxidized, tend to be rough in texture, and are primarily intergranular and/or interdendritic in appearance compared to smoother, transgranular fatigue type fractures. Often, gross plastic yielding is visible on a macroscopic scale. Commonly observed microstructural characteristics include creep voiding along grain boundaries and/or interdendritic regions. Internal voids can also nucleate at carbides and other microconstituents, especially in single crystal castings that do not possess grain boundaries.

A bent Ni-Cu Monel 400 alloy tube, which operated as part of a pipeline in a petrochemical distillery, failed by through-thickness cracking. The pipeline was used to carry a stream of gaseous hydrocarbons containing hydrochloric acid (HCl) into a reaction tower. The tower provided a caustic solution (NaOH) to remove HCl from the stream, before the latter was directed to a burner. Metallographic examination showed that the cracks were intergranular and were frequently branched. Although nominal chemical composition of the component was found within the specified range, energy dispersive x-ray analysis (EDXA) indicated significant segregation of sulfur and chlorine along the grain boundaries. Failure was attributed to hypochlorous-acid (HClO)-induced stress-corrosion cracking (SCC). The HClO was formed by the reaction of HCl with atmospheric O 2 that entered the tube during shutdowns and startups. Residual stresses, originating from in situ bend forming of the tube during assembly of the line, provided a driving force for crack growth, and the segregation of sulfur on grain boundaries made the material more susceptible to cracking.

After only a short time in service, oil-fired orchard heaters made of galvanized low-carbon steel pipe, 0.5 mm (0.020 in.) in thickness, became sensitive to impact, particularly during handling and storage. Most failures occurred in an area of the heater shell that normally reached the highest temperature in service. A 400x etched micrograph showed a brittle and somewhat porous metallic layer about 0.025 mm (0.001 in.) thick on both surfaces of the sheet. Next to this was an apparently single-phase region nearly 0.05 mm (0.002 in.) in thickness. The examination supported the conclusion that prolonged heating of the galvanized steel heater shells caused the zinc-rich surface to become alloyed with iron and reduce the number of layers. Also, heating caused zinc to diffuse along grain boundaries toward the center of the sheet. Zinc in the grain boundaries reacted with iron to form the brittle intergranular phase, resulting in failure by brittle fracture at low impact loads during handling and storage. Recommendation included manufacture of the pipe with aluminized instead of galvanized steel sheet for the combustion chamber.

The outlet-piping system of a steam-reformer unit failed by extensive cracking at four weld locations. The welded system consisted of Incoloy 800 (Fe-32Ni-21Cr-0.05C) pipe and fittings. The exterior surfaces of the system were insulated with rock wool that did not contain weatherproofing. On-site visual examination and magnetic testing indicated severe external corrosion of most of the piping. The system showed extensive cracking in weld HAZ. One specimen indicated that corrosion extended to a depth of 3.2 mm and cracks were seen at the edge of the cover bead and in the HAZ of the weld. Metallographic examination showed that cracking was intergranular and that adjacent grain boundaries had undergone deep intergranular attack. Examination at higher magnification revealed heavy carbide precipitation, primarily at grain boundaries, indicating that the alloy had been sensitized, which resulted from heating during welding. Electron probe x-ray microanalysis showed the outside surface of the tube did not have the protective chromium oxide scale normally found on Incoloy 800. The inside surface of the tube had a thin chromium oxide protective scale. This evidence supported the conclusions that the deep oxidation greatly decreased the strength of the weld HAZ and cracking followed.

Severely reduced wall thickness was encountered at the liquid line of a lead-bath pan that was used in a continuous strip or wire oil-tempering unit. Replacement of the pan was necessary after six months of service. The pan, 6.9 m (22.5 ft) long, 0.6 m (2 ft) wide, and 38 cm (15 in.) deep with a 2.5-cm (1-in.) wall thickness, was a type 309 stainless steel weldment. Operating temperatures of the lead bath in the pan ranged from 805 deg C (1480 deg F) at the entry end to 845 deg C (1550 deg F) at the exit end. Analysis (visual inspection. metallographic analysis, moisture testing, and etched micrographs using Murakami's reagent) supported the conclusions that thinning of the pan walls at the surface of the molten lead resulted from using coke of high moisture content and from the low fluctuating coke level. Recommendations included reducing the supply of oxygen attacking the grain boundaries and the hydrogen that readily promoted decarburization with the use of dry (2 to 3% moisture content) coke. Maintaining a thick layer of coke over the entire surface of molten lead in the pan would exclude atmospheric oxygen from the grain boundaries.