The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.

Visual examination, optical and scanning electron microscopy were used to determine the cause of failure in the connector groove of a marine riser coupling. The specified steel was AISI 4142 (0.40 to 0.45% C; 0.75 to 1.00% Mn; 0.20 to 0.35% Si; 0.80 to 1.10% Cr; 0.15 to 0.25% Mo) normalized from 9000C. Microscopic examination revealed the crack's initiation point and subsequent propagation. SEM examination of chemically stripped corrosion showed that corrosion fatigue and stress corrosion might have contributed to the initial slow crack growth. Impact tests revealed a fracture transition temperature in excess of 1000C. The sequence of events leading to failure was detailed. The main recommendation was to quench and temper existing couplings and to use a lower carbon quenched and tempered steel for new couplings.

An Incoloy 800H (UNS N08810) transfer line on the outlet of an ethane-cracking furnace failed during decoking of the furnace tubes after nine years in service. A metallographic examination using optical and scanning electron microscopy as well as energy-dispersive x-ray spectroscopy revealed that the failure was due to sulfidation. The source of the sulfur in the furnace effluent was either dimethyl disulfide, injected into the furnace feed to prevent coke formation and carburization of the furnace tubes, or contamination of the feed with sulfur bearing oil.

During a routine inspection on an aircraft assembly line, an airframe attachment bolt was found to be broken. The bolt was one of 12 that attach the lower outboard longeron to the wing carry-through structure. Failure occurred on the right-hand forward bolt in this longeron splice attachment. The bolt was fabricated from PH13-8Mo stainless steel heat treated to have an ultimate tensile strength of 1517 to 1655 MPa (220 to 240 ksi). A water-soluble coolant was used in drilling the bolt hole where this fastener was inserted. Investigation (visual inspection, 265 SEM images, hardness testing, auger emission spectroscopy and secondary imaging spectroscopy, tensile testing, and chemical analysis) supported the conclusion that failure of the attachment bolt was caused by stress corrosion. The source of the corrosive media was the water-soluble coolant used in boring the bolt holes. Recommendations included inspecting for corrosion all the bolts that were installed using the water-soluble coolant at the spliced joint areas, rinsing all machined bolt holes with a noncorrosive agent, and installing new PH13-8Mo stainless steel bolts with a polysulfide wet sealant.

A routine examination on a seat ejection system found that the catapult attachment swivel fabricated from 7075-T651 aluminum alloy plate contained cracks on opposite sides of the part. This swivel, or bath tub, does not experience extreme loads prior to activation of the catapult system. Some loads could be absorbed however, when the aircraft is subjected to G loads. Visual examination of the part revealed that cracks through the wall thickness initiated on the inner walls of the fixture. Scanning electron microscopy (SEM) and electron optical examination revealed that the cracking pattern initiated and progressed by an intergranular failure mechanism. It was concluded that failure of the catapult attachment swivel fixture occurred by SCC. It was recommended that the 7075 aluminum ejection seat fixture be supplied in the T-73 temper to minimize susceptibility to SCC.

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.

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.

A crack was found in an aircraft main wing spar flange fabricated from 7079-T6 aluminum alloy during a routine nondestructive x-ray inspection after the craft had logged 300 h. Scanning electron microscopy (SEM) revealed an intergranular fracture pattern indicative of stress-corrosion cracking (SCC) and fatigue striations near the crack origin. Visual examination of the crack edge revealed that the installation of the fasteners produced a fit up stress. Further inspection of the opened fracture showed that the crack had been present for some time because a heavy buildup of corrosion products was seen on the fractured surface. Metallographic examination of the flange in the area of fracture initiation showed the presence of end grain exposure, which would promote SCC. Electron optical examination of the fracture clearly showed the flange was cracking by a mixed mode of stress corrosion and fatigue. The cracking was accelerated because of an inadvertent fit up stress during installation. The age of the crack could not be established. However, a reevaluation of prior x-ray inspections in this area would result in some close estimate of the age of the crack. End grain exposure further promoted SCC.

Pitostatic system connectors were being found cracked on several aircraft. Two of the cracked connectors made of 2024-T351 aluminum alloy were submitted for failure analysis. The connectors had cut pipelike threads that were sealed with Teflon-type tape when installed. Longitudinal cracks were located near the opening of the female ends of each connector. A cross section showed intergranular cracking with multiple branching in one connector. Scanning electron microscopy (SEM) showed intergranular cracking and separation of elongated grains. A cross section of connector threads showed an incomplete thread form resulting from improper tapping. It was concluded that the pitostatic system connectors failed by SCC. The stress was caused by forcing the improperly threaded female nut over its fully threaded male counterpart to effect a seal. The one connector tested for chemical composition was not made of 2024 aluminum alloy as reported but of 2017 aluminum. It was recommended that the pitostatic system connector manufacturing process be revised to produce full-depth threads rather than pseudo pipe threads. Wall thickness should be increased to increase the hoop stress bearing area if pipe threads were to be used. A determination of proper torque values for tightening the connectors was suggested also.

Examination of a 7075-T6 aluminum alloy pylon strut revealed cracks in two locations on the ears of the strut. Because the part was still intact, the cracks had to be forced open so that the fractures could be examined. Scanning electron microscopy (SEM) of the opened cracks showed that the crack surfaces were covered with a mud crack pattern suggestive of stress-corrosion cracking (SCC). The T6 temper is susceptible to SCC. It was concluded that cracking of the strut could have been aggravated by the hard landing experienced by the aircraft. The strut, however, contained stress-corrosion cracks which were present before the landing. It was recommended that an inspection for SCC be made of all pylon struts with a similar service life.

The floors (fabricated from aluminum alloy 7178-T6 sheet, with portions of the sheet chemically milled to reduce thickness) of the fuel tanks in two aircraft failed almost identically after 1076 and 1323 h of service, respectively. Failure in both tanks occurred in the rear chemically milled section of the floor. An alkaline etch-type cleaner was used on the panels before chemical milling and before painting. Various tests and measurements indicated that the aluminum alloy used for the fuel-tank floors conformed to the specifications for 7178-T6. Low power magnification, fractographs taken with a scanning electron, and optical microscopic examination of the milled sections revealed extensive pitting on both sides of the floors. Evidence found supports the conclusions that the floors failed by fatigue cracking that initiated near the center of the fuel-tank floor and ultimately propagated as rapid ductile-overload fractures. The fatigue cracks originated in pits on the fuel-cell side of the tank floors. The pits were attributed to attack caused by the alkaline-etch cleaning process. Recommendations included monitoring of the alkaline-etch cleaning to avoid the formation of pits and careful inspection following alkaline-etch cleaning, to be scheduled before release of the floor panels for painting.

Four nose wheels fabricated from 2014-T6 aluminum alloy and cold worked at the flange were examined. Visual examination showed that the failure started in the tube well area on the wheel with serial number 31. The failure initiated in the flange fillet on wheels with serial numbers 67, 217, and 250. Scanning electron microscopy (SEM) examination of the fractures showed that failure initiated by SCC or a corrosion pit on all failures examined. The failures then progressed by fatigue. Dye penetrant testing revealed no additional flaws on the wheels that had failed in the flange area. There was, however, one flaw area in the flange of the wheel that failed in the tube well. This flaw resembled a corrosion pit. It was concluded that failure of nose wheels 67, 217, and 250 was caused by cracking due to SCC or pitting. The failures progressed by fatigue. Because failure occurred in the same general area on all three wheels, these locations are suspect as being underdesigned. It was recommended that the nose wheel be redesigned and additional service data be accumulated to understand the contributing factors that resulted in wheel failure.

One main undercarriage axle made of high strength alloy steel was subjected to simulated fatigue test for 6000 h of service. After only 300 h it broke in two along the sharp radius. The fracture revealed a coarse, irregular, and brittle surface before final fracture by thick angular shear lip zone. The presence of micropores in the cleavage facets as well as at the grain boundaries and hairline type crack indications under SEM examination were all suggestive of hydrogen embrittlement. On the basis of investigation results and observations, it was concluded that the transverse breakage of the axle had occurred intergranularly in a brittle manner, possibly, initiated by a shallow zone of fatigue along the sharp radius acting as stress riser.

A large four-engine aircraft was on a cargo flight at night when a loud bang was heard, accompanied by a loss of power from both engines on the left side. After an emergency landing, it was discovered that the propellers from both left side engines were missing. The initial investigation determined that the four-bladed propeller from the left inboard engine had separated in flight, subsequently impacting the left outboard engine, causing its propeller to separate also. Three years later, the left inboard propeller hub was recovered. All four blades had separated through the shank area adjacent to the hub. Detailed SEM examination confirmed a fatigue mode of failure in this area with a primary single origin on the inside surface of the shank. The main fatigue origin site was coincident with one of the defects on the inner surface of the blade shank. The most probable source for creating the defects on the ID bore of the shank was the blade tip chrome plating process, which was carried out during the last overhaul prior to the failure.

Cracking occurred in an ASME SB166 Inconel 600 safe-end forging on a nuclear reactor coolant water recirculation nozzle while it was in service. The safe-end was welded to a stainless-steel-clad carbon steel nozzle and a type 316 stainless steel transition metal pipe segment. An Inconel 600 thermal sleeve was welded to the safe-end, and a repair weld had obviously been made on the outside surface of the safe-end to correct a machining error. Initial visual examination of the safe-end disclosed that the cracking extended over approximately 85 deg of the circular circumference of the piece. Investigation (visual inspection, on-site radiographic inspection, limited ultrasonic inspection, chemical analysis, 53x metallographic cross sections and SEM images etched in 8:1 phosphoric acid) supported the conclusion that the cracking mechanism was intergranular SCC. No recommendations were made.

A crack was discovered in a cast steel (ASTM A 356, grade 6) steam turbine casing during normal overhaul of the turbine. The mechanical properties of the casting all exceeded the requirements of the specification. When the fracture surface was examined visually, an internal-porosity defect was observed adjoining a tapped hole. A second, much larger cavity was also detected. Investigation (visual inspection and 7500x SEM fractographs) supported the conclusions that failure occurred through a zone of structural weakness that was caused by internal casting defects and a tapped hole. The combination of cyclic loading (thermal fatigue), an aggressive service environment (steam), and internal defects resulted in gradual crack propagation, which was, at times, intergranular-with or without corrosive attack-and, at other times, was transgranular.

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.

Two vertical coal-pulverizer shafts at a coal-fired generation station failed after four to five years in service. One shaft was completely broken, and the other was unbroken but cracked at both ends. shaft material was AISI type 4340 Ni-Cr- Mo alloy steel, with a uniform hardness of approximately HRC 27. Metallographic examination of transverse sections through the surface-damaged areas adjacent to the cracks also showed additional small cracks growing at an angle of approximately 60 deg to the surface. The crack propagation mode appeared to be wholly transgranular. SEM examination revealed finely spaced striations on the crack surfaces, supporting a diagnosis of fatigue cracking. Crack initiation in the pulverizer shafts started as a result of fretting fatigue. Greater attention to lubrication was suggested, combined with asking the manufacturer to consider nitriding the splined shaft. It was suggested that the surfaces be securely clamped together and that an in-service maintenance program be initiated to ensure that the tightness of the clamping bolts was verified regularly.

A 75 cm OD x 33 mm thick pipe in a horizontal section of a hot steam reheat line ruptured after 15 years in service. The failed section was manufactured from rolled plate of material specification SA387, grade C. The longitudinal seam weld was a double butt-weld that was V-welded from both sides and failure was found to propagate along the longitudinal seam and its HAZ. The fracture surface near the inner wall of the pipe was found to have a bluish gray appearance, while the fracture surface near the outer wall was rust colored (oxides). The transverse-to-the-weld specimen from the longitudinal seam weld was revealed to have lower elongation and a shear type failure rather than the cup-cone failures. It was concluded that the welded longitudinal seam exhibited embrittlement. A low-ductility intergranular fracture that progressed through the weld metal was revealed by scanning electron microscopy. The cracks were revealed to be in existence for some time before the final failure which was indicated by the extent and amount of corrosion products. It was concluded that low ductility was responsible for the original initiation of cracks in the pipe.

Although a precise understanding of roll failure genesis is complex, the microstructure of a broken roll can often unravel intrinsic deficiencies in material quality responsible for its failure. This is especially relevant in circumstances when, even under a similar mill-operating environment, the failure involves a particular roll or a specific batch of rolls. This paper provides a microstructural insight into the cause of premature breakage of a second-intermediate Sendzimir mill drive roll used at a stainless steel sheet rolling plant under the Steel Authority of India Limited. Microstructural issues influencing roll quality, such as characteristics of carbides, tempered martensite, retained austenite, etc., have been extensively studied through optical and scanning electron microscopy, electron-probe microanalysis, image analysis, and x-ray diffractometry. These are discussed to elucidate specific microstructural inadequacies that accentuated the failure. The study reveals that even through retained austenite content is low (6.29 vol%) and martensite is non-acicular, the roll breakage is a consequence of intergranular cracking caused by improper carbide morphology and distribution.