This article discusses the operating principles, advantages, and limitations of scanning electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, and secondary ion mass spectroscopy that are used to analyze the surface chemistry of plastics.

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.

A 140 ft. (42.7 m) long boom on a dragline crane used in coal strip-mining operations failed. One of the principal load-bearing longitudinal beams or chords of the trussed boom had fractured adjacent to a bolt hole at a location about halfway along the length of the boom. Over the lifetime of the crane, several repairs had been made to the boom. At least a year before the failure, a reinforcing gusset plate had been bolted and welded to this chord at this location. Stereomicroscopy revealed microcracks in the weld metal. A fatigue crack 45 mm (1.8 in.) long was observed to emanate from this microcrack. Scanning electron microscopy showed an overload crack extended across the remaining cross section of the chord. It was concluded that the presence of the bolt hole used to attach the gusset plate to the chord created a stress riser adjacent to the hole. Repeated high tensile stresses on the chord during the lifting of enormous loads initiated a fatigue crack in the weld region adjacent to the bolt hole.

Failure analysis of a mobile harbor crane wheel hub that included SEM and EDS analyses demonstrated that the mechanism of failure was fatigue. The wheel hub was a ductile cast iron component that had been subjected to cyclic loading during a ten-year service period. The fracture surface of the fatigue failure also contained corrosion deposit, suggesting that cracking occurred over a period of time sufficient to allow corrosion of the cracked surfaces. Replacement and alignment of the failed wheel hub was recommended along with inspection of the nonfailed wheel hubs that remained on the crane.

A 230 mm (9 in.) thick casing, fabricated from ASTM 235-55 low-carbon steel, of a 450 Mg (500 ton) extrusion press failed after 27 years of service. Initial visual examination revealed an area that exhibited multiple origins and classic beach marks radiating out approximately 75 mm (3 in.) from the origin along the wall of a hydraulic-oil bleed hole. Investigation with a SEM showed corrosion pits along the bleed hole wall, but oxidation and corrosion prevented review of microfractographic details. Vacuum epoxy encapsulation, sectioning of the bleed hole, and metallographic examination revealed a basic microstructure of pearlite and ferrite with bands of slightly finer pearlite, with a large concentration of inclusion stringers in the area of the fracture origin. Further investigation using an energy-dispersive x-ray analyzer showed high concentrations of sulfur and manganese. Thus, the failure appeared to have resulted from corrosion-assisted fatigue, and the inclusion concentration in the fracture-initiated area indicated that the chemical-composition limits for sulfur and manganese would have greatly exceeded material specifications. A higher quality steel was recommended for the replacement unit to lessen the possibility of such gross inclusion segregation and to improve the fracture toughness of the cylinder.

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.

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.

A steel pot used as crucible in a magnesium alloy foundry developed a leak that resulted in a fire and caused extensive damage. Hypotheses as to the cause of the leak included a defect in the pot, overuse, overheating, and poor foundry practices. Scanning electron microscopy, transmission electron microscopy, optical microscopy, and x-ray microanalysis in conjunction with dimensional analysis, phase diagrams and thermodynamics considerations were employed to evaluate the various hypotheses. All evidence pointed to an oxide mass in the area where the hole developed, likely introduced during the steelmaking process.

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.

The US Army Research Laboratory performed a failure investigation on a broken main landing gear mount from an AH-64 Apache attack helicopter. A component had failed in flight, and initially prevented the helicopter from safely landing. In order to avoid a catastrophe, the pilot had to perform a low hover maneuver to the maintenance facility, where ground crews assembled concrete blocks at the appropriate height to allow the aircraft to safely touch down. The failed part was fabricated from maraging 300 grade steel (2,068 MPa [300 ksi] ultimate tensile strength), and was subjected to visual inspection/light optical microscopy, metallography, electron microscopy, energy dispersive spectroscopy, chemical analysis, and mechanical testing. It was observed that the vacuum cadmium coating adjacent to the fracture plane had worn off and corroded in service, thus allowing pitting corrosion to occur. The failure was hydrogen-assisted and was attributed to stress corrosion cracking (SCC) and/or corrosion fatigue (CF). Contributing to the failure was the fact that the material grain size was approximately double the required size, most likely caused from higher than nominal temperatures during thermal treatment. These large grains offered less resistance to fatigue and SCC. In addition, evidence of titanium-carbo-nitrides was detected at the grain boundaries of this material that was prohibited according to the governing specification. This phase is formed at higher thermal treatment temperatures (consistent with the large grains) and tends to embrittle the alloy. It is possible that this phase may have contributed to the intergranular attack. Recommendations were offered with respect to the use of a dry film lubricant over the cadmium coated region, and the possibility of choosing an alternative material with a lower notch sensitivity. In addition, the temperature at which this alloy is treated must be monitored to prevent coarse grain growth. As a result of this investigation and in an effort to eliminate future failures, ARL assisted in developing a cadmium brush plating procedure, and qualified two Army maintenance facilities for field repair of these components.

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.