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 splined shaft on a wood chip-to-fiber refiner failed during equipment start-up. The shaft broke into two pieces at a location close to the end of the splined part of the shaft. The failed component showed the classical fatigue-cracking fracture face. The shaft had a diam of approximately 140 mm (5.5 in.) in the unsplined section and was made of 4340 Ni-Cr-Mo alloy steel heat treated to a uniform hardness of HRC 31. Cracks from at least seven different origins had coalesced to produce the single large crack that resulted in failure. The origins of these cracks were on the flanks of the splines. SEM examination revealed the splined shaft failed by fretting fatigue.

The locking collar on a machine failed suddenly when the shaft it restrained was inadvertently subjected to an axial load slightly higher than the allowable working load. The locking collar fractured abruptly, producing four large fragments. This allowed the shaft to be propelled forcefully in the direction of the load, causing substantial damage to other machinery components in the vicinity. The failed component, which was 43 cm (17 in.) in diameter, was machined from 4140 plate and heat treated to 34 to 36 HRC. Analysis (visual inspection, composite micrographs, scanning electron microscopy, and mechanical-property analysis) supported the conclusions that the alloy steel plate used in this application contained significant brittle microstructural fibering or banding. This condition produced considerable anisotropy in ductility and toughness as revealed by mechanical testing. Unfortunately, the potential effects of anisotropy were apparently neglected when this component was designed and manufactured from the plate stock, because the loading was applied in a direction that stressed the weakest planes in the material, that is, a direction normal to the fibering. No recommendations were made.

Majority of the water feeders in a new chicken house had stopped working. The water feeders were found to be operated on the principle that when the chickens pecked a plastic bowl, a compressed spring released a squirt of water. The small compression springs were made from type 302 stainless steel, and the operating stresses were safely within the design limits given by the Goodman diagram. The springs were revealed by scanning electron microscopy to contain numerous cracks on their inside surface, and these cracks were all at 45 deg to the wire axis. The solution was recommended as to select a grade of spring steel that would be more corrosion resistant than 302 stainless.

Ball bearings made of type 440C stainless steel hardened to 60 HRC and suspected as the source of intermittent noise in an office machine were examined. A number of spots on the inner-ring raceway were revealed by scanning electron microscopy. The metal in the area around the spot was evidenced to have been melted and welded to the inner-ring raceway. It was revealed by randomly spaced welded areas on the raceways that the welding was the result of short electrical discharges between the bearing raceways and the balls. The use of an electrically nonconductive lubricant in the bearings was suspected to have caused the electric discharge by accumulation and discharge of static charge. The electrical resistance between the rotor and the motor frame lubricated with electrically conductive grease and the grease used in the current case was measured and compared to confirm the fact the currently used grease was nonconductive. It was concluded that the pits were formed by momentary welding between the ball and ring surfaces. The lubricant was replaced by electrically conductive grease as a corrective measure.

Incorrect grounding of an electric motor resulted in electric current passing through a 52100 steel ball bearing and caused multiple arcing between the rolling elements. The multiple arcing developed a pattern on the outer race known as ‘fluting’. A section of ball race outer showed the distinct banding (fluting) resulting from spark discharges while the bearing was rotating. The severe distress of the surface resulted in unacceptable levels of vibration. An SEM photograph of the banded regions showed smoothing of the asperities from continued operation is evident. In the craters the residue of partial melting was seen.

A steel lifting eye, manufactured from grade 1144 steel, failed during service. The eye ring fractured in two places, adjacent to the threaded shank and diametrically opposite to this region. Woody overload features, typical for resulfurized steels were revealed by SEM. The directionality of the features was found to be suggestive of shear overload. It was observed that fracture preferentially followed the nonmetallic inclusions. The fracture was revealed to be parallel to the direction of the manganese sulfide stringer inclusions. The presence of significant banding of the ferrite and pearlite microstructure was revealed by etching. It was also observed that the fracture is primarily along the inclusions and through bands of ferrite. It was concluded that the lifting eye failed as a result of overload. Fracture occurred parallel to the rolling direction, through manganese-sulfide stringers and ferrite bands in the base metal matrix. The material used for this application was very anisotropic, exhibiting substantially poorer long and short transverse mechanical properties than longitudinal properties.

A 60.3 mm (2.375 in.) diam drive shaft in the drive train of an overhead crane failed. The part submitted for examination was a principal drive shaft that fractured near a 90 deg fillet where the shaft had been machined down to 34.9 mm (1.375 in.) to serve as a wheel hub. A 9.5 mm (0.375 in.) wide x 3.2 mm (0.125 in.) deep keyway was machined into the entire length of the hub, ending approximately 1.6 mm (0.062 in.) away from the 90 deg fillet. A second shaft was also found to have cracked at a change in diameter, where it was machined down to serve as the motor drive hub. Investigation (visual inspection, inspection records review, optical and scanning electron microscopy, and fractography) supported the conclusion that the fracture mode for both shafts was low-cycle rotating-bending fatigue initiating and propagating by combined torsional and reverse bending stresses. Recommendations included replacing all drive shafts with new designs that eliminated the sharp 90 deg chamfers in favor of a more liberal chamfer, which would reduce the stress concentration in these areas.

Proper stress analysis during component design is imperative for accurate life and performance prediction. The total stress on a part is comprised of the applied design stress and any residual stress that may exist due to forming or machining operations. Stress-corrosion cracking may be defined as the spontaneous failure of a metal resulting from the combined effects of a corrosive environment and the effective component of tensile stress acting on the structure. However, because of the orientation dependence in aluminum, it is the residual stress occurring in the most susceptible direction that must be considered of primary importance in material selection for design configuration. A Navy UH-1N helicopter main rotor blade grip manufactured from a 2014-T6 aluminum alloy forging failed because of a design flaw that left a high residual tensile stress along the short transverse plane; this in turn provided the necessary condition for stress corrosion to initiate. A complete failure investigation to ascertain the exact cause of the failure was conducted utilizing stereomicroscopic examination, scanning electron microscopy, metallographic inspection and interpretation, energy-dispersive chemical analysis, physical and mechanical evaluation. Stereomicroscopic examination of the opened crack fracture surface revealed one large fan-shaped region that had propagated radially through the thickness of the material from two distinct origin areas on the internal diam of the grip. Higher magnification inspection near the origin area revealed a flat, wood-like appearance. Scanning electron microscopy divulged the presence of substantial mud cracking and intergranular separation on the fracture surface. Metallographic examination revealed intergranular cracking and substantial leaf separation along the elongated grains parallel to the fracture surface. Chemical composition and hardness requirements were found to be as specified. The blade grip failed due to a stress corrosion crack which initiated on the inner diam and propagated in the short transverse direction through the thickness of the component. The high residual tensile stress in the part resulting from the forging and exposed after machining of the inner diam, combined with the presence of moisture, provided the necessary conditions to facilitate crack initiation and propagation.

Suspension lugs fabricated from AISI 4340 steel used to facilitate loading of bombs onto the underside of military aircraft could not sustain required loads during routine proof load testing. Three failed lugs underwent visual examination, chemical analysis, metallography, hardness testing, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. It was determined that the failures were due to forging defects. Both forging laps and seams acted as stress concentrators when the lugs were loaded during proof testing.

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 cast steel bracket manufactured in accordance with ASTM A 148 grade 135/125 steel failed in railroad maintenance service. Ancillary property requirements included a 285 to 331 HB hardness range and minimum impact energy of 27 J (20 ft·lbf) at -40 deg C (-40 deg F). The conditions at the time of failure were characterized as relatively cold. Investigation (visual inspection, chemical analysis, and unetched 119x and 2% nital etched 119x SEM images) supported the conclusion that the bracket failed through brittle overload fracture due to a number of synergistic factors. The quenched-and-tempered microstructure contained solidification shrinkage, inherently poor ductility, and type II Mn-S inclusions that are known to reduce ductility. The macro and microscale fracture features confirmed that the casting was likely in low-temperature service at the time of failure. The composition and mechanical properties of the casting did not satisfy the design requirements. Recommendations included exerting better composition control, primarily with regard to melting, deoxidation, and nitrogen control. Better deoxidation practice was recommended to generate the more desirable Mn-S inclusion morphology, and reevaluation of the casting design was suggested to minimize shrinkage.

Grease-wiper springs for cams formed from stampings of 0.25-mm thick carbon spring steel (0.65 to 0.80% C) fractured at the 0.025 mm radius on the stamped 135 deg corner at a 90 deg bend after 5,000,000 cycles. Tool marks 2 to 2.3 mm from the center of the stamped bend were disclosed by visual examination. Fatigue striations originating from cracks at the 0.025 mm radius inside corner at the bend were revealed by SEM of the fractured surface. The maximum stress at the bend, in stock of maximum thickness and as a function of the radius of the 135 deg corner, was indicated by stress calculations to be very close to the maximum allowable fluctuating stress for the material. The wiper springs were concluded to be fractured in fatigue and the cyclic loading resulted from cam rotation. The maximum applied stress approached the allowable limit due to high stress-concentration factor in the spring (caused by the very small inside radius). The corner radius was increased to 0.76 mm and the tools were re-polished to avoid tool marks.

Alloy steel forgings used as structural members of a ski chair lift grip mechanism were identified to have contained forging laps (i.e., sharp-notched discontinuities) during an annual magnetic particle inspection of all chair lift grip structural members at a mountain resort. The material was confirmed to be 34Cr-Ni-Mo6. A heavy oxide on the dark area of one of the broken-open laps was revealed by scanning electron microscopy in conjunction with EDS. A bright area that contained ductile dimple rupture was observed adjacent to the dark area. The oxidized portion of the fracture was established to be the preexisting forging lap while the bright area was created during the breaking-open process. As a corrective action all forgings showing laps were recommended to be removed from service. Critical review and revision of the forging process and revisions to the nondestructive evaluation procedures at the forging supplier was recommended.

A welded ferritic stainless steel heat exchanger cracked prior to service. The welding filler metal was identified as an austenitic stainless steel and the joining method as gas tungsten arc welding. Investigation (visual inspection, SEM images, 5.9x images, and 8.9x/119x images etched with Vilella's reagent followed by electrolytic etching in 10% oxalic acid) supported the conclusion that the heat exchanger cracked due to weld cold cracking or postwelding brittle overload that occurred via flexure during fabrication. The brittle nature of the weld was likely due to a combination of high residual stresses, a mixed microstructure, inclusions, and gross grain coarsening. These synergistic factors resulted from extreme heat input during fillet welding. Recommendations included altering the welding variables such as current, voltage, and travel speed to substantially reduce the heat input.

Parts of 21Cr-6Ni-9Mn stainless steel that had been forged at about 815 deg C (1500 deg F) were gas tungsten arc welded. During postweld inspection, cracks were found in the HAZs of the welds. Welding had been done using a copper fixture that contacted the steel in the area of the HAZ on each side of the weld but did not extend under the tungsten arc. In SEM examination, the cracks appeared to be intergranular and extended to a depth of approximately 1.3 mm (0.05 in.). The crack appearance suggested that the surface temperature of the HAZ could have melted a film of copper on the fixture surface and that this could have penetrated the stainless steel in the presence of tensile thermal-contraction stresses. The cracks in the weldments were a form of liquid-metal embrittlement caused by contact with superficially melted copper from the fixture and subsequent grain-boundary attack of the stainless steel in an area under residual tensile stress. The copper for the fixtures was replaced by aluminum. No further cracking was encountered.

An AISI 4340 threaded steel connecting rod that was part of a connecting linkage used between a parachute and an instrumented drop test assembly fractured under high dynamic loading when the assembly was dropped from an airplane. A large flaw that originated from the root of a machined thread groove was visible on the fracture surface. Heavy oxidation at elevated temperatures was indicated as most of the surface of the flaw was black. Fine secondary cracks aligned transverse to the growth direction was revealed by scanning electron microscopy. It was established that intergranular cracking observed in this alloy was caused during heat treating as the thread root served as an effective stress concentration and induced quench cracking. It was found that fracture in the overload region occurred by a ductile void growth and coalescence process. Premature failure of the threaded rod was thus attributed to the presence of the quench crack flaw caused by an improper machining sequence and heat treatment practice.