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.

Diode leads that were to be made from OFHC copper were instead made from copper with high oxygen content. The leads had a nickel underplating, a gold final plating, and were brazed to the diode package in a hydrogen atmosphere. After brazing, the leads became embrittled. SEM examination of the fractured leads revealed voids and some oxidized areas surrounded by ductile fracture areas. High pressure steam pockets observed as voids in the microstructure caused hydrogen embrittlement of the leads. The obvious corrective action was to ensure that the lead material was OFHC copper.

In the EMD-2 Joint Directed Attack Munition (JDAM), the A357 aluminum alloy housing had been redesigned and cast via permanent mold casting, but did not meet the design strength requirements of the previous design. Mechanical tests on thick and thin sections of the forward housing assembly revealed tensile properties well below the allowable design values. Radiology and CT evaluations revealed no casting defects. Optical microscopy revealed porosity uniformly distributed throughout the casting on the order of 0.1 mm pore diam. Scanning electron microscopy revealed elongated pores, which indicated turbulent filling of the mold. Spherical pores would have indicated the melt had been improperly degassed. Based on these findings, it was recommended that the manufacturer analyze and redesign the gating system to eliminate the turbulent flow problem during the permanent mold casting process.

The U-0.8wt%Ti alloy is often used in weapon applications where high strength and fairly good ductility are necessary. Components are immersion quenched in water from the gamma phase to produce a martensitic structure that is amenable to aging. Undesirable conditions occur when a component occasionally cracks during the quenching process, and when tensile specimens fail prematurely during mechanical testing. These two failures prompted an investigative analysis and a series of studies to determine the causes of the cracking and erratic behavior observed in this alloy. Quench-related failures whereby components that cracked either during or immediately after the heat treatment/quenching operation were sectioned for metallographic examination of the microstructure to examine the degree of phase transformation. Examination of premature tensile specimen failures by scanning electron microscopy and X-ray imaging of fracture surfaces revealed pockets of inclusions at the crack origins. In addition, tests were conducted to evaluate the detrimental effects of internal hydrogen on ductility and crack initiation in this alloy.

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.

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.

A cadmium-plated 4340 Ni-Cr-Mo steel ballast elbow assembly was submitted for failure analysis to determine the element or radical present in an oxidation product found inside the elbow assembly. Energy-dispersive x-ray analysis in the SEM showed that iron was the predominant species, presumably in an oxide form. The inside surface had the appearance of typical corrosion products. Hardness measurements indicated that the 4340 steel was heat treated to a strength of approximately 862 MPa (125 ksi). It was concluded that the oxide detected on the ballast elbow was iron oxide. The possibility that the corrosion products would eventually create a blockage of the affected hole was great considering the small hole diameter (4.2 mm, or 0.165 in.). It was recommended that a quick fix to stop the corrosion would be to apply a corrosion inhibitor inside the hole. This, however, would cause the possibility of inhibitor buildup and the eventual clogging of the hole. A change in the manufacturing process to include a cadmium plating on the hole inside surface was recommended. This was to be accomplished in accordance with MIL specification QQ-P-416, Type II, Class 1. A material change to 300-series stainless steel was also recommended.

A failed laser mirror and another complete mirror of the same construction were analyzed. The laser mirror consisted of three layers of material brazed together to form channels through which the cooling water flows. Samples were analyzed with light optical and scanning electron microscopy. The corrosion product contained molybdenum and copper with a trace of gold. The base material was analyzed as molybdenum with negligible alloying additions. The primary mode of corrosion attack on the base material appeared to be intergranular, although uniform corrosion was evident also. It was concluded that corrosion attack sufficiently weakened the base material and the brazed joints, allowing catastrophic failure of the mirror due to the pressure of the cooling water. It was recommended that the mirrors be cleaned of all corrosion products present as a result of past service conditions and proof tested. It was recommended that the water system consisting of deionized water and formaldehyde be replaced with water having a low oxygen content and a cathodic inhibitor (oxygen scavenger).

A component of a water filtration unit failed while being used in service for approximately eight months. The filter system had been installed in a commercial laboratory, where it was stated to have been used exclusively in conjunction with deionized water. The failed part had been injection molded from a 30% glass-fiber and mineral-reinforced nylon 12 resin. Investigation, including visual inspection, 118x SEM images, 9x micrographs, energy-dispersive x-ray spectroscopy, micro-FTIR in the ATR mode, and TGA, supported the conclusion that the filter component failed as a result of molecular degradation caused by the service conditions. Specifically, the part material had undergone severe chemical attack, including oxidation and hydrolysis, through contact with silver chloride. The source of the silver chloride was not established, but one potential source was photographic silver recovery.

Piping and structural components used in space launch facilities such as NASA's Kennedy Space Center and the Air Force's Cape Canaveral Air Station face extreme operating conditions. Launch effluent and residue from solid rocket boosters react with moisture to form hydrochloric acid that settles on exposed surfaces as they are being subjected to severe mechanical loads imparted during lift-off. Failure analyses were performed on 304 stainless steel tubing that ruptured under such conditions, while carrying various gases, including nitrogen, oxygen, and breathing air. Hydrostatic testing indicated a burst strength of 13,500 psi for the intact sections of tubing. Scanning electron microscopy and metallographic examination revealed that the tubing failed due to corrosion pitting exacerbated by stress-corrosion cracking (SCC). The pitting originated on the outer surface of the tube and ranged from superficial to severe, with some pits extending through 75% of the tube's wall thickness. The SCC emanated from the pits and further reduced the service strength of the component until it could no longer sustain the operating pressure and final catastrophic fracture occurred. Corrosion-resistant coatings added after the investigation have proven effective in preventing subsequent such failures.

A failure analysis was conducted on a flow-sensing device that had cracked while in service. The polysulfone sensor body cracked radially, adjacent to a molded-in steel insert. This article describes the investigative methods used to conduct the failure analysis. The techniques utilized included scanning electron microscopy, Fourier transform infrared spectroscopy, differential scanning calorimetry, thermomechanical analysis, and melt flow rate determination. It was the conclusion of the investigation that the part failed via brittle fracture, with evidence also indicating low cycle fatigue associated with cyclic temperature changes from normal service. The design of the part and the material selection were significant contributing factors because of stresses induced during molding, physical aging of the amorphous polysulfone resin, and the substantial differential in coefficients of thermal expansion between the polysulfone and the mating steel insert.

A number of machined end frame steel forgings made of Cr-Si-Mn alloy showed tiny cracks during magnetic particle inspection after heat treatment. The cracks were mostly confined to base edges and fillet radius. No significant abnormality was observed in chemical composition and microstructure. SEM, optical microscopy, and gas analysis revealed that the subsurface discontinuous cracks at the bore edges and in the fillet radius of the heat-treated end frame component had occurred due to hydrogen embrittlement, and not because of faulty heat treatment. This conclusion was supported by the presence of cracklike indications in machined bore surface of the annealed part.

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.

Accelerated aging tests on detonator assemblies, to verify the compatibility of gold bridgewire and Pd-In-Sn solder with the intended explosives, revealed an unusual form of corrosion. The tests, conducted at 74 deg C (165 deg F) and 54 deg C (130 deg F), indicated a preferential attack of the gold. To investigate the problem, a matrix of test units was produced and analyzed. Scanning electron microscopy, EDX analysis, and x-ray diffraction techniques were used to determine the extent of the corrosion and identify the corrosion products. The results indicated that the preferential attack of the gold was due to HCN formed by decomposition of the explosive powder at high temperatures. Other associated reactions were also observed including the subsequent attack of the solder by the gold corrosion product and degradation of the plastic header.

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.

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.