This article provides a discussion on the metallographic techniques used for failure analysis, and on fracture examination in materials, with illustrations. It discusses various metallographic specimen preparation techniques, namely, sectioning, mounting, grinding, polishing, and electrolytic polishing. The article also describes the microstructure examination of various materials, with emphasis on failure analysis, and concludes with information on the examination of replicas with light microscopy.

Metallographic examination is one of the most important procedures used by metallurgists in failure analysis. Typically, the light microscope (LM) is used to assess the nature of the material microstructure and its influence on the failure mechanism. Microstructural examination can be performed with the scanning electron microscope (SEM) over the same magnification range as the LM, but examination with the latter is more efficient. This article describes the major operations in the preparation of metallographic specimens, namely sectioning, mounting, grinding, polishing, and etching. The influence of microstructures on the failure of a material is discussed and examples of such work are given to illustrate the value of light microscopy. In addition, information on heat-treatment-related failures, fabrication-/machining-related failures, and service failures is provided, with examples created using light microscopy.

Diagnosis of environmentally induced failures is greatly facilitated by metallographic analysis. As an example, a failure analysis of ASTM A574 material grade bolts is presented. The bolts served as bonnet screws in underground valves and failed due to stress-corrosion cracking. Metallographic methods were used to diagnose and provide solutions for the service failure. Included are photos showing crack propagation morphology and fracture surface appearance.

This article commences with a discussion on the characteristics of stress-corrosion cracking (SCC) and describes crack initiation and propagation during SCC. It reviews the various mechanisms of SCC and addresses electrochemical and stress-sorption theories. The article explains the SCC, which occurs due to welding, metalworking process, and stress concentration, including options for investigation and corrective measures. It describes the sources of stresses in service and the effect of composition and metal structure on the susceptibility of SCC. The article provides information on specific ions and substances, service environments, and preservice environments responsible for SCC. It details the analysis of SCC failures, which include on-site examination, sampling, observation of fracture surface characteristics, macroscopic examination, microscopic examination, chemical analysis, metallographic analysis, and simulated-service tests. It provides case studies for the analysis of SCC service failures and their occurrence in steels, stainless steels, and commercial alloys of aluminum, copper, magnesium, and titanium.

A femoral knee implant was returned to the casting vendor for analysis after exhibiting poor bond strength between the cast substrate and a sintered porous coating. Both the coating and the substrate were manufactured from a cobalt-chromium-molybdenum alloy. Metallographic analysis indicated that a decarburized layer existed on all surfaces of the casting, which prevented bonding during the sintering thermal cycle. Bead-to-bead bonding within the coating appeared sufficient, and no decarburized layer was present on the bead surfaces. It was concluded that the decarburization did not occur during the sintering thermal cycle. It was recommended that the prosthetic manufacturer investigate atmosphere controls for all thermal cycles prior to coating.

A thick-walled tube that was weld fabricated for use as a pressure vessel exhibited cracks. Similar cracking was apparent at the weld toes after postweld stress relief or quench-and-temper heat treatment. The cracks were not detectable by nondestructive examination after welding, immediately prior to heat treatment. Multiple-pass arc welds secured the carbon-steel flanges to the Ni-Cr-Mo-V alloy steel tubes. Investigation (visual inspection, metallographic analysis, and evaluation of the fabrication history and the analysis data) supported the conclusion that the tube failed as a result of stress-relief cracking. Very high residual stresses often result from welding thick sections of hardenable steels, even when preheating is employed. Quenched-and-tempered steels containing vanadium, as well as HSLA steels with a vanadium addition, have been shown to be susceptible to this embrittlement. Manufacturers of susceptible steels recommend use of these materials in the as-welded condition.

Hydraulic cylinder housings were being fabricated from 4140 grade seamless steel tubing. During production, magnetic-particle inspection indicated the presence of circumferential and longitudinal cracks in a large number of cylinders. Analysis (visual inspection, dye penetrant inspection, 50x/90x/400x SEM micrographs, and metallographic analysis) supports the conclusion that the cracking problem in these components was identified as quench cracks due to their brittle, intergranular nature and the characteristic temper oxide on the fracture surfaces. Although the steel met the compositional requirements of SAE 4140, the sulfur level was 0.022% and would account for the formation of the sulfide stringers observed. Apparently, the combination of the clustered, stringer-type inclusions and the quenching conditions were too severe for this component geometry. The result was a high incidence of quench cracks that rendered the parts useless. Recommendations included changing the specification, requiring the steel to have lower sulfur concentrations. Magnetic-particle cleanliness standards should be imposed that will exclude material with harmful clusters of sulfide stringers, for example, modified AMS 2301.

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.

Linear indications on the outer surface of a cross in a piping system were revealed by dye-penetrant examination. The cross was specified to be SA403 type WP 304 stainless steel. The cross had been subjected to induction-heating stress improvement. The linear indications on the cross were located in wide bands running circumferentially below the cross-to-cap weld and above the cap-to-discharge-pipe weld. The material was found to conform to the requirements both in terms of hardness and strength. Intergranular cracks filled with oxide were observed on metallographic analysis of a sectioned and oxalic acid etched sample. The grain size was found to exceed the ASTM standard. No indications of sensitization were observed during testing with practice A of ASTM A 262. Definitive evidence of contaminants to support SCC as the failure mechanism was not disclosed during analysis. It was concluded that overheating or burning of the forging, which classically results in large grain size, intergranular fractures, and fine oxide particles dispersed throughout the grains was the possible reason for the failure.

Rotor blades in the compressor section of a J79 engine had failed. Optical, stereoscopic, microhardness testing, and SEM examinations were conducted to determine the cause. The blades were made of STS403 and were used uncoated. They were damaged over an extensive area, from the 15th through the 17th compressor stages, as were stator vanes and casing sections. The fractured surface of the 17th blade showed multiple origins along with secondary cracking and extensive propagation that preceded separation. The metallographic analysis of the microstructure suggested work hardening. Based on the results, the cause of the fractured blade was high-amplitude fatigue due to severe stall. After normal engine usage of five months, the blade fractured sending fragments throughout the combustion and turbine sections.

A steel splice plate in a power transmission line tower cracked while in service. Metallographic analysis indicated the presence of a white hard martensite layer near the crack, which occurred in the heel of the plate. Mechanical property tests revealed localized hardening in the area of the crack, supporting the metallurgical findings. A substantial deterioration of the Charpy impact toughness of the material in the heel region was also observed which is believed to have caused the initiation and propagation of the cracks leading to the failure.

Two complete aircraft undercarriage-leg 2014 aluminum alloy forgings and a number of sectional ends that exhibited cracks during nondestructive testing were examined to determine the extent of damage and the type of cracking. Cracks were primarily confined to the diaphragm and adjoining wall between the steel sleeve and the steel diaphragm washer. Metallographic analysis and accelerated corrosion tests showed that the cracks had originated as stress-corrosion failures.

A type 316 stainless steel pipe reducer section failed in service of bleached pulp stock transfer within 2 years in a pulp and paper mill. The reducer section fractured in the heat-affected zone of the flange-to-pipe weld on the flange side. The pipe reducer section consisted of 250 and 200 mm (10 and 8 in.) diam flanges welded to a tapered pipe section. The tapered pipe section was 3.3 mm (0.13 in.) thick type 316 stainless steel sheet, and the flanges were 5 mm (0.2 in.) thick CF8M (type 316) stainless steel castings. Visual and metallographic analysis indicated that the fracture was caused by intergranular corrosion/stress-corrosion cracks that initiated from the external surface of the pipe reducer section. Contributory factors were the sensitized condition of the flange and the concentration of corrosive elements from the bleach stock plant environment on the external surface. In the absence of the sensitized condition of the flange, the service of the pipe reducer section was acceptable. A type 316L stainless steel reducer section was recommended to replace the 316 component because of its superior resistance to sensitization.

An aluminum bronze propeller tap bolt from a twin-screw vessel fractured just below the bolt head. Liquid penetrant testing revealed a large network of cracks that extended radially from sites in and just below the bolthead. Metallographic analysis indicated that the tap bolt failed by stress-corrosion cracking. It was surmised that seawater or some other corrosive substance was present in sufficient quantity to induce intergranular cracking at regions of high stress concentration. It was recommended that all tap bolts be replaced with new bolts made from an alloy with a higher copper content and at least the same yield strength. Steps to exclude seawater and any possible source of ammonia from the bolt shank were also suggested.

Two failures of AP15A grade J-55 electric resistance welded (ERW) tubing in as our gas environment were investigated. The first failure occurred after 112 days of service. Replacement pipe failed 2 days later. Surface examination of the failed tubing indicated that fracture initiated at the outside surface. Metallographic analysis showed that the fracture originated in the upturned fibers adjacent to the ERW bond line. Cross sections of the weld were removed from three random locations in the test sample. At each location, the up turned fibers of the weld zone contained bands of hard-appearing microstructure. Hardness measurements confirmed these observations. The cracks followed these bands. It was concluded that the tubing failed from sulfide stress cracking, which resulted from bands of susceptible microstructure in the ERW zone. The banded microstructure in the pipe suggested that chemical segregation contributed to the hard areas. Postweld normalized heat treatment apparently did not sufficiently reduce the hardness of these areas.

Two hot water reheat coil valves from a heating/ventilating/air-conditioning system failed in service. The values, a 353 copper alloy 19 mm (3/4 in.) valve and a 360 copper alloy 13 mm (1/2 in.) valve, had been failing at an increasing rate. The failures were confined to the stems and seats. Visual examination revealed severe localized metal loss in the form of deep grooves with smooth and wavy surfaces. Metallographic analysis of the grooved areas revealed uniform metal loss. No evidence of intergranular or selective attack indicating erosion-corrosion was observed, Recommendations included use of a higher-copper brass, cupronickel, or Monel for the valve seats and stems and operation of the valves in either the fully opened or closed position.

Three sprinkler system dry pipe valve castings (class 30 gray iron), two that had failed in service and one that had been rejected during machining because of porosity, were submitted for examination. The two failures consisted of cracks in a seating face. All three were from the same heat. Visual examination showed that the casting had cracked through a thin area in the casting sidewall. Evidence of a sharply machined corner at the fracture site was also discovered. Tensile testing and metallographic analysis revealed no metallurgical cause for the failure. It was recommended that the manufacturer work with the foundry to evaluate the criticality of core placement and to eliminate the undesired thin section.

Several nickel-base superalloy (UNS N06600) welded heat-exchanger tubes used in processing black liquor in a kraft paper mill failed prematurely. Leaking occurred through the tube walls at levels near the bottom tube sheet. The tubes had been installed as replacements for type 304 stainless steel tubes. Visual and stereoscopic examination revealed three types of corrosion on the inside surfaces of the tubes: uniform attack, deeper localized corrosive attack, and accelerated uniform attack. Metallographic analysis indicated that pronounced dissimilar-metal corrosion had occurred in the base metal immediately adjacent to the weld seam. The corrosion was attributed to exposure to nitric acid cleaning solution and was accelerated by galvanic differences between the tubes and a stainless steel tube sheet and between the base metal of the tubes and their dendritic weld seams. A change to type 304 stainless steel tubing made without dendritic weld seams was recommended.

Several type 304L stainless steel dished ends used in the fabrication of cylindrical vessels developed extensive cracking during storage. All of the dished ends had been procured from a single manufacturer and belonged to the same batch. When examined visually, several rust marks were observed, indicating contamination by rusted carbon steel particles. Liquid penetrant testing was used to determine the extent of the cracks, and in situ metallographic analysis was performed over the cracked region. The morphology of the cracks was indicative of transgranular stress-corrosion cracking (TGSCC). Conditions promoting the occurrence of the TGSCC included significant tensile stresses on the inside of the dished ends, the presence of surface contamination by iron due to poor handling practice using carbon steel implements, and storage in a coastal environment with an average temperature of 25 to 32 deg C (77 to 90 deg F), an average humidity ranging from 70 to 80%, and an atmospheric NaCl content ranging from 8 to 45 mg/m2 /day. Recommendations preventing further occurrence of the situation were strict avoidance of the use of carbon steel handling implements, strict avoidance of cleaning practices that cause long-term exposure to chlorine-containing cleaning fluid, and solution annealing of the dished ends at 1050 deg C (1920 deg F) for 1 h followed by water quenching to relieve residual stresses.

Rupture occurred at a bend in a superheated steam transfer line between a header and a desuperheater of a boiler producing 230 t/h of steam at 540 deg C and 118 kPa. The boiler had operated for 77,000 h. Rupture occurred along the outer bend radius of the 168 mm diam tube, this being of 1 Cr, 0.5 Mo steel with a wall thickness of 14 mm. The design temperature of this tube was 490 deg C, but there is evidence that it was operating at a temperature much above 500 deg C. Metallographic analysis disclosed an advanced stage of creep damage accumulation in the form of local cracks, microcracks, and aligned damage centers which showed up as voids upon repeated polish-etch cycles. Because of the local nature of creep damage that can occur, any inspection that involves in situ metallography must be conducted at exactly the right or critical position or the presence of damage may not be detected.