A study of the delamination behavior of a very low-carbon steel

Splitting,i.e., delamination behavior in Charpy specimens of low-carbon steel was found to be caused by cracks propagating between pancake grains parallel to the rolling plane of the as-rolled plate. The results suggest the mechanism is a decohesion of grain boundaries that is independent of the texture of the material. The number of splits increased with decreasing finishing temperature and impact test temperature. The energy absorbed in impact testing was inversely proportional to the number of splits. In specimens annealed after rolling splitting was evident until the material was almost completely recrystallized.     

Hydrogen Absorption and Desorption during Heat Treatment of AISI 4140 Steel

Hydrogen plays an important role in the formation of quench cracks of structural steels. To clarify hydrogen ab- sorption and desorption during heat treatment of AISI 4140 steel, thermal desorption spectrometry （TDS） analysis was carried out for the specimens in the as-rolled, as quenched, and quenched and tempered conditions. Results show that hydrogen content increased from 0. 127 ×10 6 in the as-rolled specimen to 0. 316 × 10-6 in the as-oil-quenched specimen. After tempering at 200 ℃, the hydrogen content in the oil-quenched specimen decreased to 0. 155 × 10-6 , and the peak temperature of hydrogen desorption increased from 200 to 360 ℃. From the dependence of hydrogen content in the as-quenched specimens on austenitizing time, it can be deduced that hydrogen absorption occurs during austenitizing. The simulation of hydrogen absorption contributes to a better understanding on the distribution of hy- drogen during the heat treatment in structural steels.     

Quench embrittlement of hardened 5160 steel as a function of austenitizing temperature

Charpy V-notch (CVN) specimens from experimental heats of 5160 steel containing 0.001 and 0.034 mass pct phosphorus were austenitized at temperatures between 830 °C and 1100 °C, quenched to martensite, and tempered at temperatures between 100 °C and 500 °C. Scanning electron microscopy (SEM) was used to characterize the fracture surfaces of tested CVN specimens and carbide formation on prior austenite grain boundaries. Quench embrittlement, the susceptibility to intergranular fracture in as-quenched and low-temperature tempered high-carbon steels due to cementite formation as affected by phosphorus segregation on austenite grain boundaries, developed readily in specimens of the high phosphorus steel austenitized at all temperatures. The low phosphorus steel developed quench embrittlement only after austenitizing at 1100 °C. Intergranular fractures correlated with low room-temperature CVN impact toughness. The results are discussed with respect to the dissolution of carbides during austenitizing and the effect of phosphorus on grain boundary, carbide formation, and stability.     

The tensile properties of an Fe-4 pct Mo-0.2 pct C martensite tempered under applied stress

In Fe-4 pct Mo-0.2 pct C martensite which is a typical secondary hardening steel, premature failure o°Curred in tensile test at 600 °C to 700°C where solute atoms could diffuse easily. To clarify this phenomenon, the quenched specimens were tempered under applied stress and tensile-tested at room temperature. The following results were obtained: (1) Typical intergranular fracture was observed in specimens tempered in a temperature range of 600 °C to 650 °C with tempering times of five minutes to 10 minutes and applied stress (70 MPa to 140 MPa). (2) Based on Auger analysis, this phenomenon was considered to be caused by segregation of P, S, and Mo on prior austenite grain boundaries due to applied stress. (3) The direction of applied stress was found to be very significant. Namely, when the tensile direction was parallel to the applied stress during tempering, the specimen was more brittle, and when tensile direction was normal to the applied stress, the specimen was not so brittle. (4) To reduce this embrittlement, solution treatment temperature was adjusted, and it was found that the embrittlement was considerably reduced both in specimens with fine prior austenite grains and with some ferrite phase on prior austenite grain boundaries. TAKATOSHI OGAWA, formerly with Kyoto University. YOSHIFUMI OHMURA, formerly with Kyoto University. This paper is based on a presentation made at the “pcter G. Winchell Symposium on Tempering of Steel” held at the Louisville Meeting of The Metallurgical Society of AIME, October 12-13, 1981, under the sponsorship of the TMS-AIME Ferrous Metallurgy and Heat Treatment Committees.     

The Tensile Properties of an Fe-4 Pct Mo-0.2 Pct C Martensite Tempered under Applied Stress

In Fe-4 pct Mo-0.2 pct C martensite which is a typical secondary hardening steel, premature failure occurred in tensile test at 600 °C to 700 °C where solute atoms could diffuse easily. To clarify this phenomenon, the quenched specimens were tempered under applied stress and tensile-tested at room temperature. The following results were obtained: (1) Typical intergranular fracture was observed in specimens tempered in a temperature range of 600 °C to 650 °C with tempering times of five minutes to 10 minutes and applied stress (70 MPa to 140 MPa). (2) Based on Auger analysis, this phenomenon was considered to be caused by segregation of P, S, and Mo on prior austenite grain boundaries due to applied stress. (3) The direction of applied stress was found to be very significant. Namely, when the tensile direction was parallel to the applied stress during tempering, the specimen was more brittle, and when tensile direction was normal to the applied stress, the specimen was not so brittle. (4) To reduce this embrittlement, solution treatment temperature was adjusted, and it was found that the embrittlement was considerably reduced both in specimens with fine prior austenite grains and with some ferrite phase on prior austenite grain boundaries. Formerly with Kyoto University Formerly with Kyoto University This paper is based on a presentation made at the “Peter G. Winchell Symposium on Tempering of Steel” held at the Louisville Meeting of The Metallurgical Society of AIME, October 12-13, 1981, under the sponsorship of the TMS-AIME Ferrous Metallurgy and Heat Treatment Committees.     

Delamination Effect on Impact Properties of Ultrafine-Grained Low-Carbon Steel Processed by Warm Caliber Rolling

Bulk ultrafine-grained (UFG) low-carbon steel bars were produced by caliber rolling, and the impact and tensile properties were investigated. Initial samples with two different microstructures, ferrite-pearlite and martensite (or bainite), were prepared and then caliber rolling was conducted at 500 °C. The microstructures in the rolled bars consisted of an elongated UFG structure with a strong α-fiber texture. The rolled bar consisting of spheroidal cementite particles that distributed uniformly in the elongated ferrite matrix of transverse grain sizes 0.8 to 1.0 μm exhibited the best strength-ductility balance and impact properties. Although the yield strength in the rolled bar increased 2.4 times by grain refinement, the upper-shelf energy did not change, and its value was maintained from 100 °C to −40 °C. In the rolled bars, cracks during an impact test branched parallel to the longitudinal direction of the test samples as temperatures decreased. Delamination caused by such crack branching appeared, remarkably, near the ductile-to-brittle transition temperature (DBTT). The effect of delamination on the impact properties was associated with crack propagation on the basis of the microstructural features in the rolled bars. In conclusion, the strength-toughness balance is improved by refining crystal grains and controlling their shape and orientation; in addition, delamination effectively enhances the low-temperature toughness.     

Hydrogen Embrittlement of a 1500-MPa Tensile Strength Level Steel with an Ultrafine Elongated Grain Structure

A deformation of a tempered martensitic structure (i.e., tempforming) at 773 K (500 °C) was applied to a 0.6 pct C-2 pct Si-1 pct Cr steel. The hydrogen embrittlement (HE) property of the tempformed (TF) steel was investigated by a slow strain rate test (SSRT) and an accelerated atmospheric corrosion test (AACT). Hydrogen content within the samples after SSRT and AACT was measured by thermal desorption spectrometry (TDS). The tempforming at 773 K (500 °C) using multipass caliber rolling with an accumulative are reduction of 76 pct resulted in the evolution of an ultrafine elongated grain (UFEG) structure with a strong 〈110〉//rolling direction (RD) fiber deformation texture and a dispersion of spheroidized cementite particles. The SSRT of the pre-hydrogen-charged notched specimens and the AACT demonstrated that the TF sample had superior potential for HE resistance to the conventional quenched and tempered (QT) sample at a tensile strength of 1500 MPa. The TDS analysis also indicated that the hydrogen might be mainly trapped by reversible trapping sites such as grain boundaries and dislocations in the TF sample, and the hydrogen trapping states of the TF sample were similar to those of the QT sample. The QT sample exhibited hydrogen-induced intergranular fracture along the boundaries of coarse prior-austenite grains. In contrast, the hydrogen-induced cracking occurred in association with the UFEG structure in the TF sample, leading to the higher HE resistance of the TF sample.     

Tempered martensite embrittlement in SAE 4340 steel

The toughness of SAE 4340 steel with low (0.003 wt pct) and high (0.03 wt pct) phosphorus has been evaluated by Charpy V notch (CVN) impact and compact tension plane strain fracture toughness (K _1c) tests of specimens quenched and tempered up to 673 K (400°C). Both the high and low P steel showed the characteristic tempered martensite embrittlement (TME) plateau or trough in room temperature CVN impact toughness after tempering at temperatures between 473 K (200°C) and 673 K (400°C). The CVN energy absorbed by low P specimens after tempering at any temperature was always about 10 J higher than that of the high P specimens given the same heat treatment. Interlath carbide initiated cleavage across the martensite laths was identified as the mechanism of TME in the low P 4340 steel, while intergranular fracture, apparently due to a combination of P segregation and carbide formation at prior austenite grain boundaries, was associated with TME in the high P steel.K _IC values reflected TME in the high P steels but did not show TME in the low P steel, a result explained by the formation of a narrow zone of ductile fracture adjacent to the fatigue precrack during fracture toughness testing. The ductile fracture zone was attributed to the low rate of work hardening characteristic of martensitic steels tempered above 473 K (200°C).     

Effect of Heat Treatment on Microstructure and Mechanical Properties of API X90 Pipeline Steel Welded Joints

In this work, X90 pipeline steel was welded by shielded metal arc welding with root and submerged arc welding with calk and cap. After that, the joint was tempered at 550 °C and 600 °C. Subsequently, the microstructure and mechanical properties were investigated by optical microscope, scanning electron microscope (SEM) and Vickers hardness tester. The fracture surface of welded joint was analyzed by SEM. The experiments show that: After high-temperature tempering treatment, the Widmanstatten structure disappears in coarse-grained region. The number of lath martensite in the original structure of the welded joint decreases, and the quantity of granular bainite increases. The acicular ferrite disappears gradually and the polygonal ferrite grains increase, and the M/A island components decompose into fine grains with the increase in tempering temperature. The mechanical properties of the joints also change and the hardness rises because of the disappearance of Widmanstatten structure improves after heat treatment, and yield strength and tensile strength of the specimens have the lowest values after tempering at 550 °C. After tempering at 600 °C, the hardness decreases and strength–ductility reaches 11,571 MPa%. The tensile fracture of 600 °C sample presents delamination and ductile fracture. Through comparative analysis, it can be concluded that the plasticity and toughness of multilayer welded joints after tempering at 600 °C is improved, and they have better comprehensive mechanical properties.

     

Effect of Aluminum Content on the Microstructure and Mechanical Properties of Hypereutectoid Steels

Hypereutectoid steels with 0, 0.69, 1.29, and 1.95 wt pct aluminum were prepared. The samples were hot rolled at 1100 °C followed by cooling in air. The microstructure of the as-rolled samples was characterized using field emission–scanning electron microscopy (FE-SEM). The electron backscattered diffraction (EBSD) technique was used to identify the grain boundary phases. The steels have a pearlitic microstructure with different amounts of grain boundary cementite. A continuous grain boundary cementite network is present in the 0 wt pct Al steel. Grain boundary cementite formation is completely suppressed in the 1.29 wt pct Al steel. Phase diagram calculations show that aluminum increases the eutectoid temperature. However, the interlamellar spacing and pearlite colony size decrease with increase in aluminum content. Dilatometry measurements show that aluminum addition increases the undercooling below the eutectoid temperature. The yield strength increases with the decrease in interlamellar spacing and colony size. Very high ultimate tensile strengths (1200 to 1400 MPa) and improved elongations to failure (7 to 9 pct) are achieved in the as-rolled condition.     

Wear Behavior and Mechanism of a Cr-Mo-V Cast Hot-Working Die Steel

The wear behavior and mechanisms of a Cr-Mo-V cast hot-working die steel with three microstructures (tempered martensite, troostite, and sorbite) were studied systematically through the dry-sliding wear tests within a normal load range of 50 to 300 N and an ambient temperature range of 298 K to 673 K (25 °C to 400 °C) by a pin-on-disk high-temperature wear machine. Five different mechanisms were observed in the experiments, namely adhesive, abrasive, mild oxidative, oxidative, and extrusive wear; one or more of those mechanisms would be dominant within particular ranges of load and temperature. The transition of wear mechanisms depended on the formation of tribo-oxides, which was related closely to load and temperature, and their delamination, which was mainly influenced by the matrix. By increasing the load and ambient temperature, the protective effect of tribo-oxides first strengthened, then decreased, and in some cases disappeared. Under a load ranging 50 to 300 N at 298 K (25 °C) and a load of 50 N at 473 K (200 °C), adhesive wear was the dominant wear mechanism, and abrasive wear appeared simultaneously. The wear was of mild oxidative type under a load ranging 100 to 300 N at 473 K (200 °C) and a load ranging 50 to 150 N at 673 K (400 °C) for tempered martensite and tempered troostite as well as under a load of 100 N at 473 K (200 °C) and a load ranging 50 to 100 N at 673 K (400 °C) for tempered sorbite. At the load of 200 N or greater, or the temperatures above 673 K (400 °C), oxidative wear (beyond mild oxidative wear) prevailed. When the highest load of 300 N at 673 K (400 °C) was applied, extrusive wear started to dominate for the tempered sorbite.     

An analysis of cavitation occurring in near-&gg titanium aluminide during superplastic deformation

In order to understand the cavitation behavior of near-&gg titanium aluminide alloys under superplastic forming conditions, the uniaxial hot-tension behavior of a Ti-45.5Al-2Cr-2Nb (at. pct) rolled sheet material containing a microduplex structure was determined. Three initial microstructures were examined: as-rolled, and two coarser-grained rolled-and-heat-treated conditions (1177 °C/4 h or 1238 °C/ 2 h). The cavitation behavior was analyzed after isothermal constant-strain-rate tests were conducted at temperatures between 900 °C and 1200 °C and strain rates in the range of 10⁻⁴ to 10⁻² s⁻¹. Interrupted tests and strain-to-failure tests were conducted in order to track cavity growth with time. After testing at a given temperature and strain rate, as-rolled specimens developed fewer large-size cavities than heat-treated specimens, possibly due to the finer grain size in the as-rolled material. Cavity growth was found to be plasticity controlled; the largest cavity size and density of cavities increased with increasing strain or strain rate and decreasing temperature. Since the number of finest-sized cavities examined did not decrease with strain, it is believed that continuous cavity nucleation occurred. For all three initial microstructures, the optimum sheet-forming temperature in the regime examined was identified as 1200 °C, at which the lowest cavity growth rates and highest ductilities were observed.     

The mechanical stability of austenite and cryogenic toughness of ferritic Fe-Mn-AI Alloys

In an attempt to understand the role of retained austenite on the cryogenic toughness of a ferritic Fe-Mn-AI steel, the mechanical stability of austenite during cold rolling at room temperature and tensile deformation at ambient and liquid nitrogen temperature was investigated, and the microstructure of strain-induced transformation products was observed by transmission electron microscopy (TEM). The volume fraction of austenite increased with increasing tempering time and reached 54 pct after 650 °C, 1-hour tempering and 36 pct after 550 °C, 16-hour tempering. Saturation Charpy impact values at liquid nitrogen temperature were increased with decreasing tempering temperature, from 105 J after 650 °C tempering to 220 J after 550 °C tempering. The room-temperature stability of austenite varied significantly according to the(α + γ) region tempering temperature;i.e., in 650 °C tempered specimens, 80 to 90 pct of austenite were transformed to lath martensite, while in 550 °C tempered specimens, austenite remained untransformed after 50 pct cold reductions. After tensile fracture (35 pct tensile strain) at -196 °C, no retained austenite was observed in 650 °C tempered specimens, while 16 pct of austenite and 6 pct of e-martensite were observed in 550 °C tempered specimens. Considering the high volume fractions and high mechanical stability of austenite, the crack blunting model seems highly applicable for improved cryogenic toughness in 550 °C tempered steel. Other possible toughening mechanisms were also discussed. Formerly Graduate Student, Seoul National University.     

Recovery and Precipitate Analysis of 9 Pct Cr-1 Pct MoVNb Steel during Creep

The effect of tempering temperature and creep exposure on the microstructure of a modified 9Cr steel was investigated. Creep-interrupted specimens, including the grip portion, were investigated precisely using mainly X-ray and inductively coupled plasma (ICP) spectroscopy. After saturation of precipitation due to creep exposure, the amount of extracted residue decreased once and then increased within a short period (dip). Chemical analysis showed that during the dip, the precipitates temporarily dissolved into the matrix and precipitated again. The size of the Cr₂₃C₆ increased gradually during creep, but the growth rate was relatively small, as compared to the Ostwald ripening. The size of the VN particles in the specimens tempered at 800 °C in the early stage of creep was very fine, approximately 20 nm, and tended to decrease further with the progress of creep. The size variations of the precipitates and the dip were explained from the annihilation or migration of precipitation sites, i.e., dislocations and boundaries, during creep. Transient creep for the specimens tempered at 500 °C was controlled by a reduction of the mobile dislocation density. On the other hand, transient creep for 800 °C was due to precipitation hardening of fine VN particles with the progress of creep, which was supported by the increase in both the lattice strain and the activation energy with creep.     

The structure of tempered martensite and its susceptibility to hydrogen stress cracking

A series of 4130 steels modified with 0.50 pct Mo and 0.75 pct Mo were tempered at temperatures between 300 and 700 °C for one hour. The changes in the carbide dispersion and matrix substructure produced by tempering were measured by transmission electron microscopy. These measurements were correlated with resistance to hydrogen stress cracking produced by cathodic charging of specimens in three-point bending. Scanning electron microscopy showed that specimens tempered between 300 and 500 °C failed by intergranular cracking while those tempered at higher temperatures failed by a transgranular fracture mode. Auger electron spectroscopy showed that the intergranular fracture was associated with hydrogen interaction with P segregation and carbide formation at prior austenite grain boundaries. Transgranular cracking was initiated at inclusion particles from which cracks propagated to produce flat fracture zones extending over several prior austenite grains. The 4130 steels modified with higher Mo content resisted tempering and showed better hydrogen stress cracking resistance than did the unmodified 4130 steel. The transition in fracture mode is attributed to a decohesion mechanism in the low temperature tempered samples and a pressure mechanism in the highly tempered samples.     

Fatigue crack initiation and microcrack growth in 4140 steel

Initiation and growth of fatigue microcracks were studied in vacuum degassed 4140 steel in three conditions: as-quenched, tempered at 400°C, and tempered at 650°C. Micro-scopic examinations were made of specimens with metallographically polished notches using a 400 times long working distance microscope with an x-y micrometer base mounted directly on an MTS machine. Following Barsom and McNicol, the cycles to fatigue crack initiationN _i were plottedvs ΔK/√p and threshhold values of gDK√p were determined. The data of logN _i vs log [ΔK/√p-ΔK/√p|_th] fit on a straight line. Microcracks grew most rapidly in as-quenched specimens and least rapidly in 650°C tempered specimens at the same ΔK/√p. In as-quenched specimens, fatigue cracks initiated at grain boundaries but in the 400 and 650°C tempered specimens they initiated at intrusions-extrusions. They are also associated with Northwestern’s Materials Research Center.     

Carbide Evolution in Temper Embrittled NiCrMoV Bainitic Steel

Phosphorus segregation to prior austenite grain boundaries in low alloy steel from exposure to temperatures of 300 to 600°C results in a susceptibility for intergranular fracture referred to as “temper embrittlement”. It has been observed that alloying steel with Mo greatly reduces the phosphorus segregation kinetics. Therefore changes in the ferrite matrix composition from carbide precipitation and evolution involving Mo can influence the segregation phenomenon and fracture properties. This study uses analytical electron microscopy of extraction replicas to characterize the changes in carbide chemistry of a NiCrMoV bainitic steel with 0.25 wt% C that accompany the phosphorus segregation during aging at 480°C for up to 3400 hr. The steel was doped with 0.02 wt% P and tempered at 650°C to two different hardness levels, i.e., two different initial carbide distributions. The amount of grain boundary phosphorus segregation produced by aging at 480°C correlates with the level of molybdenum that remains in solution in the ferritic matrix whereas changes in vanadium and chromium appear to have less influence on the temper embrittlement.     

Microstructure and fracture of 52100 steel

The fracture behavior of 52100 steel hardened and tempered to R_C62 has been investigated as a function of austenitizing over the temperature range from 800 to 1100°C. Specimens were homogenized at 1150°C and either furnace cooled or isothermally transformed at 580°C to produce a pearlitic microstructure prior to austenitizing for hardening. Furnace-cooled specimens developed a proeutectoid carbide network that did not dissolve during subsequent austenitizing below A_cm . The residual proeutectoid carbides and the carbide-free martensite-austenite structure between them controlled fracture and produced K_IC of 19 MPa \ m^1/2, the highest determined in this investigation. The specimens isothermally transformed prior to austenitizing below A_cm produced a microstructure of fine spherical carbides dispersed throughout a fine martensitic matrix and did not contain residual proeutectoid carbides. The transgranular fracture of the latter specimens by microvoid coalescence around the closely spaced spherical carbides resulted in the lowest values of fracture toughness, 14 to 16 MPa\ m^1/2, determined in these experiments. Austenitizing above A_cm caused solution of all carbides, a gradual coarsening of the austenitic grain size, a transition to plate martensite, and an increase in retained austenite. Fracture toughness increased slightly with increasing austenitizing temperature above A_cm despite the fact that fracture propagated primarily along the austenitic grain boundaries. The improved fracture toughness, verified by scanning electron microscopy of the fatigue crack-overload fracture interface, is believed to be caused in part by transgranular crack propagation during the first stages of crack extension that are most important in determining K_1C.