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).     

Hardness of tempered martensite in carbon and low-alloy steels

This paper presents the results of a systematic study of the effect of carbon, manganese, phosphorus, silicon, nickel, chromium, molybdenum, and vanadium on the hardness of martensite in low to medium carbon steels tempered for one hour at 100°F (56°C) intervals in the range 400 to 1300°F (204 to 704°C). Results show that the as-quenched hardness depends solely on carbon content. On tempering, the effect of carbon on hardness decreases markedly with increasing tempering temperature. Studies of carbon-0.5 manganese steels showed that the incremental increase in hardness from 0.5 pct manganese after a given tempering treatment was independent of carbon content. Based on this result, studies of the effects of the other alloying elements were made using a 0.2 or 0.3 pct carbon, 0.3 to 0.5 pct manganese steel base composition. The hardness of the resulting tempered martensite was assumed to be due to a given alloy addition, and when two or more alloying elements were added, their effects were assumed to be additive. Each of the seven alloying elements increased the hardness of tempered martensite by varying amounts, the increase being greater as more of each element was present. Nickel and phosphorus have substantially the same effect at all tempering temperatures. Manganese has essentially the same hardening effect at any temperature in the range 700 (371°C) to 1300°F; silicon is most effective at 600°F (316°C), chromium at 800°F (427°C), molybdenum at 1000 to 1100°F (538 to 592°C), and vanadium at 1200°F (649°C). Using the data obtained, a procedure is established for calculating the hardness of tempered martensite for carbon and alloy steel compositions in the range studied and for any combination of tempering time and temperature. R. A. GRANGE was formerly with U. S. Steel Corporation (retired)     

Retained Austenite and Tempered Martensite Embrittlement in Medium Carbon Steels

Electron microscopy, diffraction and microanalysis, X-ray diffraction, and auger spectroscopy have been used to study quenched and quenched and tempered 0.3 pct carbon low alloy steels. Some in situ fracture studies were also carried out in a high voltage electron microscope. Tempered martensite embrittlement (TME) is shown to arise primarily as a microstructural constraint associated with decomposition of interlath retained austenite into M₃C films upon tempering in the range of 250 °C to 400 °C. In addition, intralath Widmanstätten Fe₃C forms from epsilon carbide. The fracture is transgranular with respect to prior austenite. The situation is analogous to that in upper bainite. This TME failure is different from temper embrittlement (TE) which occurs at higher tempering temperatures (approximately 500 °C), and is not a microstructural effect but rather due to impurity segregation (principally sulfur in the present work) to prior austenite grain boundaries leading to intergranular fracture along those boundaries. Both failures can occur in the same steels, depending on the tempering conditions.     

Retained austenite and tempered martensite embrittlement in medium carbon steels

Electron microscopy, diffraction and microanalysis, X-ray diffraction, and auger spectroscopy have been used to study quenched and quenched and tempered 0.3 pct carbon low alloy steels. Somein situ fracture studies were also carried out in a high voltage electron microscope. Tempered martensite embrittlement (TME) is shown to arise primarily as a microstructural constraint associated with decomposition of interlath retained austenite into M₃C filM_s upon tempering in the range of 250 °C to 400 °C. In addition, intralath Widmanstätten Fe₃C forms from epsilon carbide. The fracture is transgranular with respect to prior austenite. The sit11Ation is analogous to that in upper bainite. This TME failure is different from temper embrittlement (TE) which o°Curs at higher tempering temperatures (approximately 500 °C), and is not a microstructural effect but rather due to impurity segregation (principally sulfur in the present work) to prior austenite grain boundaries leading to intergranular fracture along those boundaries. Both failures can o°Cur in the same steels, depending on the tempering conditions.     

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.     

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.     

Tempered martensite embrittlement and intergranular fracture in an ultra-high strength sulfur doped steel

This paper reports a study of tempered martensite embrittlement in a Ni-Cr steel doped with 0.01 wt pct S. The segregation of sulfur to the grain boundaries and the associated embrittlement of this material are very dependent upon the austenitizing temperature. If the austenitizing temperature is below 1050 °C very little embrittlement and very little intergranular fracture are observed because sulfur remains precipitated as chromium sulfide. At higher austenitizing temperatures the sulfides dissolve and sulfur segregates to the grain boundaries. Because of the high bulk content, the sulfur concentration at the grain boundaries becomes great enough for the sulfides to reprecipitate there. This leads to low energy intergranular ductile fracture. However, some sulfur remains unprecipitated at the boundary and can lower the cohesive strength across the boundary. When plate-like cementite precipitates at the grain boundary during tempering heat treatments at 300 to 400 °C, the combination of the carbides and the unprecipitated sulfur causes intergranular fracture and tempered martensite embrittlement.     

碳含量对Mn-B钢氢致延迟断裂行为的影响

采用电化学阴极充氢、氢热分析(TDS)和慢应变速率拉伸等试验方法,研究了4种不同碳含量Mn-B钢经不同热处理制度处理后的氢致延迟断裂行为。结果表明,在低于400℃回火时,随着碳含量的增加,试验钢的氢脆敏感性升高,当碳的质量分数高于0.3%后,试验钢的氢脆敏感性几乎不再增加;碳含量一定时,试验钢的氢脆敏感性随回火温度的升高而降低,且以20MnB试验钢的降低趋势最为明显;当回火温度达到600℃时,各试验钢对氢几乎不再敏感;TDS分析表明,试验钢充氢后的氢含量明显增加,其中以可扩散性氢量的增加为主;随碳含量的增加,试验钢充入的氢量增加;当碳含量一定时,随回火温度的升高,试验钢充入的氢量减少;SEM断口观察表明,试验钢充氢后的脆性断裂倾向性增加;随着碳含量的升高,试验钢的断裂方式由韧性断裂向脆性断裂转变;碳含量一定时,随回火温度的升高,试验钢由淬火态的脆性断裂向高温回火态的韧性断裂转变。     

Structure and mechanical properties of Fe-Cr-Mo-C alloys with and without boron

A study of the structure and mechanical properties of Fe-Cr-Mo-C martensitic steels with and without boron addition has been carried out. Nonconventional heat treatments have subsequently been designed to improve the mechanical properties of these steels. Boron has been known to be a very potent element in increasing the hardenability of steel, but its effect on structure and mechanical properties of quenched and tempered martensitic steels has not been clear. The present results show that the as-quenched structures of both steels consist mainly of dislocated martensite. In the boron-free steel, there are more lath boundary retained austenite films. The boron-treated steel shows higher strengths at all tempering temperatures but with lower Charpy V-notch impact energies. Both steels show tempered martensite embrittlement when tempered at 350 °C for 1 h. The properties above 500 °C tempering are significantly different in the two steels. While the boron-free steel shows a continuous increase in toughness when tempered above 500 °C, the boron-treated steel suffers a second drop in toughness at 600 °C tempering. Transmission electron microscopy studies show that in the 600 °C tempered boron-treated steel large, more or less continuous cementite films are present at the lath boundaries, which are probably responsible for the embrittlement. The differences in mechanical properties at tempering temperatures above 500 °C are rationalized in terms of the effect of boron-vacancy interactions on the recovery and recrystallization behavior of these steels. Although boron seems to impair room temperature impact toughness at low strength levels, it does not affect this property at high strength levels. By simple nonconventinal heat treatments of the present alloys, martensitic steels may be produced with quite good strength-toughness properties which are much superior to those of existing commercial ultra-high strength steels. It is also shown that very good combinations of strength and toughness can be obtained with as-quenched martensitic steels.     

Effect of tempering temperature on the work-hardening rate of five HSLA steels

A series of compression tests were performed to measure the work-hardening characteristics of a variety of quenched and tempered high strength low alloy (HSLA) steels as a function of tempering temperature. All of the steels tested had a minimum in their work-hardening rate when tempered in the range 300° to 450 °C and all exhibited a maximum at 700 °C, the upper limit of the range examined. The steels containing both molybdenum and vanadium exhibited delayed tempering in the range 400° to 600 °C, and this was reflected as an increased work-hardening rate. A discussion on the microstructural changes occurring over the tempering range suggests reasons for the observed behavior.     

Deformation, fracture, and mechanical properties of low-temperature-tempered martensite in SAE 43xx steels

Uniaxial tensile tests were performed on 4330, 4340, and 4350 steels in the as-quenched (AQ) condition and after quenching and tempering at 150 °C, 175 °C, and 200 °C for times of 10 minutes, 1 hour, and 10 hours, respectively. Strength parameters decreased and ductility parameters increased continuously with increasing tempering. Mechanical properties are presented as a function of tempering conditions and steel carbon content, and hardness and ultimate strength changes are given as a function of Hollomon—Jaffe tempering parameters. All tempered specimens, except for some lightly tempered 4350 specimens, deformed plastically through necking instability and failed by ductile fracture. The stresses required for the ductile fracture, estimated from an analysis of the interfacial stresses at particles in the neck at fracture, showed no systematic variation with carbon content or tempering conditions despite significant variations in deformation and strain hardening. The AQ specimens of the 4340 and 4350 steels, and some of the lightly tempered 4350 steels, failed by brittle mechanisms. The deformation and fracture of the low-temperature-tempered 43xx steels are discussed in terms of the changes in fine structure, namely, the formation of transition carbides and a rearranged dislocation substructure that evolve from an AQ martensitic substructure consisting of dislocations with and without carbon atom segregation.     

The role of nitrogen in the embrittlement of steel

Nitrogen is one of the most common impurity elements to be found in steels. Previous work has shown that it is a potential grain boundary embrittler. In this paper we examine its role in both tempered martensite embrittlement and temper embrittlement. The basic composition of the steel used for this study was, in wt pct, 3.5 Ni, 1.7 Cr, 0.3 C, and 0.01 N. It was found that nitrogen could be very detrimental to mechanical properties but not as a grain boundary embrittler in the typical sense that P, Sn, and Sb are. Rather, nitrogen is almost always precipitated as nitrides and these second phase particles can induce low energy ductile fracture. The distribution of nitrides in the solid and the type of nitride present is dependent on the heat treatment. If a low austenitizing temperature is used, the nitrides in the steel dissolve and considerable nitrogen segregates to the grain boundaries. During an oil quench it reprecipitates at the boundaries, primarily as Cr₂N. These nitrides cause low energy, ductile intergranular fracture. If a high austenitizing temperature is used, much less nitrogen segregrates so fewer nitrides precipitate during the quench. However, upon tempering the nitrogen does reprecipitate. At low tempering temperatures, small nitrides form both within the grains and along the grain boundaries. When these nitrides become sufficiently large, voids form around them as well as around the carbides during fracture. These small voids help link the large voids that form around oxide and sulfide particles and lower the energy for ductile fracture. After high temperature tempering treatments large nitrides and carbides form at the grain boundaries. These produce low energy, intergranular ductile fracture. These large grain boundary precipitates can also aid in brittle intergranular fracture by providing many more sites for nucleation of intergranular cracks when the boundary is weakened by another impurity element.     

Effect of molybdenum on the fracture characteristic of high-speed steel quenched matrix

The fractures of three model alloys, imitating by their chemical composition the matrixes of the quenched high-speed steels of various Mo: W relations were analyzed. According to the measurements of the stress intensity factor K_Ic and the differences in the precipitation processes of carbides it was found out that the higher fracture toughness of the matrix of the molybdenum high-speed steels than on the tungsten ones is the results of the differences in the kinetics of precipitation from the martensite matrix of these steels during tempering. After tempering at 250 and 650°C the percentage of the intergranular fracture increases with the increase of the relation of Mo to W in the model alloys of the high-speed steel matrix. This is probably the result of higher precipitation rate of the M₃C carbide (at 250°C) and the MC and M₆C carbides (at 650°C) in the privileged regions along the grain boundaries. The change of the character of the model alloy fractures after tempering at 450°C from the completely transgranular one in the tungsten alloy to the nearly completely intergranular one in the molybdenum alloy indicates that the coherent precipitation processes responsible for the secondary hardness effect in the tungsten matrix begin at a lower temperature than in the molybdenum matrix. After tempering for the maximum secondary hardness the matrix fractures of the high-speed steels reveal a transgranular character regardless the relation of Mo to W. The higher fracture toughness of the Mo matrix can be the result of the start of the coherent precipitation processes at a higher temperature and their intensity which can, respectively, influence the size of these precipitations, their shape and the degree of dispersion. The transgranular character of the fractures of the S 6-5-2 type high-speed steel in the whole range tempering temperatures results from the presence of the undissolved carbides which while cracking in the region of stress concentration can constitute flaws of critical size which form the path of easy cracking through the grains. The transgranular cracking of the matrix of the real high-speed steels does not change the adventageous influence of molybdenum upon their fracture toughness. On the other hand, the carbides, undissolved during austenitizing, whose size distribution in the molybdenum steels from the point of view of cracking mechanics seems to be unsatisfactory, influence significantly the fracture toughness of these steels.     

Tribological Performance of Austempered and Tempered Ductile Iron

Austempered ductile iron with its unique ausferritic structure is produced by an isothermal heat treatment process. Austempered ductile iron is a potential material to substitute for traditional steel castings and forgings in current industry due to its excellent mechanical properties. The tempering process is frequently used to enhance the ductility and toughness of a material and reduce residual stress. In this research, the phase transformation of austempered ductile iron was studied by applying various tempering temperatures with constant holding duration. It was found that the ausferritic structure was decomposed into dispersive cementite particles after receiving a tempering temperature of 538 °C or higher. The specific amount of retained austenite was analyzed by X-ray diffraction. The wear resistance of tempered austempered ductile iron was investigated by using a ball-on-disk sliding test configuration. The results were compared with conventional quenched and tempered ductile iron under equivalent hardness. Both austempered ductile iron and tempered austempered ductile iron samples had better wear resistance than quenched and tempered ductile iron. The results presented in this research can be utilized as a reference in the tempering treatment of austempered ductile iron material for future applications.     

Effects of chromium on the temper embrittlement and wear resistance of 0.25% C low-alloy cast steel

The effects of additions of 0.6 to 2.0% Cr on the temper embrittlement behaviour of 0.25 C–1.0 Si–1.3 Mn cast steel under several hardening conditions were studied. The susceptibility to temper embrittlement, transgranular and intergranular fracture were increased as the chromium content increased when the steels were tempered at 350°C and slowly cooled from 550°C. The impact toughness and abrasion resistance of the steels were found to depend to a great extent on the Cr-content and tempering temperature.     

Role of Microstructure and Temperature on the Tensile Fracture Behavior of Oxide Dispersion Strengthened 18Cr Ferritic Steel

The tensile fracture behavior of oxide dispersion strengthened 18Cr (ODS-18Cr) ferritic steels milled for varying times was studied along with the oxide-free 18Cr steel (NODS) at 25, 200, 400, 600, and 800 °C. At all the test temperatures, the strengths of ODS–18Cr steels increased and total elongation decreased with the duration of milling time. Oxide dispersed 18Cr steel with optimum milling exhibited enhanced yield strength of 156 pct at room temperature and 300 pct at 800 °C when compared to oxide-free 18Cr steel. The ductility values of ODS-18Cr steels are in the range 20 to 35 pct for a temperature range 25 to 800 °C, whereas NODS alloy exhibited higher ductility of 37 to 82 pct. The enhanced strength of ODS steels when compared to oxide-free steel is due to the development of ultrafine grained structure along with nanosized dispersion of complex oxide particles. While the pre-necking elongation decreased with increasing temperature and milling time, post-necking elongation showed no change with the test temperature. Fractographic examination of both ODS and NODS 18Cr steel fractured tensile samples, revealed that the failure was in ductile fracture mode with distinct neck and shear lip formation for all milling times and at all test temperatures. The fracture mechanism is in general followed the sequence; microvoid nucleation at second phase particles, void growth and coalescence. The quantified dimple sizes and numbers per unit area were found to be in linear relation with the size and number density of dispersoids. It is clearly evident that even nanosized dispersoids acted as sites for microvoid nucleation at larger strains and assisted in dimple rupture.

     

Effects of Tempering Temperature and Mo/Ni on Microstructures and Properties of Lath Martensitic Wear-Resistant Steels

 The tempering behavior was experimentally studied in lath martensitic wear-resistant steels with various Mo/Ni contents after tempering at different temperatures from 200 to 600 ℃. It is shown that a good combination of hardness (HV) (420-450) and -20 ℃ impact toughness (38-70 J) can be obtained after quenching and tempering at 200-250 ℃. The microstructure at this temperature is lath structure with rod-like and/or flake-like ε-carbide with about 10 nm in width and 100 nm in length in the matrix, and the fracture mechanism is quasi-cleavage fracture combining with ductile fracture. Tempering at temperature from 300 to 400 ℃ results in the primary quasi-cleavage fracture due to the carbide transformation from resolved retained austenite and impurity segregation between laths or blocks. However, when the tempering temperature is higher than 500 ℃, the hardness (HV) is lower than 330 and the fracture mechanism changes to ductile fracture due to the spheroidization and coarsening of cementite. Additions of Mo and Ni have no significant effects on the carbides morphologies at low tempering temperatures, but improve the resistance to softening and embrittling for steels when tempered at above 350 ℃.     

Effect of hydrogen on fracture behavior of a quenched and tempered medium-carbon steel

This work examined the effects of hydrogen on fracture of quenched and tempered 1045 steel. Tests were made at room temperature on tensile, Charpy impact, and 4-point notched bend specimens. This steel exhibits tempered martensite embrittlement (TME) for tempering temperatures between 300 and 375 °C. Thus hydrogen in most cases affected fracture by increasing the amount of intergranular fracture. In bend specimens, hydrogen also induced quasicleavage (QC) fracture at points of maximum normal stress below the notch root, points which appeared to be the locations of crack initiation. Tear ridges on theseQC surfaces were at martensite lath packet boundaries. Crack orientations were largely mode I in uncharged specimens, with mode II appearing at the notch root in most hydrogen-charged specimens. These observations are in general agreement with earlier work on martensitic steel. Formerly graduate student, Carnegie-Mellon University     

Influence of thermomechanical treatments on the microstructure and mechanical properties of HSLA-100 steel plates

The influence of thermomechanical treatment (TMT), i.e., controlled rolling and direct quenching, as a function of rolling temperature and deformation on the microstructure and mechanical properties of HSLA-100 steel have been studied. The optical microstructure of the direct quenched (DQ) and tempered steel rooled at lower temperatures (800 °C and 900 °C) showed elongated and deformed grains, whereas complete equiaxed grains were visible after rolling at 1000 °C. The transmission electron microscope (TEM) microstructure of the 800 °C rooled DQ steel showed shorter, irregular, and closer martensite laths with extremely fine Cu and Nb(C,N) precipitates after tempering at 450 °C. The precipitates coarsened somewhat after tempering at 650 °C; the degree of coarsening was, however, less compared to that of the reheat-quenched (RQ) and tempered steel, indicating that the DQ steel was slightly more resistant to tempering. Similar to the RQ steel, at a 450 °C tempering condition, the DQ steel exhibited peak strength with extremely poor impact toughness. After tempering at 650 °C, the toughness of the DQ steel improved significantly, but at the expense of its strength. In general, the strength of the DQ and tempered steel was good and comparable to that of the RQ and tempered steel, although, its impact toughness was marginally less than the latter. The optimum combination of strength and toughness in the DQ steels was achieved after 900 °C rolling with 50 pct deformation, followed by direct quenching and tempering at 650 °C (yield strength (YS)=903 MPa, ultimate tensile strength (UTS)=928 MPa, and Charpy V-notch (CVN) strength=143 J at −85 °C).     

Development of High Strength Plates with Low Yield Ratio by the Combination of TMCP and Inter‐Critical Quenching and Tempering

A new processing route of thermo‐mechanical processing (TMCP) followed by inter‐critical quenching and tempering (L‐T) was developed to produce 590MPa grade high strength plates based on a relatively lean composition of plain carbon manganese steels microalloyed with Nb, V and Ti. The effect of quenching temperatures on the evolution of microstructure and mechanical properties were investigated. The nano‐hardness measurements of martensite were performed with a nano‐indenter, which indicated that the fractions of as quenched and tempered martensite increased and their hardness values decreased with increasing quenching temperatures in the range from 760 °C to 810 °C. For both as quenched and tempered samples, ferrite grain sizes decreased with increasing quenching temperature in almost linear relationships. The yield strength increased with increasing the fraction of martensite while the tensile strength remained almost unchanged, leading to the increase of yielding ratio with increasing quenching temperatures. The optimum quenching temperature was determined to be around 760 °C in terms of strengths and yield ratio.