Ferrite recrystallization and austenite formation in cold-rolled intercritically annealed steel

The recrystallization of ferrite and austenite formation during intercritical annealing were studied in a 0.08C-1.45Mn-0.21Si steel by light and transmission electron microscopy. Normalized specimens were cold rolled 25 and 50 pct and annealed between 650 °C and 760 °C. Recrystallization of the 50 pct deformed ferrite was complete within 30 seconds at 760 °C. Austenite formation initiated concurrently with the ferrite recrystallization and continued beyond complete recrystallization of the ferrite matrix. The recrystallization of the deformed ferrite and the spheroidization of the cementite in the deformed pearlite strongly influence the formation and distribution of austenite produced by intercritical annealing. Austenite forms first at the grain boundaries of unrecrystallized and elongated ferrite grains and the spheroidized cementite colonies associated with ferrite grain boundaries. Spheroidized cementite particles dispersed within recrystallized ferrite grains by deformation and annealing phenomena were the sites for later austenite formation.     

Effects of austenite grain size and cooling rate on Widmanstätten ferrite formation in low-alloy steels

Deformation dilatometry is used to simulate the hot rolling of 0.20 pct C-1.10 pct Mn steels over a product thickness range of 6 to 170 mm. In addition to a base steel, steels with additions of 0.02 pct Ti, 0.06 pct V, or 0.02 pct Nb are included in the study. The transformation behavior of each steel is explored for three different austenite grain sizes, nominally 30, 55, and 100 μm. In general, the volume fraction of Widmanst?tten ferrite increases in all four steels with increasing austenite grain size and cooling rate, with austenite grain size having the more significant effect. The Nb steel has the lowest transformation temperature range and the greatest propensity for Widmanst?tten ferrite formation, while the amount of Widmanst?tten ferrite is minimized in the Ti steel (as a result of intragranular nucleation of polygonal ferrite on coarse TiN particles). The data emphasize the importance of a refined austenite grain size in minimizing the formation of a coarse Widmanst?tten structure. With a sufficiently fine prior austenite grain size (e.g., ≤30 μm), significant amounts of Widmanst?tten structure can be avoided, even in a Nb-alloyed steel.     

Interrelations of cooling rate,microstructure, and mechanical properties in four HSLA steels

The present study was carried out on four steels containing 0.1 pct C-1.5 pct Mn-0.003 pct B* in common, with additions of 1 pct Cr, 0.5 pct Mo, 0.25 pct Mo + 1 pct Cr, 0.2 pct Ti + 1 pct Cr. They were designated, accordingly, as Cr, Mo, Mo-Cr, and Cr-Ti steels. All the steels exhibited a complete lath martensite microstructure with thin interlaths of retained austenite (≈0.05 pct) in the quenched condition. The normalized microstructures, granular bainite, contained massive areas of ferrite and granules of bainite laths. Both microconstituents contained a fine dispersion of cementite particles (size ≈50 Å) together with high dislocation densities. A mechanism explaining their for-mation has been given. The Cr steel, due to its low hardenability, showed in addition polygonal ferrite in the neighborhood of the so-called M-A constituent (twinned martensite and/or austenite). The annealed microstructure (using a cooling rate of 0.033 °C s^?1) of the Cr steel consisted of coarse ferrite-pearlite. Addition of 0.2 pct Ti to the Cr steel markedly refined the structure, whereas an addition of 0.25 pct Mo altered the microstructure to ferrite-lower bainite. In the 0.5 pct Mo steel, polygonal ferrite was found to be completely missing. The mechanical properties of the four steels after quenching, normalizing, and annealing were investigatedvia hardness and tensile test mea-surements. An empirical equation, relating the ultimate tensile strength to the steel composition, for steels that had granular bainite microstructures in the normalized condition, was proposed. The fracture surfaces exhibited cleavage and variable-size dimples depending on the microstructure and steel composition.     

Solidification parameters,microstructures, and mechanical properties of rapidly solidified iron-based alloys

Cooling rate measurements were carried out using a computer controlled melt spinning unit for the production of rapidly solidified Fe 6.3 wt.% Si and Fe 3.2 wt.% C melt spun ribbons employing a wide range of process parameters. The cooling rates are mainly a function of the ribbon thickness, and are independent of the alloy composition and wheel material. The resulting microstructures have been characterized by light optical and electron microscopy (SEM and TEM) investigations and were found to be influenced by the cooling conditions during and after solidification. Grain sizes and secondary dendrite arm spacings are related to the cooling rates by means of exponential relationships. In addition to this, rapidly solidified eutectic Fe 4.2 wt. %C alloy powder was produced by argon melt-atomization. Powder particles of 20 μm to 80 μm size solidified microcrystalline and exhibit cementite, metastable γ-phase, and martensite. The cementite matrix is of dendritic structure. After consolidating the powder by hot pressing below A, the microstructure changes to the fine equiaxed grains containing about 66 Vol.% Fe₃C and a dispersoid of ferrite ≤1 μm within the cementite matrix. This material exhibits high tensile strength and wear resistance at room temperature. At elevated temperatures in the region between 650°C and 750°C, and at strain rates of ε ? 10^?4s^?1 the fine grained ceramic-like material reveals superplastic behaviour.     

Microstructures and superplastic behavior of eutectic Fe-C and Ni-Cr white cast irons produced by rapid solidification

Superplastic behavior of two commercial grade white cast irons, eutectic Fe-C and Ni-Cr white cast irons, was investigated at intermediate temperatures (650 to 750 °C). For this purpose, rapidly solidified powders of the cast irons were fully consolidated by compaction and rolling at about 650 °C. The volume fractions of cementite in the eutectic cast iron and in the Ni-Cr cast iron were 64 pct and 51 pct, respectively, and both cast irons consisted of fine equiaxed grains of cementite (1 to 2 μm) and ferrite (0.5 to 2 μm). The cast iron compacts exhibited high strain-rate sensitivity (strain-rate-sensitivity exponent of 0.35 to 0.46) and high tensile ductility (total elongation of 150 pct to 210 pct) at strain rates of 10^-4 to 10^-3 s^-1 and at 650 °C to 750 °C. Microstructure evaluations were made by TEM, SEM, and optical microscopy methods. The equiaxed grains in the as-compacted samples remained unchanged even after large tensile deformation. It is concluded that grain boundary sliding (e.g., along cementite grain boundaries in the case of the eutectic cast iron) is the principal mode of plastic deformation in both cast irons during superplastic testing conditions. Formerly with the Department of Materials Science and Engineering, Stanford University Formerly Visiting Scholar, Department of Materials Science and Engineering, Stanford University     

Microstructural evolution of submicron sized ferrite in bimodal structural ultrafine grained ferrite/cementite steels by annealing below austenized temperature

The microstructural evolution of submicron sized ferrite in bimodal structural ultrafine grained ferrite/cementite steels with 0.15 pct carbon content and 0.45 pct carbon content upon annealing below the austenized temperature was investigated. The average grain sizes of the ferrites with a normal density and with a high density of cementite particles were plotted, respectively, as a function of the annealed temperature and time, and exhibited different coarsening behaviors. The average grain sizes of the ferrites with a normal density of cementite particles gradually coarsened by increasing the annealing temperature or time, while those with a high density of cementite particles hardly changed at first, and then coarsened after reaching a certain annealing condition. The coarsening of the ferrite grain size in the steel with 0.15 pct carbon content occurred much more readily than that in the steel with 0.45 pct carbon content upon annealing. The spacing and the critical spacing of cementite particle were measured and hypothetically calculated, respectively. The size and the distribution of cementite particles was one of the critical factors affecting the microstructural evolution in this type of cementite particle spherodized steels. Most of the coarsening of the ferrite grain size occurred after the cementite particle spacing reached the required critical value.     

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.     

Recovery of Ductility in Ultrafine-Grained Low-Carbon Steel Processed Through Equal-Channel Angular Pressing Followed by Cold Rolling and Flash Annealing

The low-carbon steel workpieces are deformed by equal-channel angular pressing at 293 K (20 °C) up to an equivalent strain of ~12 using route B _c, which results in the bulk ultrafine-grained (UFG) structure with high dislocation density and partial dissolution of cementite. The yield strength (YS) is enhanced from 208 (as-received) to 872 MPa and the tensile strength is increased from 362 to 996 MPa, but the material loses total elongation (TE) from 36.2 to 2.9 pct. Cold rolling of equal-channel angular pressed steel produces the refined structure of grain size 0.11 μm. The YS increases further to 924 MPa with a marginal gain in ductility due to the reappearance of the γ fiber component. Flash annealing the samples, which were equal-channel angular pressed followed by cold rolling, at 873 K (600 °C) results in 27 pct of micron-sized (9 µm) ferrite grains in submicron-sized (<1 µm) matrix with a reduced defect density and small amount of precipitation of cementite. TE increases from 2.9 to 23.3 pct. The material retains a YS of 484 MPa and tensile strength of 517 MPa, which are higher than those of the as-received material. The UFG grains are failed by cleavage, but the micron-sized grains display ductile fracture. The ductility of the flash-annealed material is recovered significantly due to bimodal grain size distribution in ferrite and the development of a good amount of γ fiber texture components. The major contribution toward recovery of ductility comes from the bimodal grain size distribution in ferrite rather the precipitation of cementite.

     

Phosphorus and carbon segregation: Effects on fatigue and fracture of gas-carburized modified 4320 steel

Phosphorus and carbon segregation to austenite grain boundaries and its effects on fatigue and fracture were studied in carburized modified 4320 steel with systematic variations, 0.005, 0.017, and 0.031 wt pct, in alloy phosphorus concentration. Specimens subjected to bending fatigue were characterized by light metallography, X-ray analyses for retained austenite and residual stress measurements, and scanning electron microscopy (SEM) of fracture surfaces. Scanning Auger electron spectroscopy (AES) was used to determine intergranular concentrations of phosphorus and carbon. The degree of phosphorus segregation is directly dependent on alloy phosphorus and carbon content. The degree of carbon segregation, in the form of cementite, at austenite grain boundaries was found to be a function of alloy phosphorus concentration. The endurance limit and fracture toughness decreased slightly when alloy phosphorus concentration was increased from 0.005 to 0.017 wt pct. Between 0.017 and 0.031 wt pct phosphorus, the endurance limit and fracture toughness decreased substantially. Other effects related to increasing alloy phosphorus concentration include increased case carbon concentration, decreased case retained austenite, increased case compressive residual stresses, and increased case hardness. All of these results are consistent with the phosphorus-enhanced formation of intergranular cementite and a decrease in carbon solubility in intragranular austenite with increasing phosphorus concentration. Differences in fatigue and fracture correlate with the degree of cementite coverage on the austenite grain boundaries and the buildup of phosphorus at cementite/matrix interfaces because of the insolubility of phosphorus in cementite.     

Microstructure-strength relations in a hardenable stainless steel with 16 pct Cr, 1.5 pct Mo,and 5 pct Ni

Metallographic studies have been conducted on a 0.024 pct C-16 pct Cr-1.5 pct Mo-5 pct Ni stainless steel to study the phase reactions associated with heat treatments and investigate the strengthening mechanisms of the steel. In the normalized condition, air cooled from 1010 °C, the microstructure consists of 20 pct ferrite and 80 pct martensite. Tempering in a temperature range between 500 and 600 °C results in a gradual transformation of martensite to a fine mixture of ferrite and austenite. At higher tempering temperatures, between 600 and 800 °C, progressively larger quantities of austenite form and are converted during cooling to proportionally increasing amounts of fresh martensite. The amount of retained austenite in the microstructure is reduced to zero at 800 °C, and the microstructure contains 65 pct re-formed martensite and 35 pct total ferrite. Chromium rich M₂₃C₆ carbides precipitate in the single tempered microstructures. The principal strengthening is produced by the presence of martensite in the microstructure. Additional strengthening is provided by a second tempering treatment at 400 °C due to the precipitation of ultrafine (Cr, Mo) (C,N) particles in the ferrite.     

The effect of austenite grain size on microcracking in martensite of an Fe-1.22C alloy

Austenitic grain sizes of ASTM No. 9 and coarser were produced in an Fe-1.22 pct C alloy austenitized by immersion in molten lead at 1640†F (893°C), a temperature just above theA _cm for this alloy, for periods between 20 s and 1 h. Microcracking sensitivity,Sv, measured as crack area/unit volume martensite, was determined as a function of grain size in brine quenched specimens. Two locations of microcracks were observed in this investigation: 1) intragranular, resulting from the impingement of one martensite plate with another, and 2) grain boundary or intergranular resulting from the impingement of martensite plates at prior austenite grain boundaries. Intragranular microcracking sensitivity, the subject of previous investigations, increased and became the dominant type of cracking with increasing grain size, and reached a constant level for grain sizes of ASTM No. 4.5 and coarser. Total microcracking sensitivity, consisting of both intragranular and grain boundary microcracks, also increased with increasing grain size, then decreased to approach the intragranular value for grain sizes coarser than ASTM No. 3.5. On the other end of the scale, grain boundary microcracking made up a much larger proportion of the total microcracking in the fine grained specimens.     

The effect of prior heat treatments on the structure and properties of warm-rolled AlSl 52100 steel

Isothermal rolling of AISI 52100 steel at 923 K (650 °C) has been used to produce very fine spheroidized carbide particles 0.1 to 0.2 μm in size in a submicron grain size ferrite matrix. Pearlitic starting structures are not completely spheroidized by such warm rolling and some isolated pearlite colonies remain after rolling. Tempered martensitic starting structures result in more uniform structures after rolling. The effect of varying the austenitizing time and temperature and of two cycle austenitizing treatments before rolling of tempered martensite were studied. After rolling, the room temperature yield strength was raised, a result of the finer dispersion of carbides and the associated reduction in ferrite grain size. The presence of isolated pearlite colonies in rolled material reduces the room temperature ductility. Formerly Graduate Student, Department of Mechanical Engineering, United States Naval Postgraduate School     

Dispersion strengthening in a hypereutectic Al-Si alloy prepared by extrusion of rapidly solidified powder

When a hypereutectic aluminum-silicon alloy containing 16 wt pct silicon was rapidly solidified into powder using the spinning water atomization process, the individual powder grains were predominantly aluminum that was supersaturated with silicon and also contained well-dispersed 0.02-μm silicon particles. Although the silicon particles grew when the powder was extruded into a bar at temperatures from 673 to 803 K at an extrusion ratio of 4.3 and an extrusion speed of 0.9 mm/s, the average diameter was maintained on a submicron level. When the extrusion temperature was decreased from 803 to 673 K, the average diameter of the silicon particles in the extruded bar decreased from 0.8 to 0.5 μm, while the Vickers hardness (HV) and the ultimate tensile strength of the extruded bar increased from 120 to 160 (HV) and from 330 to 500 MPa, respectively. Both the hardness and the tensile strength of the extruded bars were several times higher than those of conventionally cast bars of the same alloy with cooling rates from 10⁻¹ to 10² K/s. On the other hand, the elongation decreased from 5.5 to 3.1 pct when the extrusion temperature was decreased from 803 to 673 K.     

Decomposition of Fe-Ni martensite: Implications for the low-temperature (≤500 °C) Fe-Ni phase diagram

The low-temperature (<500 °C) decomposition of Fe-Ni martensite was studied by aging martensitic Fe-Ni alloys at temperatures between 300 °C and 450 °C and by measuring the composition of the matrix and precipitate phases using the analytical electron microscope (AEM). For aging treatments between 300 °C and 450 °C, lath martensite in 15 and 25 wt pct Ni alloys decomposed with γ [face-centered cubic (fcc)] precipitates forming intergranularly, and plate martensite in 30 wt pct Ni alloys decomposed with γ (fcc) precipitates forming intragranularly. The habit plane for the intragranular precipitates is {111}_fcc parallel to one of the {110}_bcc planes in the martensite. The compositions of the γ intergranular and intragranular precipitates lie between 48 and 58 wt pct Ni and generally increase in Ni content with decreasing aging temperature. Diffusion gradients are observed in the matrix α [body-centered cubic (bcc)] with decreasing Ni contents close to the martensite grain boundaries and matrix/precipitate boundaries. The Ni composition of the matrix α phase in decomposed martensite is significantly higher than the equilibrium value of 4 to 5 wt pct Ni, suggesting that precipitate growth in Fe-Ni martensite is partially interface reaction controlled at low temperatures (<500 °C). The results of the experimental studies modify the γ/α + γ phase boundary in the present low-temperature Fe-Ni phase diagram and establish the eutectoid reaction in the temperature range between 400 °C and 450 °C. Formerly Research Assistant, Department of Materials Science and Engineering, Lehigh University     

Effect of Nitrogen Content on Grain Refinement and Mechanical Properties of a Reversion-Treated Ni-Free 18Cr-12Mn Austenitic Stainless Steel

Martensite reversion treatment was utilized to obtain ultrafine grain size in Fe-18Cr-12Mn-N stainless steels containing 0 to 0.44 wt pct N. This was achieved by cold rolling to 80 pct reduction followed by reversion annealing at temperatures between 973 K and 1173 K (700 °C and 900 °C) for 1 to 10⁴ seconds. The microstructural evolution was characterized using both transmission and scanning electron microscopes, and mechanical properties were evaluated using hardness and tensile tests. The steel without nitrogen had a duplex ferritic-austenitic structure and the grain size refinement remained inefficient. The finest austenitic microstructure was achieved in the steels with 0.25 and 0.36 wt pct N following annealing at 1173 K (900 °C) for 100 seconds, resulting in average grain sizes of about 0.240 ± 0.117 and 0.217 ± 0.73 µm, respectively. Nano-size Cr₂N precipitates observed in the microstructure were responsible for retarding the grain growth. The reversion mechanism was found to be diffusion controlled in the N-free steel and shear controlled in the N-containing steels. Due to a low fraction of strain-induced martensite in cold rolled condition, the 0.44 wt pct N steel displayed relatively non-uniform, micron-scale grain structure after the same reversion treatment, but it still exhibited superior mechanical properties with a yield strength of 1324 MPa, tensile strength of 1467 MPa, and total elongation of 17 pct. While the high yield strength can be attributed to strengthening by nitrogen alloying, dislocation hardening, and slight grain refinement, the moderate strain-induced martensitic transformation taking place during tensile straining was responsible for enhancement in tensile strength and elongation.     

Retained carbide distribution in intercritically austenitized 52100 steel

Two 52100 steels, one containing 0.009 pct P, the other 0.023 pct P, were homogenized at 1150 °C, slowly cooled to form proeutectoid carbides and pearlite, partially spheroidized, austenitized at 850 °C for one hour, oil quenched, and tempered at 200 °C. Light microscopy and transmission electron microscopy of carbon extraction replicas showed that cementite particles were retained as three different morphologies in the fine-grained austenite formed during the 850 °C intercritical austenitizing treatment. The morphologies are characterized as follows: (1) closely spaced intragranular carbides most of which are less than 0.25 μm in diameter, (2) carbides about 1 μm in diameter, located on austenite grain boundaries, and (3) branched proeutectoid carbides arranged in networks corresponding to the coarse, 130 μm diameter austenite grains formed during homogenizing. The major effect of high phosphorus content was to retard the spheroidization of the retained carbides.     

Pearlite phase transformation in Si and V steel

Systematic research has been undertaken on the effects of single and combined additions of vanadium and silicon on the phase transformation and microstructure of pearlitic steels. Both alloy additions were found to result in the formation of nonlamellar products in the vicinity of austenite grain boundaries in hypereutectoid compositions (0.77 to 0.95 wt pct C). The products comprise discrete initial cementite particles and grain boundary ferrite, which is embedded with interphase precipitates of vanadium carbide. As the carbon content is increased further (up to 1.05 wt pct), the amount of grain boundary ferrite gradually decreases without any dramatic change in the morphology of the initial cementite particles. No continuous embrittling grain boundary cementite network was formed. The aspect ratios of the grain boundary cementite particles were decreased from 60:1 to 25:1 by the addition of the alloy elements. A compre-hensive model has been suggested to explain these effects. Other effects of these alloy elements on the microstructure of pearlitic steels have also been examined. For given austenitization conditions, an increase in carbon and vanadium content produced a decrease in austenite grain size. Silicon was found to increase the rate of interphase precipitation of vanadium carbides. Formerly Graduate Student, Department of Materials, Oxford University Formerly University Lecturer, Department of Materials, Oxford University     

Plasma Nitriding Behavior of Fe-C-M (M = Al, Cr, Mn, Si) Ternary Martensitic Steels

Change in surface hardness and nitrides precipitated in Fe-0.6C binary and Fe-0.6 mass pct C-1 mass pct M (M = Al, Cr, Mn, Si) ternary martensitic alloys during plasma nitriding were investigated. Surface hardness was hardly increased in the Fe-0.6C binary alloy and slightly increased in Fe-0.6C-1Mn and Fe-0.6C-1Si alloys. On the other hand, it was largely increased in Fe-0.6C-1Al and Fe-0.6C-1Cr alloys. In all the Fe-0.6C-1M alloys except for the Si-added alloy, fine platelet alloy nitrides precipitated inside martensite laths. In the Fe-0.6C-1Si alloy, Si-enriched film was observed mainly at a grain boundary and an interface between cementite and matrix. Crystal structure of nitrides observed in the martensitic alloys was similar to those in Fe-M binary ferritic alloys reported previously. However, there was a difference in hardening behavior between ferrite and martensite due to a high density of dislocations acting as a nucleation site of the nitrides and partitioning of an alloying element between martensite and cementite changing the driving force of precipitation of the nitrides.     

Effect of interpass time on austenite grain refinement by means of dynamic recrystallization of austenite

A 0.06 pct C-0.3 pct Mn and a 0.07 pct C-0.6 pct Mn-0.028 pct Nb steel were deformed in torsion at a constant strain rate of 2/s. Two schedules were used. In schedule A, seven roughing passes executed between 1260°C and 1130°C were followed by a single large finishing pass with a strain of 3.5 at constant temperatures between 1010°C and 840°C. The time between roughing and finishing was 200 seconds. In schedule B, the seven roughing passes were followed by 10 finishing passes, again applied isothermally, with strains of 0.3 and interpass times of 0.6, 2, and 10 seconds. The results indicate that for the Nb steel, low rolling temperatures (870°C) and strains above 2 are required for complete dynamic recrystallization, which results in austenite grain sizes under 6μm. Cooled at a rate of 10°C/s, the dynamically recrystallized austenite grain structures transform into ferrite with grain sizes under 4 μ. Extrapolations from the present data suggest that at industrial strain rates and cooling rates, ferrite grain sizes under 2 μm should be achieved. Y.W. BOWDEN, formerly CSIRA Research Associate, Department of Mining and Metallurgical Engineering, McGill University