Influence of annealing treatment on the formation of nano/submicron grain size AISI 301 Austenitic stainless steels

Nano/submicron austenitic stainless steels have attracted increasing attention over the past few years due to fine structural control for tailoring engineering properties. At the nano/submicron grain scales, grain boundary strengthening can be significant, while ductility remains attractive. To achieve a nano/submicron grain size, metastable austenitic stainless steels are heavily cold-worked, and annealed to convert the deformation-induced martensite formed during cold rolling into austenite. The amount of reverted austenite is a function of annealing temperature. In this work, an AISI 301 metastable austenitic stainless steel is 90 pct cold-rolled and subsequently annealed at temperatures varying from 600 °C to 900 °C for a dwelling time of 30 minutes. The effects of annealing on the microstructure, average austenite grain size, martensite-to-austenite ratio, and carbide formation are determined. Analysis of the as-cold-rolled microstructure reveals that a 90 pct cold reduction produces a combination of lath type and dislocation cell-type martensitic structure. For the annealed samples, the average austenite grain size increases from 0.28 μm at 600 °C to 5.85 μm at 900 °C. On the other hand, the amount of reverted austenite exhibits a maximum at 750 °C, where austenite grains with an average grain size of 1.7 μm compose approximately 95 pct of the microstructure. Annealing temperatures above 750 °C show an increase in the amount of martensite. Upon annealing, (Fe, Cr, Mo)₂₃C₆ carbides form within the grains and at the grain boundaries.     

The influence of Mo2C morphology and distribution on the fatigue crack initiation and propagation behavior of Fe-C-Mo dual-phase steels

Dual-phase microstructures consisting of ferrite with carbides (Mo₂C) surrounding equiaxed martensite packets have been developed in two alloys, Fe-O. 2C-4Mo and Fe-O. 2C-2Mo. These alloys were chosen because of the presence of two distinct carbide morphologies: (1) a needle-shaped interphase carbide structure, and (2) a fibrous carbide structure. Isothermal transformations were used to control the carbide morphology and distribution in the ferritic regions of the dual-phase microstructures. In the present research the effects of changes in carbide structure on low cycle fatigue (LCF) and fatigue crack growth (FCG) behavior were studied. Crack initiation was observed at prior austenite grain boundaries in the fibrous microstructure, and along intrusion/extrusion defects in the interphase needle microstructures for LCF tests. TEM studies revealed a carbide free region at prior austenite grain boundaries where initiation occurs for the fibrous case. The cyclic stress/strain response of the ferritic portions of the microstructure is determined by the ability of the carbides to homogenize the strain found there. This affects the stress/strain distribution in the composite ferrite-martensite microstructure by changing the hardness ratio of the two phases and subsequently alters the fatigue crack growth behavior and the macroscopic cyclic stress/strain response. Strain localization was also found to affect the roughness induced closure found for fatigue crack growth tests for low R tests (R = 0.1).     

On the Relation between Carbide Density and Grain Boundary Character in Tempered Martensite Ferritic Steels

In the present study we investigate the microstructure of tempered martensite ferritic steels. It is well known that inside former austenite grains and inside packets of former martensite laths ultrafine micro grains (average size near: 1 μm) govern the strength of this material class. Micro grain boundaries are decorated by carbides (average size after creep near: 0.05 μm). However, in transmission electron micrographs it is commonly found that there are micro grain boundaries with a high carbide density while there are others where no carbides can be detected. In the present study we make an attempt to decide whether the crystallographic character of micro grain boundaries can be related to the number density of carbides at the boundaries. Kikuchi line diffraction patterns were used to determine the misorientation angle between two adjacent micro grains; we select only micro grain boundaries which represent <110> ‐ and <100> ‐ twist boundaries. A quantitative microstructural analysis was performed to determine the density of carbides on boundaries. Our results are discussed on the basis of general tendencies which were reported for grain boundaries in the literature.     

The microstructure and fracture of a carburized steel

The case microstructure and fracture of a coarse-grained 8620 steel carburized to 1 pet surface carbon are quite sensitive to austenitizing conditions. Reheating martensitic speci-mens below theA _cm produces in the case a refined austenitic grain size, a very fine mar-tensite, spherical carbide particles and a minimum of retained austenite and microcrack-ing. Overload fracture through the latter microstructure is transgranular and scanning electron microscopy shows both microvoid coalescence around thecarbide particles and an apparent fine cleavage in other areas. As-carburized specimens and specimens re-austenitized above theA _cm developed a case microstructure characterized by a coarse austenitic grain structure in which plate martensite with microcracks developed on cool-ing within a large amount of retained austenite. The overload fracture through this mi-crostructure followed a predominately intergranular path and effectively by-passed the retained austenite and microcracked martensite. Auger electron analysis showed that C and P were present on the intergranular fracture surfaces at concentrations above bulk, an observation consistent with literature reports of P segregation during austenitizing. This paper is based on a presentation made at a symposium on “Carburizing and Nitriding: Fundamentals, Processes and Properties” held at the Cincinnati Meeting of The Metallurgical Society of AIME, November 11 and 12, 1975 under the sponsorship of the Heat Treatment Committee.     

The rapid heat treatment of steel

The technique of austenitizing steel by heating rapidly through the Ac₁ to Ac₃ range, limiting the maximum temperature to the minimum required for complete austenitization and quenching immediately is discussed. Rapid austenitizing refines the austenite grain size if the initial microstructure is a fine aggregate, such as martensite or tempered martensite. Additional grain refinement usually results from two or more cycles and most steels hardenable by heat treatment become ultrafine grained and hence exhibit increased strength and toughness. Rapid austenitizing can also be applied, particularly to high-carbon steels, to develop a unique microstructure comprised of a uniform dispersion of very small carbide particles in an ultrafine grained martensitic matrix. This paper is based on a presentation made at a symposium on Altering the Time Cycle of Heat Treatment, held at the Philadelphia meeting of The Metallurgical Society of AIME, October 14, 1969, under the sponsorship of the IMD Heat Treatment Committee.     

Solidification mechanism of martensitic stainless steel

Abstract

In an unidirectional solidification experiment, an 8 kg stainless steel ingot with the composition 0·25%C, 17%Cr, and 1%Mn was solidified under continuous casting conditions. The dwell time of primary cooling was varied, followed by secondary spray cooling. Metallographic investigation, heat transfer, and segregation were carried out to study the solidification mechanism. The partition ratio of the elements present in ferrite and in austenite (martensite) was determined. It was indicated that the solidification follows: L → L + δ → L + δ + γ → δ + γ + carbides. Under high cooling rates γ austenite solidifies as a leading phase. The beginning of spray cooling has the main effect in controlling the obtained microstructures. Carbide thickening is observed in the rapidly cooled zone between the ferrite and the martensitic matrix. Tempered martensite increases by lowering the cooling rate, which gives more time for carbide dissolution and for carbon to diffuse into the ferrite, eventually increasing the austenite (martensite) fraction in the final matrix at the expense of ferrite.     

The effect of cooling rate on the microstructures formed during solidification of ferritic steel

This article describes in detail the effect of cooling rate on the microstructure of a low-carbon Fe-12 pct Cr alloy. The alloy was prepared using a relatively simple technique, i.e., rapid cooling of the melt in a copper wedge mold. The dependence of microstructure on the cooling rate (∼40 to 10⁵ K/s) has been determined by X-ray diffraction (XRD), microhardness measurement, optical microscopy (OM), and transmission electron microscopy (TEM). It has been found that the matrix structure over a large cooling rate range is composed of columnar ferrite grains, the size of which decreases with increasing cooling rate. Precipitation of second phases has been observed at either the ferrite grain boundaries or within the ferrite grains. The former takes place along the entire wedge sample, whereas the latter characterizes a region 12 mm away from the tip of the wedge sample. The essential structure of the grain boundary precipitates was identified as martensite, which is a transformation product of austenite precipitated at high temperatures. Retained austenite was identified at the tip region as isolated particles (<4 μm). The precipitates within the ferrite grains appeared as planar colonies consisting of two sets of needles. The density of these precipitates increases with increasing the cooling rate while their size decreases. Characteristic precipitate-free zones (PFZs) at the ferrite grain boundaries were observed and are discussed.     

Effect of Cyclic Thermal Process on Ultrafine Grain Formation in AISI 304L Austenitic Stainless Steel

As-received hot-rolled commercial grade AISI 304L austenitic stainless steel plates were solution treated at 1060 °C to achieve chemical homogeneity. Microstructural characterization of the solution-treated material revealed polygonal grains of about 85-μm size along with annealing twins. The solution-treated plates were heavily cold rolled to about 90 pct of reduction in thickness. Cold-rolled specimens were then subjected to thermal cycles at various temperatures between 750 °C and 925 °C. X-ray diffraction showed about 24.2 pct of strain-induced martensite formation due to cold rolling of austenitic stainless steel. Strain-induced martensite formed during cold rolling reverted to austenite by the cyclic thermal process. The microstructural study by transmission electron microscope of the material after the cyclic thermal process showed formation of nanostructure or ultrafine grain austenite. The tensile testing of the ultrafine-grained austenitic stainless steel showed a yield strength 4 to 6 times higher in comparison to its coarse-grained counterpart. However, it demonstrated very poor ductility due to inadequate strain hardenability. The poor strain hardenability was correlated with the formation of strain-induced martensite in this steel grade.     

The microstructural evolution,crystallography, and thermal processing of ultrahigh carbon Fe-1.85 pct C melt-spun ribbon

The microstructural evolution, mechanisms of grain refinement, crystallography, and thermal processing of a rapidly solidified Fe-1.85 pct C alloy have been studied by transmission electron microscopy (TEM). Melt-spun ribbons quenched in liquid nitrogen consist of carbide-free highly twinned martensite plates between 0.5-and 2.0-μm long and 0.1-and 0.5 -μm thick, with approximately 40 pct retained austenite also present. Ribbons tempered at 600 °C for 10 seconds consist of ferrite of approximately the same grain size and both intragranular and intergranular cementite precipitates. The intragranular cementite particles are about 0.1 /um or less in size and exhibit a single variant of the Bagaryatskii orientation relationship with respect to a given ferrite grain; the intergranular particles are about 0.1 μm in thickness and can be as long as 0.5 μm due to growth and/or coalescence along ferrite grain boundaries. A heat-treatment cycle investigated with a view toward generating structures suited for superplastic consolidation of the rapidly solidified ribbons consists of quenching the ribbon in liquid nitrogen, tempering at 600 °C for 10 seconds, “upquenching” to 750 °C (austenitizing) for 10 seconds, and subsequently quenching again in liquid nitrogen. This treatment results in martensite grains highly misoriented with respect to one another and typically 0.5 μm or less in both length and thickness and cementite particles 0.4 μm or less in size. (Occasionally, longer martensite plates were observed; but they never exceeded 1 μm in length.) The microstructures produced here offer the potential for producing fine-grained ultrahigh carbon steels of very high strength without the brittleness associated with the formation of coarse carbide particles or the loss of strength due to graphite formation. This investigation has thus provided the basis for follow-on studies currently underway in ultrahigh carbon Fe-C-Cr and Fe-C-Cr-Si steels, with the intent of producing similar microstructures which will also exhibit enhanced high-temperature stability.     

Microstructure and Property of Coarse Grain HAZ X80 Pipeline Steel

The coarse grain HAZ microstructure and property of X80 pipeline steel with different carbon content was investigated. The weld thermal simulation test was carried out on Gleeble 1500 thermal mechanical test machine. The Charpy tests were completed at --20 ℃ for evaluating the toughness of coarse grain heat affected zone （CGHAZ）. The microstructure was examined by optical microscope （OM） and transmission electron microscopy （TEM）, and the austenite constituent was quantified by X-ray diffraction. The results showed that the ultra-low carbon can improve the toughness of CGHAZ by suppressing the formation of carbide, decreasing the martensite austenite （M-A） constituent and increasing the residual austenite in the M A.     

奥氏体组织对低碳中锰钢冷弯性能的影响

摘要：采用冷弯直径0～60mm，弯曲角度180°，研究了20mm厚度低碳中锰钢的冷弯性能，冷弯后外表均无可见裂纹，判定合格。利用光学显微镜、扫描电镜、透射电镜、电子背散射衍射（EBSD）、X射线衍射仪等手段分析了显微组织，尤其是奥氏体组织在冷弯过程中对冷弯性能的影响。结果表明，冷弯前显微组织由板条马氏体和奥氏体组成，其中原始奥氏体晶界明显；冷弯直径为0mm变形后，样品弧顶部分奥氏体的体积分数由12.3%降至1.1%，维氏硬度由295HV1增至364HV1，晶粒尺寸由4.07μm增至4.30μm。主要原因是在冷弯过程在中奥氏体组织发生塑性变形，奥氏体晶界变形消失，沿冷弯方向呈拉伸带状组织形貌，冷弯形变时奥氏体发生TRIP效应显著。     

Microstructural evolution during laser cladding of M2 high-speed steel

Laser cladding of gas-atomized M2 high-speed steel on the mild steel substrate was performed using scan rates of 1 to 10 mm/s, scan line spacings of 0.1 to 0.5 mm, and powder feed rates of 1 to 10 g/min, for a given laser power of 400 W. This article presents a detailed study of the microstructural evolution during laser cladding. The effect of scan rate, scan line spacing, and powder feed rate on cooling rate can be described in terms of the cladding-layer thickness, i.e., the thinner the layer, the higher the cooling rate. The degree of metastability in the laser-clad microstructure can be understood in terms of the lattice parameter of the bcc phase. The lattice parameter of the bcc phase increased with increasing layer thickness and reached a maximum value at a thickness of 0.3 mm. Correspondingly, the microstructure varied from a cellular or dendritic structure of δ ferrite and austenite to a mixture of martensite and retained austenite. However, further increasing the layer thickness led to a decrease of both the lattice parameters of the bcc phase and the proportion of retained austenite in the martensite. This was accompanied by an increase of the amount of carbide at the prior austenitic grain boundaries and a decrease of the carbon content in the martensite and retained austenite.     

Reverse Martensitic Transformation and Resulting Microstructure in a Cold Rolled Metastable Austenitic Stainless Steel

The reverse martensitic transformation in cold‐rolled metastable austenitic stainless steel has been investigated via heat treatments performed for various temperatures and times. The microstructural evolution was evaluated by differential scanning calorimetry, X‐ray diffraction and microscopy. Upon heat treatment, both diffusionless and diffusion‐controlled mechanisms determine the final microstructure. The diffusion reversion from α′‐martensite to austenite was found to be activated at about 450°C and the shear reversion is activated at higher temperatures with A_f′ ~600°C. The resulting microstructure for isothermal heat treatment at 650°C was austenitic, which inherits the α′‐martensite lath morphology and is highly faulted. For isothermal heat treatments at temperatures above 700°C the faulted austenite was able to recrystallize and new austenite grains with a low defect density were formed. In addition, carbo‐nitride precipitation was observed for samples heat treated at these temperatures, which leads to an increasing M_s‐temperature and new α′‐martensite formation upon cooling.     

Microstructural investigation of a rapidly solidified 12Cr-Mo-V steel

Rapidly solidified martensitic stainless steel (11.59Cr-0.98Mo-0.28V (in wt pct) ribbons have been produced by the melt-spinning process. The microstructure of the ribbons showed three distinct zones: a columnar, a cellular, and a cellular-dendritic zone. The height of the columnar grain zone is independent of the process parameters such as the wheel material or the wheel velocity. Due to a high level of undercooling and a high growth velocity of the solid/liquid interface, the rapid solidification process is found to suppress the formation of δ-ferrite and enhance the formation of austenite. The austenite is transformed into martensite upon cooling. In comparison with conventional solidification, a reduction in the initial austenite grain size has been found to result in a very fine lath martensite (M) structure. Investigations of the texture within the ribbons along the growth direction show a weak fiber texture. Transmission electron microscopy (TEM) has revealed a [111]_M1 ‖ [001]_M2 and (011)_M1 ‖ (110)_M2 orientation relationship between two neighboring martensite laths. The observed orientation relationship is a result of a superposition of both the Kurdjumov-Sachs (K-S) and Nishiyama-Wasserman (N-W) orientation relations.     

Stability and Constitutive Modelling in Multiphase TRIP Steels

Multiphase TRIP steels are a relatively new class of steels exhibiting excellent combinations of strength and cold formability, a fact that renders them particularly attractive for automotive applications. The present work reports models regarding the prediction of the stability of retained austenite, the optimisation of the heat‐treatment stages necessary for austenite stabilization in the microstructure, as well as the mechanical behaviour of these steels under deformation. Austenite stability against mechanically‐induced transformation to martensite depends on chemical composition, austenite particle size, strength of the matrix and stress state. The stability of retained austenite is characterized by the M^σ_S temperature, which can be expressed as a function of the aforementioned parameters by an appropriate model presented in this work. Besides stability, the mechanical behaviour of TRIP steels also depends on the amount of retained austenite present in the microstructure. This amount is determined by the combinations of temperature and temporal duration of the heat‐treatment stages undergone by the steel. Maximum amounts of retained austenite require optimisation of the heat‐treatment conditions. A physical model is presented in this work, which is based on the interactions between bainite and austenite during the heat‐treatment of multiphase TRIP steels, and which allows for the selection of treatment conditions leading to the maximization of retained austenite in the final microstructure. Finally, a constitutive micromechanical model is presented, which describes the mechanical behaviour of multiphase TRIP steels under deformation, taking into account the different plastic behaviour of the individual phases, as well as the evolution of the microstructure itself during plastic deformation. This constitutive micromechanical model is subsequently used for the calculation of forming limit diagrams (FLD) for these complex steels, an issue of great practical importance for the optimisation of stretch‐forming and deep‐drawing operations.     

Elementary Transformation and Deformation Processes and the Cyclic Stability of NiTi and NiTiCu Shape Memory Spring Actuators

The present work addresses functional fatigue of binary NiTi and ternary NiTiCu (with 5, 7.5, and 10 at. pct Cu) shape memory (SM) spring actuators. We study how the alloy composition and processing affect the actuator stability during thermomechanical cycling. Spring lengths and temperatures were monitored and it was found that functional fatigue results in an accumulation of irreversible strain (in austenite and martensite) and in increasing martensite start temperatures. We present phenomenological equations that quantify both phenomena. We show that cyclic actuator stability can be improved by using precycling, subjecting the material to cold work, and adding copper. Adding copper is more attractive than cold work, because it improves cyclic stability without sacrificing the exploitable actuator stroke. Copper reduces the width of the thermal hysteresis and improves geometrical and thermal actuator stability, because it results in a better crystallographic compatibility between the parent and the product phase. There is a good correlation between the width of the thermal hysteresis and the intensity of irrecoverable deformation associated with thermomechanical cycling. We interpret this finding on the basis of a scenario in which dislocations are created during the phase transformations that remain in the microstructure during subsequent cycling. These dislocations facilitate the formation of martensite (increasing martensite start (M _S ) temperatures) and account for the accumulation of irreversible strain in martensite and austenite.     

Effect of simulated thermal cycles on the microstructure of the heat-affected zone in HSLA-80 and HSLA-100 steel plates

The influence of weld thermal simulation on the transformation kinetics and heat-affected zone (HAZ) microstructure of two high-strength low-alloy (HSLA) steels, HSLA-80 and HSLA-100, has been investigated. Heat inputs of 10 kJ/cm (fast cooling) and 40 kJ/cm (slow cooling) were used to generate single-pass thermal cycles with peak temperatures in the range of 750 °C to 1400 °C. The prior-austenite grain size is found to grow rapidly beyond 1100 °C in both the steels, primarily with the dissolution of niobium carbonitride (Nb(CN)) precipitates. Dilatation studies on HSLA-80 steel indicate transformation start temperatures (T _s ) of 550 °C to 560 °C while cooling from a peak temperature (T _p ) of 1000 °C. Transmission electron microscopy studies show here the presence of accicular ferrite in the HAZ. The T _s value is lowered to 470 °C and below when cooled from a peak temperature of 1200 °C and beyond, with almost complete transformation to lath martensite. In HSLA-100 steel, the T _s value for accicular ferrite is found to be 470 °C to 490 °C when cooled from a peak temperature of 1000 °C, but is lowered below 450 °C when cooled from 1200 °C and beyond, with correspondingly higher austenite grain sizes. The transformation kinetics appears to be relatively faster in the fine-grained austenite than in the coarse-grained austenite, where the niobium is in complete solid solution. A mixed microstructure consisting of accicular ferrite and lath martensite is observed for practically all HAZ treatments. The coarse-grained HAZ (CGHAZ) of HSLA-80 steel shows a higher volume fraction of lath martensite in the final microstructure and is harder than the CGHAZ of HSLA-100 steel.     

Effect of simulated thermal cycles on the microstructure of the heat-affected zone in HSLA-80 and HSLA-100 steel plates

The influence of weld thermal simulation on the transformation kinetics and heat-affected zone (HAZ) microstructure of two high-strength low-alloy (HSLA) steels, HSLA-80 and HSLA-100, has been investigated. Heat inputs of 10 kJ/cm (fast cooling) and 40 kJ/cm (slow cooling) were used to generate single-pass thermal cycles with peak temperatures in the range of 750 °C to 1400 °C. The prior-austenite grain size is found to grow rapidly beyond 1100 °C in both the steels, primarily with the dissolution of niobium carbonitride (Nb(CN)) precipitates. Dilatation studies on HSLA-80 steel indicate transformation start temperatures (T _s ) of 550 °C to 560 °C while cooling from a peak temperature (T _p ) of 1000 °C. Transmission electron microscopy studies show here the presence of accicular ferrite in the HAZ. The T _s value is lowered to 470 °C and below when cooled from a peak temperature of 1200 °C and beyond, with almost complete transformation to lath martensite. In HSLA-100 steel, the T _s value for accicular ferrite is found to be 470 °C to 490 °C when cooled from a peak temperature of 1000 °C, but is lowered below 450 °C when cooled from 1200 °C and beyond, with correspondingly higher austenite grain sizes. The transformation kinetics appears to be relatively faster in the fine-grained austenite than in the coarse-grained austenite, where the niobium is in complete solid solution. A mixed microstructure consisting of accicular ferrite and lath martensite is observed for practically all HAZ treatments. The coarse-grained HAZ (CGHAZ) of HSLA-80 steel shows a higher volume fraction of lath martensite in the final microstructure and is harder than the CGHAZ of HSLA-100 steel.     

Correlation of the microstructure and fracture toughness of the heat-affected zones of an SA 508 steel

In this study, microstructures of a heat-affected zone (HAZ) of an SA 508 steel were identified by Mossbauer spectroscopy in conjunction with microscopic observations, and were correlated with fracture toughness. Specimens with the peak temperature raised to 1350 °C showed mostly martensite. With the peak temperature raised to 900 °C, the martensite fraction was reduced, while bainite or martensite islands were formed because of the slow cooling from the lower austenite region and the increase in the prior austenite grain size. As the martensite fraction present inside the HAZ increased, hardness and strength tended to increase, whereas fracture toughness decreased. The microstructures were not changed much from the base metal because of the minor tempering effect when it was raised to 650 °C or 700 °C. However, fracture toughness of the subcritical HAZ with the peak temperature raised to 650 °C to 700 °C was seriously reduced after postweld heat treatment (PWHT) because carbide particles were of primary importance in initiating voids. Thus, the most important microstructural factors affecting fracture toughness were the martensite fraction before PWHT and the carbide fraction after PWHT.     

High Temperature Deformation-Induced Transformation in Nb-Bearing Medium Mn Steel

Dynamic transformation (DT) of deformed austenite to ferrite at temperatures above A_e3 occurs during a multi-step hot torsion test of a Nb-bearing medium manganese steel. In torsion tested specimens, equiaxed grains are dispersed within a martensite matrix, and the average grain size is less than 1 μm. Electron back-scattering diffraction results confirm that most of the equiaxed grains are recrystallized ferrite, and there is a small fraction of retained austenite.