Recrystallization Behavior of a Heavily Deformed Austenitic Stainless Steel During Iterative Type Annealing

The study describes evolution of the recrystallization microstructure in an austenitic stainless steel during iterative or repetitive type annealing process. The starting heavily cold deformed microstructure consisted of a dual phase structure i.e., strain-induced martensite (SIM) (43 pct in volume) and heavily deformed large grained retained austenite. Recrystallization behavior was compared with Johnson Mehl Avrami and Kolmogorov model. Early annealing iterations led to reversion of SIM to reversed austenite. The microstructure changes observed in the retained austenite and in the reverted austenite were mapped by electron backscatter diffraction technique and transmission electron microscope. The reversed austenite was characterized by a fine polygonal substructure consisting of low-angle grain boundaries. With an increasing number of annealing repetitions, these boundaries were gradually replaced by high-angle grain boundaries and recrystallized into ultrafine-grained microstructure. On the other hand, recrystallization of retained austenite grains was sluggish in nature. Progress of recrystallization in these grains was found to take place by a gradual evolution of subgrains and their subsequent transformation into fine grains. The observed recrystallization characteristics suggest continuous recrystallization type process. The analysis provided basic insight into the recrystallization mechanisms that enable the processing of ultrafine-grained fcc steels by iterative type annealing. Tensile properties of the processed material showed a good combination of strength and ductility.     

Microstructural stability of ultrafine grained low-carbon steel containing vanadium fabricated by intense plastic straining

Two grades of low-carbon steel, one containing vanadium and the other without vanadium, were subjected to equal channel angular pressing (ECAP) at 623 K up to an effective strain of ∼4. After equal channel angular pressing, a static annealing treatment for 1 hour was undertaken on both pressed steels in the temperature range of 693 to 873 K. By comparing the microstructural evolution during annealing and the tensile properties of the two steels, the effect of the addition of vanadium on the thermal stability of ultrafine-grained (UFG) low-carbon steel fabricated by intense plastic straining was examined. For the steel without vanadium, coarse recrystallized ferrite grains appeared at annealing temperatures above 753 K, and a resultant degradation of the strength was observed. For the steel containing vanadium, submicrometer-order ferrite grain size and ultrahigh strength were preserved up to 813 K. The enhanced thermal and mechanical stabilities of the steel containing vanadium were attributed to its peculiar microstructure, which consisted of ill-defined pearlite colonies and ultrafine ferrite grains with uniformly distributed nanometer-sized cementite particles. This microstructure resulted from the combined effects of (a) the preservation of high dislocation density providing an effective diffusion path, due to the effect of vanadium on increasing the recrystallization temperature of the steel; and (b) precipitation of fine cementite particles at ferrite grain boundaries through the enhanced diffusion of carbon atoms (which were dissolved from pearlitic cementite by severe plastic straining) along ferrite grain boundaries and dislocation cores.     

Influences of Austenization Temperature and Annealing Time on Duplex Ultrafine Microstructure and Mechanical Properties of Medium Mn Steel

A duplex ultrafine microstructure in a medium manganese steel(0.2C-5Mn)was produced by austenite reverted transformation annealing(ART-annealing).The microstructural evolution during annealing was examined by scanning electron microscopy(SEM),transmission electron microscopy(TEM)and X-ray diffraction(XRD).Based on the microstructure examination,it was found that some M3 C type carbides appeared in the martensitic matrix at the beginning of the ART-annealing.But with further increasing annealing time,these carbides would be dissolved and finally disappeared.Meanwhile,the austenite lath was developed in the ART-annealing process and the volume fraction of austenite increased with the increase of the annealing time,which resulted in a duplex microstructure consisting of ultrafine-grained ferrite and large fraction of reverted austenite after long time annealing.The mechanical property examinations by uniaxial tensile tests showed that ART-annealing(6h,650 ℃)resulted in a superhigh product of strength to elongation up to 42GPa·%.     

Recrystallization kinetics of an austenitic high-manganese steel subjected to severe plastic deformation

The evolution of the microstructure and the properties of an austenitic high-manganese steel subjected to severe deformation by cold rolling and subsequent recrystallization annealing is investigated. Cold rolling is accompanied by mechanical structural twinning and shear banding. The microhardness and microstructural analysis of annealed samples are used to study the recrystallization kinetics of the high-manganese steel. It is shown that large plastic deformation and subsequent annealing result in rapid development of recrystallization processes and the formation of an ultrafine-grained structure. A completely recrystallized structure with an average grain size of 0.64 μm forms after 30-min annealing at a temperature of 550°C. No significant structural changes are observed when the annealing time increases to 18 h, which indicates stability of the recrystallized microstructure. The steel cold rolled to 90% and annealed at 550°C for 30 min demonstrates very high strength properties: the yield strength and the tensile strength achieve 650 and 850MPa, respectively. The dependence of the strength properties of the steel on the grain size formed after rolling and recrystallization annealing is described by the Hall–Petch relation.     

Effect of Annealing on Thermal Stability, Precipitate Evolution, and Mechanical Properties of Cryorolled Al 7075 Alloy

The effect of annealing on microstructural stability, precipitate evolution, and mechanical properties of cryorolled (CR) Al 7075 alloy was investigated in the present work employing hardness measurements, tensile test, X-ray diffraction (XRD), differential scanning calorimetry (DSC), electron backscattered diffraction (EBSD), and transmission electron microscopy (TEM). The solution-treated bulk Al 7075 alloy was subjected to cryorolling to produce fine grain structures and, subsequently, annealing treatment to investigate its thermal stability. The recrystallization of CR Al 7075 alloys started at an annealing temperature of 423 K (150 °C) and completed at an annealing temperature of 523 K (250 °C). The CR Al 7075 alloys with ultrafine-grained microstructure are thermally stable up to 623 K (350 °C). Within the range of 523 K to 623 K (250 °C to 350 °C), the size of small η phase particles and AlZr₃ dispersoids lies within 300 nm. These small precipitate particles pin the grain boundaries due to the Zener pinning effect, which suppresses grain growth. The hardness and tensile strength of the CR Al 7075 alloys was reduced during the annealing treatment from 423 K to 523 K (150 °C to 250 °C) and subsequently it remains constant.     

Deformation and Damage Mechanisms in Ultrafine-Grained Austenitic Stainless Steel During Cyclic Straining

The ultrafine-grained (UFG) structure of an austenitic stainless steel (Type 301LN), processed by controlled phase-reversion annealing, was fatigued to study the deformation and damage mechanisms during cyclic straining. Fatigue cracking along the grain boundaries and the formation of extended persistent slip band-like shear bands (SBs) were observed to be the fatigue-induced microstructural features in the ultrafine-grained structure. Characterization of SBs was performed by electron backscattered diffraction and atomic force microscopy to study the fine features.     

On the Effect of Manganese on Grain Size Stability and Hardenability in Ultrafine-Grained Ferrite/Martensite Dual-Phase Steels

Two plain carbon steels with varying manganese content (0.87 wt pct and 1.63 wt pct) were refined to approximately 1 μm by large strain warm deformation and subsequently subjected to intercritical annealing to produce an ultrafine grained ferrite/martensite dual-phase steel. The influence of the Mn content on microstructure evolution is studied by scanning electron microscopy (SEM). The Mn distribution in ferrite and martensite is analyzed by high-resolution electron backscatter diffraction (EBSD) combined with energy dispersive X-ray spectroscopy (EDX). The experimental findings are supported by the calculated phase diagrams, equilibrium phase compositions, and the estimated diffusion distances using Thermo-Calc (Thermo-Calc Software, McMurray, PA) and Dictra (Thermo-Calc Software). Mn substantially enhances the grain size stability during intercritical annealing and the ability of austenite to undergo martensitic phase transformation. The first observation is explained in terms of the alteration of the phase transformation temperatures and the grain boundary mobility, while the second is a result of the Mn enrichment in cementite during large strain warm deformation, which is inherited by the newly formed austenite and increases its hardenability. The latter is the main reason why the ultrafine-grained material exhibits a hardenability that is comparable with the hardenability of the coarse-grained reference material.     

Texture Evaluation of a Bi-Modal Structure During Static Recrystallization of Hot-Deformed Mg-Al-Sn Alloy

In this study, Mg-Al-Sn alloy was hot compressed at 523 K (250 °C) and annealed at 623 K (350 °C) for various times. The initial as-deformed microstructure was partially dynamic recrystallized with strain-induced precipitates on the recrystallized grain boundaries. After annealing at 623 K (350 °C), static recrystallization (SRX) of the bimodal microstructure took place where, at this temperature, no static precipitates formed. The goal of this work was to study the effect of dynamic precipitation on the texture evolution during the SRX process. Progressive texture evolution was studied during annealing by electron backscattered diffraction technique through a microstructure-tracking process. It was found that the grain-coarsening mechanism during the early stage of annealing is not totally controlled by the basal-oriented grains. Also, it was found that the dynamic precipitates may have significant influence in the early texture weakening during annealing of a bimodal structure.     

连续退火温度对高硅双相钢组织及性能影响

 用连续退火模拟试验机,在实验室试制了冷轧高硅DP590,并通过扫描电镜、EBSD、透射电镜和力学性能测试研究了不同退火温度（735~835℃）对其组织和力学性能的影响。结果表明：退火温度对高硅双相钢强度和塑性有重要的影响,当退火温度为785℃时,材料获得良好的综合力学性能。不同温度退火后得到的组织均为铁素体和均匀分布在其晶界上的岛状马氏体;利用EBSD技术清晰地观察到离散分布于铁素体和马氏体晶界处的残余奥氏体。运用透射电镜观察到马氏体周围的位错线及位错团,这是双相钢连续屈服特性的重要保障。     

Thermal stability in bulk cryomilled ultrafine-grained 5083 Al alloy

Thermal stability in bulk ultrafine-grained (UFG) 5083 Al that was processed by gas atomization followed by cryomilling, consolidation, and extrusion, and that exhibited an average grain size of 305 nm, was investigated in the temperature range of 473 to 673 K (0.55 to 0.79 T _m , where T _m is the melting temperature of the material) for different annealing times. Appreciable grain growth was observed at temperatures > 573 K, whereas there was limited grain growth at temperatures < 573 K even after long annealing times. The values of the grain growth exponent, n, deduced from the grain growth data were higher than the value of 2 predicted from elementary grain growth theories. The discrepancy was attributed to the operation of strong pinning forces on boundaries during the annealing treatment. An examination of the microstructure of the alloy suggests that the origin of the pinning forces is most likely related to the presence of dispersion particles, which are mostly introduced during cryomilling. Two-grain growth regimes were identified: the low-temperature region (<573 K) and the high-temperature region (>573 K). For temperatures lower than 573 K, the activation energy of 25 ± 5 kJ/mol was determined. It is suggested that this low activation energy represents the energy for the reordering of grain boundaries in the UFG material. For temperatures higher than 573 K, an activation energy of 124 ± 5 kJ/mol was measured. This value of activation energy, 124 ± 5 kJ/mol, lies between that for grain boundary diffusion and lattice diffusion in analogous aluminum polycrystalline systems. The results show that the strength and ductility of bulk UFG 5083 Al, as obtained from tensile tests, correlate well with substructural changes introduced in the alloy by the annealing treatment.     

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.     

Annealing behavior of submicrocrystalline oxide-bearing iron produced by mechanical alloying

The structural changes upon annealing of an ultrafine-grained iron containing dispersed oxides were studied. The starting material was subjected to mechanical milling followed by consolidating bar rolling. The fine-grained microstructures were essentially stable against discontinuous grain growth and/or primary recrystallization during annealing at temperatures up to 800 °C, where the specimens maintain a very fine ferrite grain size. The annealing behavior is mainly characterized by normal grain growth accompanied by recovery. The grain-growth kinetics correlates with the oxide coarsening. Both the grain growth and the oxide coarsening can be enhanced by an increase in the temperature. The static restoration/recrystallization processes operating in the ultrafine-grained matrices, as well as the effect of dispersed oxides particles, are discussed in some detail.     

Effect of silicon carbide nanoparticles on hot deformation of ultrafine-grained aluminium nanocomposites prepared by hot powder extrusion process

The flow behaviour of Al–SiC nanocomposites prepared by mechanical milling and hot powder extrusion methods was studied at different temperatures (350–500°C) and strain rates (0.005–0.5 s^?1). The flow of the Powder metallurgy nanocomposites exhibited a peak stress followed by a dynamic flow softening behaviour. It was shown that mechanical milling increased high-temperature strain rate sensitivity of ultrafine-grained (UFG) aluminium while decreasing its flow dependence to temperature. Constitutive analysis of the hot deformation process by Zener–Hollomon parameter (Z) also indicated a remarkable increase in the deformation activation energy (about 40%). Likewise, SiC nanoparticles (up to 2vol.-%) were shown to contribute in the high-temperature strengthening of UFG aluminium with a significant effect on its thermal stability. The findings were explained based on the pinning effect of hard nanoparticles on grain boundaries and mobile dislocations as well as microstructure stabilisation at elevated temperatures.     

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.     

On the Microstructural Stability of Ultrafine-Grained Interstitial-Free Steel under Cyclic Loading

The microstructural stability of ultrafine-grained (UFG) interstitial-free (IF) steel under cyclic loading was investigated. The samples were extracted from material processed along two different equal channel angular extrusion (ECAE) routes (4C and 4E) at room temperature. Low-cycle fatigue tests were carried out in addition to electron and optical microscopy in order to characterize the microstructural evolution induced by cyclic deformation. The results revealed substantial differences in microstructure resulting from different processing routes. Specifically, the volume fraction of high-angle grain boundaries (HAGBs) and low-angle grain boundaries (LAGBs) varied significantly depending on the processing route. The different microstructural characteristics stemming from different ECAE routes expressively influence the fatigue response. Route-4C-processed material displays cyclic softening, while processing along route 4E leads to microstructural stability under cyclic loading. This highly route-dependent trend in the cyclic stress-strain response is attributed to the instability of the LAGBs and stability of HAGBs during cyclic deformation, which is further supported by electron backscattering diffraction results. This article is based on a presentation made in the symposium entitled “Ultrafine-Grained Materials: from Basics to Application,” which occurred September 25–27, 2006 in Kloster Irsee, Germany.     

The microstructure of rolled and annealed tungsten rod

This paper reports a study of the microstructural changes that occur when potassium-doped tungsten ingots are rolled at elevated temperatures. The effect of annealing on the microstructure of the rolled material is also considered. All samples were rolled on a Kocks mill. At low levels of deformation, the grain boundaries are primarily high-angle boundaries, and many grains are dislocation free. Both of these features probably result from dynamic recrystallization during rolling. As deformation increases, the grains become more elongated, and more low-angle boundaries are found within the material. Also, the potassium gets drawn into narrower and longer tubes. When these rolled rods are annealed at temperatures between 1275 ‡C and 1950 ‡C, several changes occur in the microstructure. The material undergoes abnormal grain growth. The temperature at which this occurs depends on the length of the anneal, the amount of de-formation the rod has received, and the spatial location in the rod. This spatial distribution most likely results from strain gradients that exist in the rolled rod. The abnormal grain growth is accompanied by a decrease in hardness. The potassium-containing tubes in the rod also break up into bubbles during annealing. The temperature at which this breakup occurs again depends on the length of the anneal and the amount of deformation.     

Microstructural evolution during the austenite-to-ferrite transformation from deformed austenite

It is well established that the ferrite grain size of low-carbon steel can be refined by hot rolling of the austenite at temperatures below the nonrecrystallization temperature (T _nr ). The strain retained in the austenite increases the number of ferrite nuclei present in the initial stages of transformation. In this work, a C-Mn-Nb steel has been heavily deformed by torsion at temperatures below the determined T _nr for this steel. After deformation, specimens are cooled at a constant cooling rate of 1 °C/s, and interrupted quenching at different temperatures is used to observe different stages of transformation. The transformation kinetics and the evolution of the ferrite grain size have been analyzed. It has been shown that the stored energy due to the accumulated deformation is able to influence the nucleation for low undercoolings by acting on the driving force for transformation; this influence becomes negligible as the temperature decreases. At the early stages of transformation, it has been observed that the preferential nucleation sites of ferrite are the austenite grain boundaries. At the later stages, when impingement becomes important, ferrite coarsening accompanies the transformation and a significant reduction in the number of the ferrite grains per unit volume is observed. As a result, a wide range of ferrite grain sizes is present in the final microstructure, which can influence the mechanical properties of the steel.     

Annealing Temperature Dependence of the Tensile Behavior of 10 pct Mn Multi-phase TWIP-TRIP Steel

In the present study, the relationship between the microstructure and the mechanical properties of Fe-10 pct Mn-3 pct Al-2 pct Si-0.3 pct C multi-phase steel was investigated. The 10 pct Mn multi-phase steel exhibits a combination of high tensile strength and enhanced ductility resulting from deformation-twinning and strain-induced transformation occurring in succession. A pronounced intercritical annealing temperature dependence of the tensile behavior was observed. The annealing temperature dependence of the retained austenite volume fraction, composition, and the grain size was analyzed experimentally, and the effect of the microstructural parameters on the kinetics of mechanical twinning and strain-induced martensite formation was quantified. A dislocation density-based constitutive model was developed to predict the mechanical properties of 10 pct Mn multi-phase steel. The model also allows for the determination of the critical strain for dynamic strain aging effect.