Study of the austempering transformation kinetics in compacted graphite cast irons

In this work, the phases involved in the transformation austenite→ferrite+high-carbon austenite in cast irons were assessed by means of Mössbauer spectroscopy and hardness measurements for samples austempered at five different temperatures between 573 and 673 K with two Mn contents. The C content in the high-carbon austenite was found to have a dependence of t ^0.40±0.05 on the austempering time t, which evidences that diffusion of carbon has taken place. The kinetic parameter k determined using the Johnson-Mehl-Avrami equation has a maximum of 3.9×10^?3 (s^?1) at ≈623 K and corroborates that Mn slows the transformation rate.     

Effect of Retained Austenite on the Fracture Toughness of Quenching and Partitioning (Q&P)-Treated Sheet Steels

Fracture toughness K _IC was measured by double edge-notched tension (DENT) specimens with fatigue precracks on quenching and partitioning (Q&P)-treated high-strength (ultimate tensile strength [UTS] superior to 1200 MPa) sheet steels consisting of 4 to 10 vol pct of retained austenite. Crack extension force, G _IC, evaluated from the measured K _IC, is used to analyze the role of retained austenite in different fracture behavior. Meanwhile, G _IC is deduced by a constructed model based on energy absorption by martensite transformation (MT) behavior of retained austenite in Q&P-treated steels. The tendency of the change of two results is in good agreement. The Q&P-treated steel, quenched at 573 K (300 °C), then partitioned at 573 K (300 °C), holding for 60 seconds, has a fracture toughness of 74.1 MPa·m^1/2, which is 32 pct higher than quenching and tempering steel (55.9 MPa·m^1/2), and 16 pct higher than quenching and austempering (QAT) steel (63.8 MPa·m^1/2). MT is found to occur preferentially at the tips of extension cracks on less stable retained austenite, which further improves the toughness of Q&P steels; on the contrary, the MT that occurs at more stable retained austenite has a detrimental effect on toughness.     

Thermally Stable Ni-rich Austenite Formed Utilizing Multistep Intercritical Heat Treatment in a Low-Carbon 10 Wt Pct Ni Martensitic Steel

Austenite reversion and its thermal stability attained during the transformation is key to enhanced toughness and blast resistance in transformation-induced-plasticity martensitic steels. We demonstrate that the thermal stability of Ni-stabilized austenite and kinetics of the transformation can be controlled by forming Ni-rich regions in proximity of pre-existing (retained) austenite. Atom probe tomography (APT) in conjunction with thermodynamic and kinetic modeling elucidates the role of Ni-rich regions in enhancing growth kinetics of thermally stable austenite, formed utilizing a multistep intercritical (Quench-Lamellarization-Tempering (QLT)-type) heat treatment for a low-carbon 10 wt pct Ni steel. Direct evidence of austenite formation is provided by dilatometry, and the volume fraction is quantified by synchrotron X-ray diffraction. The results indicate the growth of nm-thick austenite layers during the second intercritical tempering treatment (T-step) at 863 K (590 °C), with austenite retained from first intercritical treatment (L-step) at 923 K (650 °C) acting as a nucleation template. For the first time, the thermal stability of austenite is quantified with respect to its compositional evolution during the multistep intercritical treatment of these steels. Austenite compositions measured by APT are used in combination with the thermodynamic and kinetic approach formulated by Ghosh and Olson to assess thermal stability and predict the martensite-start temperature. This approach is particularly useful as empirical relations cannot be extrapolated for the highly Ni-enriched austenite investigated in the present study.     

Kinetics of Martensite Formation in Substitutional Fe-Al Alloys: Dilatometric Analysis

High-resolution differential dilatometry was employed to study the kinetics of the martensite formation upon isochronal cooling/quenching of substitutional Fe-(0.5, 0.7, and 1.0) at. pct Al alloys at fast cooling/quenching rates in the range of 17 K (17 °C) through 100 K (100 °C) s^?1, with an emphasis on the as-yet unexpected influence of cooling/quenching rate. The martensite transformation initiated at nearly the same temperature (i.e., the $ M_{\text{S}} $ temperature) in the ferrite-phase region for all cooling/quenching rates applied, which indicates athermal nucleation: the chemical driving force governs the initiation of the nucleation of the martensite plates. Variation of the cooling/quenching rates revealed two principal kinetic features: both the temperature ranges passed during transformation and the grain size of the product martensite increase with the increase of cooling/quenching rates. A modular phase-transformation model, incorporating a classic partitioning analysis for nucleation and anisotropic growth for impingement, has been employed to extract the velocity of the migrating martensite/austenite interface from the dilatometric data. The thus obtained velocity of the martensite/austenite interface as function of temperature indicates a thermally activated growth governed by relatively lower activation energy, as determined by evaluation of the martensite-formation-rate maximum as function of cooling/quenching rate.     

低于Ms温度变形对等温贝氏体相变动力学和组织的影响

摘要：变形和等温热处理是高强贝氏体钢主要生产工艺,已有研究表明低于马氏体相变起始温度（Ms）的等温热处理可以促进贝氏体相变动力学,低温奥氏体预变形也可以加速贝氏体相变。研究了低于Ms温度变形对后续等温贝氏体相变动力学和组织的影响,结果表明,并未出现预想的加速相变叠加效应,反而,变形温度低于Ms温度时,贝氏体相变动力学减弱,等温贝氏体相变孕育期延长。低于Ms温度等温相变时,贝氏体铁素体与母相奥氏体位向关系接近K-S关系,变形试样虽然获得了一部分先马氏体,且能提高贝氏体形核率,但并非所有的胚核都能发生长大,变形改变母相奥氏体取向,使贝氏体原本的位向关系遭受破坏,导致有效形核率降低。     

Mechanism of Dynamic Strain Aging in a Niobium-Stabilized Austenitic Stainless Steel

Dynamic strain aging (DSA) behavior of a niobium (Nb)-stabilized austenitic stainless steel (TP347H) was studied from room temperature (RT) to 973 K via tensile testing, transmission electron microscopy (TEM), and internal friction (IF) measurements. The DSA effect is nearly negligible from 573 K to 673 K, and it becomes significant at temperatures between 773 K and 873 K with strain rates of 3 × 10^?3 s^?1, 8 × 10^?4 s^?1, and 8 × 10^?5 s^?1, respectively. The results indicate that a dislocation planar slip is dominant in the strong DSA regime. The Snoek-like peak located at 625 K is highly sensitive to the diffusion of free carbon (C) atoms in solid solution. C-Nb octahedrons are formed by C chemical affinity to substitutional Nb solute atoms. Octahedron structure is very stable and captures most free C atoms and inhibits DSA at low tensile test temperatures of 573 K to 673 K. At high test temperatures in the range from 773 K to 873 K, C-Nb octahedrons break up and release free C and Nb atoms, resulting in the stronger Snoek-like peak. The interaction between C atoms and dislocations is responsible for DSA at low temperatures ranging from 573 K to 673 K. At higher temperature of 773 K to 873 K, the Cr and Nb atoms lock the dislocations, and this formation contributes to DSA.     

Simulation of Ferrite Formation in Fe-C Alloys Based on a Three-Dimensional Mixed-Mode Transformation Model

A three-dimensional mixed-mode (MM) transformation model accounting for both soft impingement and hard impingement was developed that calculates the growth kinetics of ferrite grains in an austenite matrix. The simulations are compared to the kinetics of ferrite formation in high-purity Fe-C alloys for which phase-transformation kinetics were measured isothermally by dilatometry at several temperatures in the range of 973 K to 1043 K (700 °C to 770 °C). The interface mobility is obtained from the best fit of the data at 1023 K (750 °C) for which the nucleus density N is estimated from the final microstructure. Subsequently, the experimental ferrite kinetics in Fe-0.36C at the other temperatures are simulated. The values of N extracted from the fits can be described with a nucleation model. The significance of the MM calculations is rationalized by comparing the results for Fe-0.17C with simulations assuming purely diffusion-controlled (DC) and purely interface-controlled (IC) growth. Comparison of simulated fraction curves for Fe-0.57C with the three models demonstrates that the transformation in high-carbon steels is essentially DC.     

Microstructure Evolution and Mechanical Behavior of a Hot-Rolled High-Manganese Dual-Phase Transformation-Induced Plasticity/Twinning-Induced Plasticity Steel

The microstructures and deformation behavior were studied in a high-temperature annealed high-manganese dual-phase (28 vol pct δ-ferrite and 72 vol pct γ-austenite) transformation-induced plasticity/twinning-induced plasticity (TRIP/TWIP) steel. The results showed that the steel exhibits a special Lüders-like yielding phenomenon at room temperature (RT) and 348 K (75 °C), while it shows continuous yielding at 423 K, 573 K and 673 K (150 °C, 300 °C and 400 °C) deformation. A significant TRIP effect takes place during Lüders-like deformation at RT and 348 K (75 °C) temperatures. Semiquantitative analysis of the TRIP effect on the Lüders-like yield phenomenon proves that a softening effect of the strain energy consumption of strain-induced transformation is mainly responsible for this Lüders-like phenomenon. The TWIP mechanism dominates the 423 K (150 °C) deformation process, while the dislocation glide controls the plasticity at 573 K (300 °C) deformation. The delta-ferrite, as a hard phase in annealed dual-phase steel, greatly affects the mechanical stability of austenite due to the heterogeneous strain distribution between the two phases during deformation. A delta-ferrite-aided TRIP effect, i.e., martensite transformation induced by localized strain concentration of the hard delta-ferrite, is proposed to explain this kind of Lüders-like phenomenon. Moreover, the tensile curve at RT exhibits an upward curved behavior in the middle deformation stage, which is principally attributed to the deformation twinning of austenite retained after Lüders-like deformation. The combination of the TRIP effect during Lüders-like deformation and the subsequent TWIP effect greatly enhances the ductility in this annealed high-manganese dual-phase TRIP/TWIP steel.     

Influence of Copper Addition and Temperature on the Kinetics of Austempering in Ductile Iron

Austempered ductile iron (ADI) is a material that exhibits excellent mechanical properties because of its special microstructure, combining ferrite and austenite supersaturated with carbon. Two ADI alloys, Fe-3.5 pct C-2.5 pct Si and Fe-3.6 pct C-2.7 pct Si-0.7 pct Cu, austempered for various times at 623 K (350 °C) and 673 K (400 °C) followed by water quenching, were investigated. The first ferrite needles nucleate mainly at the graphite/austenite interface. The austenite and ferrite weight fractions increase with the austempering time until stabilization is reached. The increase in the lattice parameter of the austenite during austempering corresponds to an increase of carbon content in the austenite. The increase in the ferrite weight fraction is associated with a decrease in microhardness. As the austempering temperature increases, the ferrite weight fraction decreases, the high carbon austenite weight fraction increases, but the carbon content in the latter decreases. Copper addition increases the high carbon austenite weight fraction. The results are discussed based on the phases composing the Fe-2Si-C system.     

Investigation of Austenite-to-Ferrite Transformation in Ultralow and Low-Carbon Steel Using High-Speed Quenching Dilatometry and Thermokinetic Simulation

The isothermal austenite decomposition kinetics is studied in 0.004 wt pct C ultralow carbon (ULC) and 0.11 wt pct C low-carbon (LC) steel using high-speed quenching dilatometry. Standard samples of these steels are heated to austenitization temperatures of 1223 K and 1373 K (950 °C and 1100 °C) and then quenched to testing temperatures between 1163 K and 933 K (890 °C and 660 °C). The measured and calculated austenite-to-ferrite phase fractions are compared with dilatation values to analyze the ferrite nucleation and growth conditions during austenite decomposition. Ferrite evolution profiles are assessed to investigate the underlying growth kinetics. The analysis in ULC steel shows regimes of partitionless, partitioning, and two-stage transformation kinetics. In contrast, LC steel shows only diffusion-controlled transformation kinetics. The experimental results are well reproduced with thermokinetic calculations, thus supporting our interpretation of governing mechanisms during transformation.     

Kinetics of the fcc → hcp Phase Transformation in Cu-Ge Solid Solutions Upon Isothermal Aging

The kinetics of the ζ-phase formation from a supersaturated α-Cu(Ge) solid solution (i.e., transformation from the fcc crystal structure to the hcp crystal structure) containing 10.8 at. pct Ge [at isothermal temperatures of 573 K, 613 K, and 653 K (300 °C, 340 °C, and 380 °C)] were studied by X-ray diffraction (XRD) for phase fraction determination. Both in situ and ex situ annealing experiments were performed. The transformation kinetics were modeled on the basis of a versatile modular model. The transformation kinetics complied with a site-saturation nucleation mode and strongly anisotropic interface-controlled growth mode in association with a corresponding impingement mode: diffusion of Ge (towards the stacking faults, SFs) does not control the transformation rate. Transmission electron microscopy (TEM) investigations showed that segregation of Ge at the stacking faults (SFs) takes place (relatively fast) prior to the structural transformation (fcc → hcp).     

Relationship between austenite dislocation density introduced during thermal cycling and M s temperature in an Fe-17 wt pct Mn alloy

The reason why thermal cycling decreases the martensite start (M _s ) temperature of an Fe-17 wt pct Mn alloy was quantitatively investigated, based on the nucleation model of ε martensite and a thermodynamic model for a martensitic transformation. The M _s temperature decreased by about 22 K after nine cycles between 303 and 573 K, due to the increase in shear-strain energy (ΔG _sh ) required to advance the transformation dislocations through dislocation forests formed in austenite during thermal cycling. The ΔG _sh value increased from 19.3 to 28.8 MJ/m³ due to the increase in austenite dislocation density from 1.5 × 10¹² to 3.8 × 10¹³/m² with the number of thermal cycles (in this case, up to nine cycles). The austenite dislocation density increased rapidly for up to five thermal cycles and then increased gradually with further thermal cycles, showing a good agreement with the increase in austenite hardness with the number of thermal cycles.     

In Situ Thermo-magnetic Investigation of the Austenitic Phase During Tempering of a 13Cr6Ni2Mo Supermartensitic Stainless Steel

The formation of austenite during tempering of a 13Cr6Ni2Mo supermartensitic stainless steel (X2CrNiMoV13-5-2) was investigated using an in situ thermo-magnetic technique to establish the kinetics of the martensite to austenite transformation and the stability of austenite. The austenite fraction was obtained from in situ magnetization measurements. It was found that during heating to the tempering temperature 1 to 2 vol pct of austenite, retained during quenching after the austenitization treatment, decomposed between 623 K and 753 K (350 °C and 480 °C). The activation energy for martensite to austenite transformation was found by JMAK-fitting to be 233 kJ/mol. This value is similar to the activation energy for Ni and Mn diffusion in iron and supports the assumption that partitioning of Ni and Mn to austenite are mainly rate determining for the austenite formation during tempering. This also indicates that the stability of austenite during cooling after tempering depends on these elements. With increasing tempering temperature the thermal stability of austenite is decreasing due to the lower concentrations of austenite-stabilizing elements in the increased fraction of austenite. After cooling from the tempering temperature the retained austenite was further partially decomposed during holding at room temperature. This appears to be related to previous martensite formation during cooling.     

Relative Influences of Aluminium and Silicon on the Kinetics of Bainite Formation from Intercritical Austenite

Bainite formation from intercritical austenite is of great practical importance for the production of TRIP‐assisted steels. Silicon and aluminium play important roles during this transformation by delaying carbide precipitation, thus favouring the carbon enrichment of untransformed austenite, which makes its stabilisation down to room temperature possible. Previous studies have shown a strong dependence of bainite formation kinetics on both chemical composition and transformation temperature. In the present work, the effect of silicon and aluminium contents on bainite formation kinetics is investigated experimentally using dilatometry combined with microscopical observations. The experimental results are analysed by comparison with thermodynamic parameters, such as the activation energy G¹ for nucleation of bainite and the carbon content C_to corresponding to the T_o‐curve. It is shown that the faster transformation kinetics induced by the substitution of silicon by aluminium can be ascribed (i) to a higher driving force for nucleation, (ii) to a higher carbon content C_to at the To‐curve and (iii) to the precipitation of carbide in austenite in steels with a low Al content.     

Temperature-Dependent Multi-Scale Pore Evolution and Nitrogen Diffusion in Nuclear Graphite

Two- and three-dimensional pore evolutions along with nitrogen diffusion behavior in nuclear graphite were studied using thermogravimetric analysis, X-ray computed tomography, scanning electron microscopy, and the Brunauer-Emmett-Teller method. Calculated nitrogen diffusion activation energy was approximately 2.5 kJ·mol⁻¹. Stable weight loss of graphite specimens increased with temperature, primarily due to more escaped nitrogen from the graphite matrix. Fewer nano-pores and more micro-pores were formed because of the nano-pore coalescence. At 873 K (600 °C), graphite microstructure evolution might be induced by temperature and mild oxidation. Before being placed into high temperature gas-cooled reactors (HTGRs), porous nuclear graphite should be subjected to vacuum at 573 K to 673 K (300 °C to 400 °C) to minimize ¹⁴N in the pores and ¹⁴C generated during operation of HTGRs.

     

A Microscale Model for Ausferritic Transformation of Austempered Ductile Irons

This paper presents a new metallurgical model for the ausferritic transformation of ductile cast iron. The model allows predicting the evolution of phases in terms of the chemical composition, austenitization and austempering temperatures, graphite nodule count, and distribution of graphite nodule size. The ferrite evolution is predicted according to the displacive growth mechanism. A representative volume element is employed at the microscale to consider the phase distributions, the inhomogeneous austenite carbon content, and the nucleation of ferrite subunits at the graphite nodule surface and at the tips of existing ferrite subunits. The performance of the model is evaluated by comparison with experimental results. The results indicate that the increment of the ausferritic transformation rate, which is caused by increments of austempering temperature and graphite nodule count, is adequately represented by this model.

     

Modeling of the Austenitization of Ultra-high Strength Steel with Cellular Automation Method

A model for simulating the austenitization of ultra-high strength steel during hot stamping is developed using a cellular automata approach. The microstructure state before quenching can be predicted, including grain size, volume fraction of austenite, and distribution of carbon concentration. In this model, a real initial microstructure is used as an input to simulate austenitization, and the intrinsic chemical difference is utilized to describe the ferrite and pearlite phases. The kinetics of austenitization is simulated by simultaneously considering continuous nucleation, grain growth, and grain coarsening. The UHSS is reduced to a Fe-Mn-C ternary system to calculate the driving force during extent growth in ferrite. The simulation results show that the transformation of ferrite to austenite can be divided into three stages in the condition of a heating rate of 10 K (?263 °C)/s. The transformation rate is determined by two factors, carbon concentration and temperature. The carbon concentration plays a major role at the early stages, as well as the temperature is the main factor at the later stages. The A _c3 calculated is about 1073 K (800 °C) close to the measured value [1067.1 K (794.1 °C)]. Austenite grain coarsening was calculated by a curvature-driven model. The simulated morphology of the microstructure agrees well with the experimental result. Most of the dihedrals of the grain boundaries at the triple junctions are close to 120 deg. Finally, tensile tests were implied, as dwelling time increased from 3 to 10 minutes, the austenite grain size increased from 6.95 to 9.44 μm while the tensile strength decreased from 276.4 to 258.3 MPa.     

Acceleration or Suppression of α-Phase Precipitation Using Isothermal ω Phase in Ti-20 at.pct Nb Alloy

Homogeneous precipitation of a fine α phase in the β matrix of Ti alloys is a promising method for obtaining a highly strengthened Ti-based alloy. Isothermal ω particles are known to be the nucleation sites for fine α-phase precipitation, but an understanding of the kinetics of α-phase formation on isothermal ω particles is still lacking. This study aimed to reveal the effect of isothermal ω particles on α-phase precipitation onset time. Two-step isothermal aging of a Ti-20 at.pct Nb alloy after solid solution treatment at 1273 K (1000 °C) was carried out. The first step of the aging at 633 K (360 °C) involved the formation of isothermal ω particles in the β matrix. This was followed by a second aging step at 673 K, 723 K, and 773 K (400 °C, 450 °C, and 500 °C) for α-phase precipitation. Suppression of α-phase nucleation on the isothermal ω particles occurred at 673 K (400 °C), whereas acceleration of α-phase nucleation on the isothermal ω particles was observed at 723 K and 773 K (450 °C and 500 °C). Thermodynamic stability of the isothermal ω particles and solute partitioning were controlling factors for the α-phase precipitation kinetics.     

Influence of the Mn content on the kinetics of austempering transformation in compacted graphite cast iron

Mossbauer spectroscopy has been used to monitor the kinetics of austempering transformation in two compacted graphite (CG) cast irons alloyed with 0.11 and 0.58 wt pct of Mn, respectively. The phase relations were analyzed in terms of the Johnson-Mehl’s equation, determining the kinetics parameters n (time exponent) and k (constant rate of the transformation). The values obtained were n=1.4 and k=7.47 × 10⁻³ s⁻¹ for the low-Mn alloy, and n=2.2 and k=3.9×10⁻³ s⁻¹ for the high-Mn alloy. These results, which reveal a faster kinetics for the low-Mn alloy, are coherent with metallographic observations, and the driving force obtained through the determination of the austenite carbon concentration that was determined from the Mossbauer data using the Genins model for the Fe-C configurations in the fcc lattice. The kinetics parameters are further compared to those obtained in austempered ductile iron (ADI), by analyzing the graphite morphology influence on the austempering transformation.