The effect of aluminium and phosphorus on the stability of individual austenite grains in TRIP steels

We have performed in situ synchrotron X-ray diffraction experiments to assess the influence of aluminium and phosphorus on the austenite stability in low-alloyed transformation-induced plasticity steels during the high-temperature bainitic holding and the subsequent martensitic transformation during cooling to temperatures between room temperature and 100 K. Although the addition of aluminium increases the chemical driving force for the formation of bainitic ferrite plates significantly, the phosphorus exerts a larger influence on the bainitic transformation kinetics. Consequently, the addition of phosphorus leads to a higher degree of carbon enrichment and a narrower grain volume distribution of the metastable austenite. The stability of the individual austenite grains with respect to their martensitic transformation depends on both the local carbon content and the grain volume for austenite grains smaller than 20 μm³. The presence of aluminium and phosphorus further stabilizes the austenite grains.     

Load partitioning between single bulk grains in a two-phase duplex stainless steel during tensile loading

The lattice strain tensor evolution for single bulk grains of austenite and ferrite in a duplex stainless steel during tensile loading to 0.02 applied strain has been investigated using in situ high-energy X-ray measurements and finite-element modeling. Single-grain X-ray diffraction lattice strain data for the eight austenite and seven ferrite grains measured show a large variation of residual lattice strains, which evolves upon deformation to the point where some grains with comparable crystallographic orientations have lattice strains different by 1.5 × 10^?3, corresponding to a stress of ～300 MPa. The finite-element simulations of the 15 measured grains in three different spatial arrangements confirmed the complex deformation constraint and importance of local grain environment.     

Time-dependent synchrotron X-ray diffraction on the austenite decomposition kinetics in SAE 52100 bearing steel at elevated temperatures under tensile stress

We have studied the decomposition kinetics of the metastable austenite phase present in quenched-and-tempered SAE 52100 steel by in situ high-energy synchrotron X-ray diffraction experiments at elevated temperatures of 200–235 °C under a constant tensile stress. We have observed a continuous decomposition of austenite into ferrite and cementite. The decomposition kinetics is controlled by the long-range diffusion of carbon atoms into the austenite ahead of the moving austenite/ferrite interface. The presence of a tensile stress of 295 MPa favours the carbon diffusion in the remaining austenite, so that the activation energy for the overall process decreases from 138–148 to 82–104 kJ mol^?1. Before the austenite starts to decompose, a significant amount of carbon atoms partition from the surrounding martensite phase into the metastable austenite grains. This carbon partitioning takes place simultaneously with the carbide precipitation due to the over-tempering of the martensite phase. As the austenite decomposition proceeds gradually at a constant temperature and stress, the elastic strain in the remaining austenite grains continuously decreases. Consequently, the remaining austenite grains act as a reinforcement of the ferritic matrix at longer isothermal holding times. The texture evolution in the constituent phases reflects both significant grain rotations and crystal orientation relationships between the parent austenite phase and the newly formed ferritic grains.     

Experimental evidence and thermodynamics analysis of high magnetic field effects on the austenite to ferrite transformation temperature in Fe–C–Mn alloys

The non-isothermal decomposition of austenite into ferrite and pearlite in Fe–xC–1.5 wt.% Mn steels with x = 0.1, 0.2 and 0.3 wt.% C is investigated by in situ dilatometry and microstructure characterization in magnetic fields up to 16 T. The global shift towards higher temperatures of the respective austenite, ferrite + austenite and ferrite + pearlite stability regions is experimentally quantified. A systematic increase in the ferrite area fraction and proportional reduction of the Vickers hardness values with the magnetic field intensity are also reported. Moreover, the steels’ magnetizations, measured up to 3.5 T and 1100 K, are used to calculate the magnetic contribution to the free energy of the transformation and to account thermodynamically for the field dependence of the transformation temperature. The impact of magnetic field is found to be greater with increasing carbon content in the steels.     

Deformation mechanisms of a 20Mn TWIP steel investigated by in situ neutron diffraction and TEM

The deformation mechanisms and associated microstructure changes during tensile loading of an annealed twinning-induced plasticity steel with chemical composition Fe–20Mn–3Si–3Al–0.045C (wt.%) were systematically investigated using in situ time-of-flight neutron diffraction in combination with post mortem transmission electron microscopy (TEM). The initial microstructure of the investigated alloy consists of equiaxed γ grains with the initial α′-phase of ～7% in volume. In addition to dislocation slip, twinning and two types of martensitic transformations from the austenite to α′- and ε-martensites were observed as the main deformation modes during the tensile deformation. In situ neutron diffraction provides a powerful tool for establishing the deformation mode map for elucidating the role of different deformation modes in different strain regions. The critical stress is 520 MPa for the martensitic transformation from austenite to α′-martensite, whereas a higher stress (>600 MPa) is required for actuating the deformation twin and/or the martensitic transformation from austenite to ε-martensite. Both ε- and α′-martensites act as hard phases, whereas mechanical twinning contributes to both the strength and the ductility of the studied steel. TEM observations confirmed that the twinning process was facilitated by the parent grains oriented with 〈1 1 1〉 or 〈1 1 0〉 parallel to the loading direction. The nucleation and growth of twins are attributed to the pole and self-generation formation mechanisms, as well as the stair-rod cross-slip mechanism.     

Effects of aluminum content on cracking phenomenon occurring during cold rolling of three ferrite-based lightweight steel

The effects of Al content on cracking phenomena occurring during cold rolling of ferritic lightweight steels were investigated in relation to microstructural modification including κ-carbides. Three steels were fabricated, varying the Al content between 4 and 6 wt.%, and the center and edge areas of steel sheets containing 6 wt.% Al were cracked during cold rolling. The three steels were composed of ferrite grains and κ-carbides in a banded shape, and the overall volume fraction of κ-carbide increased with increasing Al content. The shape of lamellar κ-carbides inside κ-carbide bands was changed from short and thin to long and thick. Microstructural observation of the deformed region of fractured tensile specimens revealed that deformation bands were homogeneously formed in wide areas of ferrite matrix in the steels containing 4–5 wt.% Al, and κ-carbide bands and boundary κ-carbides were hardly cracked. In the steel containing 6 wt.% Al, however, microcracks were initiated at grain boundary κ-carbides and long lamellar κ-carbides inside κ-carbide bands. They led to the center or edge cracking during cold rolling. To prevent or minimize cracking, it was necessary to avoid the lengthening or thickening of lamellar κ-carbides. Therefore, it was recommended that the steels should be rapidly cooled from the finish rolling temperature to the coiling temperature through the formation temperature of κ-carbide.     

Nucleation process control of undercooled stainless steel by external nucleation seed

Competitive phase selection of undercooled melts between equilibrium ferrite and metastable austenite has been investigated as a function of undercooling. Stainless steel type 316 was undercooled up to 250 K using an electromagnetic levitation method. The microstructure showed different morphologies depending on the undercooling due to different solid phase transformation mechanisms. However, metastable austenite was not formed during the solidification for the undercooling up to 250 K due to the favorable nucleation kinetics of ferrite. The control of the phase selection has also been attempted using an external nucleation seed. Undercooled melts were touched by Fe–50 at.% Ni powders in the levitation coil, whose lattice constant is almost the same as that of metastable austenite. The microstructure showed a dramatic change in the solidification mode from equilibrium ferrite to metastable austenite during the first stage of the solidification.     

Molecular dynamics simulations of grain boundary sliding: The effect of stress and boundary misorientation

Molecular dynamics simulations were used to study the effect of applied force and grain boundary misorientation on grain boundary sliding in aluminum at 750 K. Two grains were oriented with their 〈1 1 0〉 axes parallel to their boundary plane and one grain was rotated around its 〈1 1 0〉 axis to various misorientation angles. For any given misorientation, increasing the applied force leads to three sliding behaviors: no sliding, constant velocity sliding and a parabolic sliding over time. The last behavior is associated with disordering of atoms along the grain boundary. For the second sliding behavior, the constant sliding velocity varied linearly with the applied stress. A linear fit of this relationship did not intersect the stress axis at the origin, implying that a threshold stress for sliding exists. This threshold stress was found to decrease with increasing grain boundary energy. The ramifications of this finding for modeling grain boundary sliding in polycrystals are discussed.     

A new approach to designing a grain refiner for Mg casting alloys and its use in Mg–Y-based alloys

A totally new grain refiner, Al₂Y, for cast Mg alloys has been predicted using the recently developed edge-to-edge matching (E2EM) crystallographic model. An addition of 0.6–1.0 wt.% Al into the Mg–10 wt.% Y melt promotes the in situ formation of Al₂Y, which reduces the average grain size from about 180 to 36 μm. Active nucleation Al₂Y particles were reproducibly observed at the centres of many refined grains. The excellent grain-refining efficiency is comparable to that of Zr for the same alloy, but the thermal stability of the grains refined by Al₂Y is much higher than those refined by Zr up to a temperature of 550 °C for 48 h. The mechanisms of grain refinement and the superior thermal stability of the refined grains due to Al addition in the Mg–Y alloy are discussed based on the current experimental results.     

Nanoscale austenite reversion through partitioning,segregation and kinetic freezing: Example of a ductile 2 GPa Fe–Cr–C steel

Austenite reversion during tempering of a Fe–13.6 Cr–0.44 C (wt.%) martensite results in an ultra-high-strength ferritic stainless steel with excellent ductility. The austenite reversion mechanism is coupled to the kinetic freezing of carbon during low-temperature partitioning at the interfaces between martensite and retained austenite and to carbon segregation at martensite–martensite grain boundaries. An advantage of austenite reversion is its scalability, i.e. changing tempering time and temperature tailors the desired strength–ductility profiles (e.g. tempering at 400 °C for 1 min produces a 2 GPa ultimate tensile strength (UTS) and 14% elongation while 30 min at 400 °C results in a UTS of ～1.75 GPa with an elongation of 23%). The austenite reversion process, carbide precipitation and carbon segregation have been characterized by X-ray diffraction, electron back-scatter diffraction, transmission electron microscopy and atom probe tomography in order to develop the structure–property relationships that control the material’s strength and ductility.     

Microstructural analysis of thermally induced and deformation induced martensitic transformations in Fe–12.5 wt.% Mn–5.5 wt.% Si–9 wt.% Cr–3.5 wt.% Ni alloy

Martensitic transformations induced by thermally and compression deformation at room temperature in Fe–12.5 wt.% Mn–5.5 wt.% Si–9 wt.% Cr–3.5 wt.% Ni alloy were studied in detail by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). From microstructural observations, it was seen that heat treated samples exhibited regular overlapping of stacking faults and ɛ martensite plates were formed parallel to each other. Also, TEM investigations showed that the orientation relationship between γ (fcc) and ɛ (hcp) phases corresponds to Shoji–Nishiyama type. With applied low plastic deformation rate, only ɛ martensite occurred in austenite grain. As a consequence, 4 and 25% plastic deformation at room temperature caused ɛ martensite formation in austenite phase and the new ɛ (hcp) and α′ (bcc) martensite formation in martensite phases, respectively. Orientation relationship between ɛ and α′ phases was found by the electron diffraction analysis.     

Spatial correlation in grain misorientation distribution

Grain misorientation was studied in relation to the nearest neighbor’s mutual distance using electron back-scattered diffraction measurements. The misorientation correlation function was defined as the probability density for the occurrence of a certain misorientation between pairs of grains separated by a certain distance. Scale-invariant spatial correlation between neighbor grains was manifested by a power law dependence of the preferred misorientation vs. inter-granular distance in various materials after diverse strain paths. The obtained negative scaling exponents were in the range of ?2 ± 0.3 for high-angle grain boundaries. The exponent decreased in the presence of low-angle grain boundaries or dynamic recrystallization, indicating faster decay of correlations. The correlations vanished in annealed materials. The results were interpreted in terms of lattice incompatibility and continuity conditions at the interface between neighboring grains. Grain-size effects on texture development, as well as the implications of such spatial correlations on texture modeling, were discussed.     

Effect of annealing temperature on microstructural modification and tensile properties in 0.35 C–3.5 Mn–5.8 Al lightweight steel

The microstructural modifications occurring during annealing treatment of an Fe–0.35 C–3.5 Mn–5.8 Al ferrite-based lightweight steel and its effects on the tensile properties were investigated with respect to (α + γ) duplex microstructures. Steels annealed above the dissolution finishing temperature of κ-carbides (795 °C) were basically composed of ferrite band and austenite band in a layered structure. As the annealing temperature was increased the tensile strength increased, while the yield strength and elongation decreased. This could be explained by a decrease in the mechanical as well as thermal stability of austenite with increasing size and austenite volume fraction. In the 980 °C annealed steel in particular, whose mechanical stability due to austenite was lowest, cracks were readily formed at ferrite/austenite (or martensite) interfaces with little deformation, thereby leading to the least tensile elongation. In order to obtain the best combination of strength and ductility the formation of austenite having an appropriate mechanical stability was essentially needed, and could be achieved when 22–24 vol.% fine austenite was homogeneously distributed in the ferrite matrix, as in the 830 °C or 880 °C annealed steels.     

Nanocrystalline Fe–C alloys produced by ball milling of iron and graphite

A series of nanocrystalline Fe–C alloys with different carbon concentrations (x_tot) up to 19.4 at.% (4.90 wt.%) are prepared by ball milling. The microstructures of these alloys are characterized by transmission electron microscopy and X-ray diffraction, and partitioning of carbon between grain boundaries and grain interiors is determined by atom probe tomography. It is found that the segregation of carbon to grain boundaries of α-ferrite can significantly reduce its grain size to a few nanometers. When the grain boundaries of ferrite are saturated with carbon, a metastable thermodynamic equilibrium between the matrix and the grain boundaries is approached, inducing a decreasing grain size with increasing x_tot. Eventually the size reaches a lower limit of about 6 nm in alloys with x_tot > 6.19 at.% (1.40 wt.%); a further increase in x_tot leads to the precipitation of carbon as Fe₃C. The observed presence of an amorphous structure in 19.4 at.% C (4.90 wt.%) alloy is ascribed to a deformation-driven amorphization of Fe₃C by severe plastic deformation. By measuring the temperature dependence of the grain size for an alloy with 1.77 at.% C additional evidence is provided for a metastable equilibrium reached in the nanocrystalline alloy.     

Tensile strength of 〈1 0 0〉 and 〈1 1 0〉 tilt bicrystal copper interfaces

Molecular dynamics (MD) simulations are used to model dislocation nucleation at or near symmetric tilt bicrystal copper interfaces with 〈1 0 0〉 or 〈1 1 0〉 misorientation axes. MD simulations indicate that orientation of the opposing lattice regions and the presence of certain structural units are two critical attributes of the interface structure that affect the stress required for dislocation nucleation. Boundaries that contain the E structural unit are found to emit dislocations at comparatively low tensile stress magnitudes. A simple model is proposed to illustrate the impact of interfacial porosity and stresses acting on the slip-plane in non-glide directions on tensile interface strength. Accounting for interfacial porosity through an average measure is found to be sufficient to model the tensile strength of boundaries with a 〈1 0 0〉 misorientation axis and many boundaries with a 〈1 1 0〉 misorientation axis.     

A novel thermomechanical approach to produce a fine ferrite and low-temperature bainitic composite microstructure

A novel thermomechanical processing was developed in the present study to produce a unique microstructure consisting of fine ferrite grains (i.e. ～4 μm on average) and low-temperature bainite in a relatively low-carbon steel with a modest hardenability. The thermomechanical route consisted of warm deformation of supercooled austenite followed by reheating in the ferrite region and then cooling to the bainitic transformation regime (i.e. 400–200 °C). The low-temperature bainite consisted of high dislocation density bainitic laths and very fine retained austenite films. This microstructure offered a high work hardening rate leading to a unique combination of ultimate tensile strength and elongation. This was due to the presence of ductile fine ferrite grains and hard low-temperature bainitic ferrite laths with retained austenite films. The microstructural characteristics of bainite were studied using optical microscopy in conjunction with scanning and transmission electron microscopy, electron backscatter diffraction and atom probe tomography techniques.     

Sigma-phase precipitation upon industrial-like heating of cast heat-resistant steels

In order to investigate the formation of sigma-phase in two cast heat-resistant steels of wide industrial use, two ferrous alloys containing 25.02Cr–4.26Ni–0.53C and 31.23Cr–6.08Ni-0.36C were prepared by casting techniques and then subjected to sigma precipitation by heating the alloys, for increasing periods of time, at a temperature which resembles the average thermal level usually encountered in service conditions of these materials. Initially, the phase nucleates along ferrite–austenite boundaries, but with more time sigma precipitates inside the ferrite grains. Furthermore, both alloys showed a behavior that resembles the well-known Johnson–Mehl–Avrami's mechanism, stated for a nucleation and diffusion-controlled growth process in metallic systems. Hence, the phenomenon reached asymptotic values of approximately 25 and 55 vol.% in the HC- and HD-grade, respectively, after 120 h heating at 1053 K. The experimental results may help in controlling the behavior of these materials when they are to be utilized in industrial applications at elevated temperatures.     

Stress-driven migration of symmetrical 〈1 0 0〉 tilt grain boundaries in Al bicrystals

Stress-induced migration of planar grain boundaries in aluminum bicrystals was measured for both low- and high-angle symmetrical 〈1 0 0〉 tilt grain boundaries across the entire misorientation range (0–90°). Boundary migration under a shear stress was observed to be coupled to a lateral translation of the grains. Boundaries with misorientations smaller than 31° and larger than 36° moved in opposite directions under the same applied external stress. The measured ratios of the normal boundary motion to the lateral displacement of grains are in an excellent agreement with theoretical predictions. The coupled boundary motion was measured in the temperature range between 280 and 400 °C, and the corresponding activation parameters were determined. The results revealed that for mechanically induced grain-boundary motion there is a misorientation dependence of migration activation parameters. The obtained results are discussed with respect of the mechanism of grain-boundary motion.     

Dislocation–grain boundary interaction in 〈1 1 1〉 textured thin metal films

The interaction of lattice dislocations with symmetrical and asymmetrical tilt grain boundaries in 〈1 1 1〉 textured thin nickel films was investigated using atomistic simulation methods. It was found that the misorientation angle of the grain boundary, the sign of the Burgers vector of the incoming dislocation and the exact site where the dislocation meets the grain boundary are all important parameters determining the ability of the dislocation to penetrate the boundary. Inclination angle, however, does not make an important difference on the transmission scenario of full dislocations. Only limited partial dislocation nucleation was observed for the investigated high-angle grain boundary. The peculiarities of nucleation of embryonic dislocations and their emission from tilt grain boundaries are discussed.     

Effect of deformation and annealing on the formation and reversion of ε-martensite in an Fe–Mn–C alloy

Microstructure and texture evolution during cold rolling and subsequent annealing were studied in an Fe–22 wt.% Mn–0.376 wt.% C alloy. During rolling the deformation mechanisms were found to be dislocation slip, mechanical twinning, deformation-induced ε-martensite transformation and shear banding. At higher strains, the brass-type texture with a spread towards the Goss-type texture dominated. A decrease in the Cu- and S- components was attributed to the preferential transformation to ε-martensite in Cu- and S-oriented grains. The texture of ε-martensite was sharp and could be described as {1 1 2 9}〈3 3 6 2〉. The orientation relationship {1 1 1}^γ//{0 0 0 1}^ε and 〈110〉^γ//〈1 1 –2 0〉^ε between ε-martensite and austenite was observed but only certain variants were selected. On subsequent annealing, the ε-martensite transformed reversely to austenite by a diffusionless mechanism. Changes in length along rolling, normal and transverse directions on heating were anisotropic due to a combination of volume expansion and shape memory effects. The S-texture component increased significantly due to transformation from the ε-martensite.