A computational 3D model that accounts for both nucleation and interface migration is a very useful tool to monitor and grasp the complexity of microstructure formation in low-alloyed steels. In the present study we have developed a 3D mixed-mode multigrain model for the austenite-ferrite and the austenite-ferrite-austenite formation capable of following diffusional phase transformations under arbitrary thermal routes. This new model incorporates the solute drag effect of a substitutional element (in this case Mn) and ensures an automatic change in transformation direction when changing from heating to cooling and vice-versa. An analytical solution for calculating the energy dissipation of solute drag together with multiple regression approximations for chemical potentials are proposed which significantly accelerate the computation. The modelling results are first benchmarked for an Fe-0.1C-0.5Mn (wt.%) alloy under different continuous cooling and isothermal holding conditions. The model revealed relatively large variations in transformation kinetics of individual grains as a result of interactions with neighboring grains. Then the model is applied to predict the transformation kinetics of a series of Fe-C-Mn alloys during cyclic partial phase transformations. The comparison with experimental dilatometer results nicely validates the predictions of this model regarding the change in overall transformation kinetics of the ferrite transformation as a function of the Mn content. New features of this model are its efficient algorithm to compute energy dissipation by solute drag, its capabilities of predicting the microstructural state for spatially resolved grains and the minimal fine tuning of modelling parameters. The code to implement this model is publicly available.

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It is still a big challenge to obtain excellent low-temperature toughness for bulk steel materials. Delamination is an effective method to improve low-temperature toughness. In the present study, delamination toughening in a low carbon microalloyed steel plate with elongated and ultrafine-grained microstructure rolled in the dual-phase region has been investigated in detail. When toughness was measured along normal direction, the steel plate had a high upper shelf energy and no delamination occurred in the upper shelf region. A large delaminated crack parallel to rolling plane started to appear and changed the propagation path of main crack when testing temperature was lower than −60 °C. We find this kind of delamination induces a second upper shelf in the Charpy transition–temperature curve. The second upper shelf, reaching up to 300 J in the temperature range of −60 °C to −140 °C, results in excellent low-temperature toughness for the steel plate, and the ductile-brittle transition temperature is lowered to −157 °C. The developed steel plate also has high low-temperature toughness measured along transverse direction due to delamination. The effect factors on upper shelf energy, delamination mechanism and delamination toughening are discussed.

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Solid-state phase transformations in steels cover a broad range of aspects. The underlying physics behind these phase transformations usually include nucleation, diffusion, lattice reconstruction and interactions between solutes and grain boundaries and interfaces. These features and the fact that the events take place at high temperatures, in the bulk, at time scales ranging from milliseconds to hours and at length scales ranging from atomic dimensions to millimeters make even the most widely studied phase transformation in steel, the austenite-ferrite phase transformation, only approximately understood and therefore an attractive topic for investigation. Quantitative data obtained by sophisticated physical characterization techniques in combination with supporting physical microstructural models addressing the relevant length and time scale are required to bring the field of ferrous physical metallurgy further. This thesis focusses on two new approaches to orchestrate phase transformations in steels such that more physical insight is obtained or that new properties can be reached: (1) cyclic partial austenite-ferrite phase transformations that are designed to unravel the grain growth, and more specifically the interface mobility by avoiding concurrent nucleation of new phases. This topic is studied by computational studies and 3D neutron depolarization studies that are capable to in-situ monitor the ferrite grain size and fraction. (2) Self healing of creep damage by site selective precipitation of supersaturated iron-based alloys. A strong preference for precipitation at free creep cavity surfaces compared to that in the bulk can result in a filling of creep cavities and a significant extension of the creep life time. To make this self-healing mechanism applicable for creep-resistant steels, a search for an alternative healing agent for Au in Fe is to be executed and new design recipes need to be extracted on the basis of the experimental input from advanced characterization techniques such as electron microscopy and X-ray nanotomography.@en

When metals are mechanically loaded at elevated temperatures for extended periods of time, creep damage will occur in the form of cavities at grain boundaries. In the present experiments it is demonstrated that in binary iron-tungsten alloys creep damage can be self healed by selective precipitation of a W-rich phase inside these cavities. Using synchrotron X-ray nano-tomography the simultaneous evolution of creep cavitation and precipitation is visualized in 3D images with a resolution down to 30 nm. The degree of filling by precipitation is analysed for a large collection of individual creep cavities. Two clearly different types of behaviour are observed for isolated and linked cavities, where the isolated cavities can be filled completely, while the linked cavities continue to grow. The demonstrated self-healing potential of tungsten in iron-based metal alloys provides a new perspective on the role of W in high-temperature creep-resistant steels.@en

The magnetic configuration of a ferromagnetic system with mono-disperse and poly-disperse distribution of magnetic particles with inter-particle interactions has been computed. The analysis is general in nature and applies to all systems containing magnetically interacting particles in a non-magnetic matrix, but has been applied to steel microstructures, consisting of a paramagnetic austenite phase and a ferromagnetic ferrite phase, as formed during the austenite-to-ferrite phase transformation in low-alloyed steels. The characteristics of the computational microstructures are linked to the correlation function and determinant of depolarisation matrix, which can be experimentally obtained in three-dimensional neutron depolarisation (3DND). By tuning the parameters in the model used to generate the microstructure, we studied the effect of the (magnetic) particle size distribution on the 3DND parameters. It is found that the magnetic particle size derived from 3DND data matches the microstructural grain size over a wide range of volume fractions and grain size distributions. A relationship between the correlation function and the relative width of the particle size distribution was proposed to accurately account for the width of the size distribution. This evaluation shows that 3DND experiments can provide unique in situ information on the austenite-to-ferrite phase transformation in steels.@en

A 3D model has been developed to predict the average ferrite grain size and grain size distribution for an austenite-to-ferrite phase transformation during continuous cooling of an Fe-C-Mn steel. Using a Voronoi construction to represent the austenite grains, the ferrite is assumed to nucleate at the grain corners and to grow as spheres. Classical nucleation theory is used to estimate the density of ferrite nuclei. By assuming a negligible partition of manganese, the moving ferrite–austenite interface is treated with a mixed-mode model in which the soft impingement of the carbon diffusion fields is considered. The ferrite volume fraction, the average ferrite grain size, and the ferrite grain size distribution are derived as a function of temperature. The results of the present model are compared with those of a published phase-field model simulating the ferritic microstructure evolution during linear cooling of an Fe-0.10C-0.49Mn (wt pct) steel. It turns out that the present model can adequately reproduce the phase-field modeling results as well as the experimental dilatometry data. The model presented here provides a versatile tool to analyze the evolution of the ferrite grain size distribution at low computational costs.@en

We have analyzed the evolution of the ferrite fraction and average ferrite grain size during partial cyclic austenite-to-ferrite and ferrite-to-austenite phase transformations in an Fe-0.25C-2.1Mn (wt pct) steel using three-dimensional neutron depolarization (3DND). In the 3DND experiments, the ferrite fraction is derived from the rotation angle of the neutron polarization vector, and the average grain size is determined from the shortening of the polarization vector. From these, the number density of ferrite grains is derived, which indicates that grain nucleation is negligible during partial cycling in the intercritical regime and that all transformation kinetics can be attributed to growth processes only. In the multiple successive cyclic partial transformations, the interfacial migration rate was found to be sluggish due to Mn partitioning. The transformation kinetics determined with 3DND was compared to the predicted behaviors for diffusion-controlled simulations under local equilibrium and para-equilibrium interfacial conditions. It was found that the simulation predictions under local equilibrium only qualitatively capture the transformation kinetic with a difference of one order of magnitude in the variation in the ferrite fraction during cycling. The cyclic behavior of this Fe-0.25C-2.1Mn (wt pct) steel shows that the austenite-ferrite interface indeed migrates back and forth during cycling, while at the same time, there is a gradual increase in both the ferrite fraction and the average ferrite grain size over subsequent cycles. The intrinsic cyclic behavior is only visible after subtracting the effect of the progressive interfacial migration into austenite. The present study demonstrates the advantage of 3DND in studying partial cyclic phase transformations over conventional experimental approaches.

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The precipitation of Au-rich precipitates on the external surfaces of Fe-Au alloys has been studied by scanning and transmission electron microscopy. The surface precipitates formed at elevated temperatures are found to self-organize in regular patterns and their growth rate is determined quantitatively. The observed surface precipitation at a free surface is compared to the precipitation at the internal surface of grain boundary cavities induced by creep loading. A close agreement between both processes is observed.@en

The autonomous filling of creep-loading induced grain-boundary cavities by gold-rich precipitates at a temperature of 550 °C has been studied as a function of the applied load for Fe-Au alloys using synchrotron X-ray nano-tomography. The alloy serves as a model alloy for future self-healing creep resistant steels. The size, shape and spatial distribution of cavities and precipitates are analyzed quantitatively in 3D at a nanometer resolution scale. The filling ratios for individual cavities are determined and thus a map of the filling ratio evolution is obtained. It is found that the gold-rich precipitates only form at cavity surfaces and thereby repair the creep cavity. The shape of the cavities changes from equiaxed to planar crack like morphologies as the cavities grow. The time evolution of the filling ratio is explained by a simple model considering isolated cavities as well as linked cavities. The model predictions are in good agreement with the measurements.

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We have investigated the autonomous repair of creep damage by site-selective precipitation in a binary Fe-Mo alloy (6.2 wt pct Mo) during constant-stress creep tests at temperatures of 813 K, 823 K, and 838 K (540 °C, 550 °C, and 565 °C). Scanning electron microscopy studies on the morphology of the creep-failed samples reveal irregularly formed deposits that show a close spatial correlation with the creep cavities, indicating the filling of creep cavities at grain boundaries by precipitation of the Fe₂Mo Laves phase. Complementary transmission electron microscopy and atom probe tomography have been used to characterize the precipitation mechanism and the segregation at grain boundaries in detail.

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