© 2023 Universidade Federal de Sao Carlos. All rights reserved.Aerospace and automotive industries utilize advanced high strength steels due to their exceptional mechanical strength and ductility. Laser beam welding has shown potential in reducing the melted zone, heat affected zone, and process time for these steels. This study focused on dissimilar welding between DP 780 and 300M steel sheets, commonly used in the automotive and aerospace industries, respectively. The aim was to expand the range of possibilities and innovations by enabling the use of these steels in both applications. The study investigated the optimal process parameters, microstructure, and mechanical properties for the laser welding process. It also examined the influence of intercritical quenching and tempering on the microstructure and mechanical properties of the laser welded steels. The materials underwent dilution and different phase transformations due to the welding process and heat treatments, as revealed by microstructural characterization. The weld showed a notable increase in hardness, however without compromising toughness. The fractures during tensile testing occurred in the DP 780 steel, far from the MZ and HAZ. Heat treatments increased ultimate tensile strength, but lowered ductility. Welding affected the fatigue life, especially in the intercritically quenched joint, which showed a quasi-cleavage crack growth mechanism and a decrease in fracture toughness.

© 2023 Universidade Federal de Sao Carlos. All rights reserved.Hybrid casting is a new fabrication concept that can reduce costs and production time of large tools, such as stamping tools for the automotive industry. In this work, we analyzed a hybrid material composed of a high chromium cast iron (HCCI) and a low carbon steel (WCB). SEM analyses indicate that the interface is free of non-metallic inclusions and porosities. The metallurgical bonding between alloys is confirmed by the diffusion of chromium and carbon from HCCI to WCB. Vickers microhardness, EDS and XRD confirmed the presence of M7C3 carbides in the HCCI and at the interface. One set of the samples was submitted to regular quenching in calm air and tempering, while another set was additionally submitted to subzero quenching before tempering. In both cases, a slight reduction of the HCCI hardness and an increase of the interface hardness were observed. The subzero treatment was effective to reduce the amount of retained austenite at the HCCI and limiting its hardness reduction. WCB microstructure and hardness showed no significative change, making it an ideal material to use with HCCI in hybrid casts. The results showed that is possible to produce bimetallic reliable components for industrial applications by means of hybrid casting.

© 2023 Universidade Federal de Sao Carlos. All rights reserved.The objective of this work is to study the possibility of obtaining dense parts using water atomized AISI 316L steel powder in the L-PBF process. Despite its irregular, non-spherical, particle morphology, it has a significantly lower cost. 25 samples were produced varying the laser power and the scanning speeds to determine the optimal processing conditions. Additionally, hot isostatic pressing (HIP) was performed after the L-PBF process to further increase densification. Selected samples were subjected to microstructural characterization. The best densification results obtained were for the sample produced with the laser power of 173 W and scanning speed of 600 mm/s, where densifications close to 98% were obtained. HIP post-processing promoted increased densification of samples with closed porosity, allowing samples with densification above 95% to reach values close to 100%. HIP did not promote the closure of open pores. The results indicate that the use of water atomized AISI 316L in the L-PBF process combined with post-processing by HIP can produce dense engineering components and at the same time reduce the production costs of the manufactured components, mainly because it is a lower cost raw material when compared to the commonly used feedstock obtained by gas atomization.

© 2023 Universidade Federal de Sao Carlos. All rights reserved.WC-Co cutting tools are widely used by the metalworking industry. In order to improve the properties of these tools, research on the application of wear-resistant coatings, such as polycrystalline diamond, are of great importance to several applications. It is known that the occurrence of high-stress levels between the coating and the substrate can lead to adhesion failures. One strategy to minimize these failures is applying an intermediate layer of SiC. In this work, the deposition of a SiC layer was carried out by a novel two-step laser cladding approach. Instead of cladding directly the presynthesized SiC on the substrates, a 200 µm silicon powder layer was pre-deposited on the WC-Co substrates and then irradiated with a 30 W CO2 laser. To improve metallurgical bonding between the tungsten and the Si layer, all substrates were chemically attacked. This attack allows cobalt removal from the surface and increases surface roughness, improving the laser cladding process. After the SiC laser cladding, samples were coated with a 200 µm graphite powder layer and irradiated again by a CO2 laser. The samples were characterized by SEM, EDS, and XRD analysis. The results showed that in the first step, an irradiation energy of about 0.27 J was enough to fuse the silicon powder to the substrate and in the second step, 0.13 J was enough to promote the reaction between silicon, carbon and the WC substrate, resulting in the in-situ synthesis of SiC. Finally, a new method was proposed for the deposition of SiC on WC-Co based substrates and the observed results allowed the proposal of an empirical equation to describe the chemical reactions of the process.

© 2022 Elsevier Inc.Austenite reversion, i.e., a’-martensite → γ phase transformation in UNS S32304 lean duplex steel was investigated. The material was cold rolled to a true strain (ε) of 1.61 and subjected to continuous annealing up to 1000 °C with a heating rate of 3 °C/min. From the dilatometric curve, an unexpected thermal expansion at around 545 °C was found within the temperature range where the austenite reversion occurs. Based on this unexpected behavior, additional samples were annealed at the same heating rate until key temperatures. Besides dilatometry, microstructural changes were followed by means of magnetic measurements at room temperature, Vickers microhardness testing, high-resolution electron backscatter diffraction (EBSD), and electron channeling contrast imaging (ECCI). From EBSD data, a protocol was developed to distinguish the different constituents in the material during the austenite reversion, i.e., α'-martensite, ferrite, and both reversed and untransformed austenite. The driving force for the austenite reversion was calculated using thermodynamic calculations. The a’-martensite → γ transformation begins at about 545 °C and ends at almost 800 °C. In the early beginning, the austenite reversion is governed by a shear mechanism. At higher temperatures, at about 725 °C, KAM (kernel average misorientation) distributions and texture of both reversed and untransformed austenite show evidence of a diffusion-controlled austenite reversion mechanism. These results are supported by thermodynamic calculations and microstructural evidence revealed by ECCI.

© 2022, The Author(s).The enormous magnitude of 2 billion tons of alloys produced per year demands a change in design philosophy to make materials environmentally, economically, and socially more sustainable. This disqualifies the use of critical elements that are rare or have questionable origin. Amongst the major alloy strengthening mechanisms, a high-dispersion of second-phase precipitates with sizes in the nanometre range is particularly effective for achieving ultra-high strength. Here, we propose an alternative segregation-based strategy for sustainable steels, free of critical elements, which are rendered ultrastrong by second-phase nano-precipitation. We increase the Mn-content in a supersaturated, metastable Fe-Mn solid solution to trigger compositional fluctuations and nano-segregation in the bulk. These fluctuations act as precursors for the nucleation of an unexpected α-Mn phase, which impedes dislocation motion, thus enabling precipitation strengthening. Our steel outperforms most common commercial alloys, yet it is free of critical elements, making it a new platform for sustainable alloy design.

© 2022, ASM International.Additive manufacturing (AM) has emerged as an outstanding technique for obtaining complex geometries and custom parts, without the material loss of conventional subtractive manufacturing processes. In this work, AISI 316L stainless steel specimens were fabricated by laser powder bed fusion (L-PBF), and its microstructure was characterized by several techniques. Tensile tests with in situ x-ray diffraction (XRD) measurements were performed using synchrotron radiation. Stress–strain curves and diffractograms were obtained for the as-printed AM 316L, annealed AM 316L and conventional/rolled 316L samples for comparison. The results indicated lower ductility for the AM samples when compared to the sheet. This can be a result of the remaining porosity associated with the AM process. The annealing of the AM samples led to a reduction of the residual stress and an improvement of ductility without significant loss on the ultimate tensile strength. In situ XRD data indicated that AM samples did not undergo phase transformation during straining, maintaining a fully austenitic microstructure and preventing a transformation-induced plasticity (TRIP) effect. On the other hand, in the rolled sample, peaks of α′-martensite were identified. Electron backscattered diffraction (EBSD) measurements indicated that a random texture was achieved by the parameters and scanning strategy used. The results indicate that process parameters must be carefully chosen in order to avoid porosity, and excessive residual stresses, features that directly affect the mechanical behavior of the material.

© 2022 Universidade Federal de Sao Carlos. All rights reserved.The effect of temperature was investigated on the consolidation of blended elemental powders of aluminum and copper by equal channel angular pressing (ECAP). Aluminum and Copper powders (1:1% vol.) were blended and consolidated in a 90° ECAP die at room (RT) and cryogenic temperatures (CT - ∼77 K). ECAP samples were pressed until 4 passes at room temperature in route Bc. As a reference, a sample was obtained by conventional uniaxial pressing. The obtained results indicated a much denser (>99.5%) and harder structure by cryogenic ECAP. The hardness after one pass at CT was comparable with 4 passes at room temperature. Tensile tests performed at CT for materials with similar chemical composition showed a simultaneous increase in strength and ductility at CT, corroborating the results obtained by ECAP. The partial suppression of dynamic recovery and the activation and the transition between deformation mechanisms at CT, as well as stacking fault energies (SFE) of such metals, played an important role in these results. Copper presented a much higher capability of strain hardening than aluminum, due to its lower SFE and much lower homologous temperature. X-ray diffraction indicated a strong correlation between the variation of average microstrain and the variation of hardness on both metals. The results of this study demonstrated the great potential of the application of very low temperatures for the obtaining of deformation metal-metal composites.

© 2021Parts produced by laser powder-bed fusion (LPBF) show unique microstructures consisting of dislocation structures and an oxide nanoparticle dispersion usually embedded in epitaxially-grown grains. Thermomechanical processing is an alternative to enhance the microstructure of such materials. However, the deformation mechanisms and the resulting microstructures following annealing are not yet well understood, hindering further microstructure control. We apply cold rolling and subsequent annealing in AISI 316L stainless steel processed by LPBF and perform an in-depth microstructural characterization to understand the origin of abnormal growth and how to avoid it. Upon deformation, mechanical twinning occurs. Early plastic instabilities arise due to the fine substructure with high defect density, resulting in profuse shear banding. Such shear bands carry most of the subsequent deformation, reducing the volume fraction of oxide particles along these regions due to enhanced particle dissolution via cracking/fragmentation. Upon annealing, the cold-rolled specimens show abnormal <110> || ND grains nucleating at shear bands. The earlier recrystallization onset and fragmented particle dissolution in shear bands result in a local lower Zener pinning and generate a size advantage for <110> || ND grains. Based on this investigation, abnormal growth may be triggered by shear bands in cold-rolled and annealed LPBF alloys for grain boundary engineering. Our results suggest that avoiding shear banding (and the consequent particle fragmentation) inhibits abnormal grain growth, thus yielding a more uniform and fine-grained microstructure.

© 2021Alloys manufactured by laser powder-bed fusion have intrinsic and hierarchical microstructural features inherited from the fast solidification (up to 104 K/s) and subsequent thermal cycles. This creates epitaxed grains, dislocation cell structures, and second-phase oxide nanoparticles. Epitaxed grains follow a pattern where finer grains are found in the melt pool centerline along the laser track. Upon further annealing, this characteristic microstructure has pronounced consequences on the recrystallization mechanisms and thus on grain topology. By changing the scanning strategy, we control the emerging grain patterns in a representative alloy (AISI 316L austenitic stainless steel) by creating linear strings for unidirectional scans, while a chessboard grain pattern arises by applying a 90°-rotation between layers. Upon post-processing annealing (at 1150 °C from 15 min to 8 h), we study the relationship between the as-built and recrystallized microstructures. Recrystallization starts with fine nuclei in regions with high dislocation density along the melt pool centerlines, resulting in early-stage linear impingement (linearly clustered nucleation), as revealed by microstructural path analysis. Recrystallization is sluggish, due to dynamic Zener-Smith pinning. This effect leads to jerky boundary motion due to periodic pinning and depinning from oxide particles, caused by their gradual coarsening. Lower nuclei number density slows kinetics for the case of unidirectional scanning, while twinning aids in the nucleation of grains with mobile grain boundaries. Our findings show that changes in the laser scanning strategy are a suitable design tool for tailoring recrystallization and thus microstructure.

© 2021 Elsevier B.V.The annealing behavior of cold-rolled 317L austenitic stainless steel was investigated. The material was rolled to a true strain (ε) of 2.04 and subjected to both stepwise and continuous annealing up to 1000 °C, the latter conducted in the presence of an external magnetic field. Electron backscatter diffraction, dilatometry, thermodynamic calculations, Vickers microhardness testing, and electron channeling contrast imaging were used to follow the microstructure evolution upon annealing. The microstructure of the cold-rolled steel has about 2.3% of strain-induced α′-martensite, 4% of delta ferrite, and austenite as the predominant phase. Eye-shaped deformation heterogeneities are also noticeable and contrast with the predominant lamellar structure typical of cold-rolled materials. Microstructure changes were followed by means of magnetic measurements, with emphasis on both Ms (saturation magnetization) and Hc (coercive field) parameters. Our findings confirm the occurrence of austenite reversion, decrease of delta ferrite, and massive sigma phase precipitation for the annealing temperature and time intervals herein investigated. At 800 °C the steel is almost fully recrystallized, except for the eye-shaped structures, in whose interior precipitation is much less intense. Precipitation of sigma phase occurs preferentially at the delta ferrite lamellae. Magnetization was able to capture the fragmentation of the ferromagnetic delta ferrite lamellae due to sigma phase precipitation and the changes associated with the decrease of delta ferrite and austenite reversion upon annealing.

© 2021 Elsevier Inc.The 15-5PH (UNS S 15500) stainless steel combines high mechanical strength, ductility, and good corrosion resistance for aircraft and aerospace applications. This set of properties and its high added-value applications make it an excellent choice for additive manufacturing processes such as laser powder-bed fusion (LPBF). However, there is a need to understand the complex microstructure developed in LPBF-processed parts, which may show particularities such as columnar solidification, preferential orientation, different kinds of porosities, chemical segregation along the melt pools, metastable phases, and oxide nanoinclusions. We report the microstructural characterization of LPBF-processed 15-5PH stainless steel in the as-built condition and after aging. Low porosity (<1%), high hardness (420 HV0.1), and a large amount of retained austenite (15%) were found in the as-built samples. The microstructure shows the usual “fish scale”-like morphology. Grain size and hardness vary depending on the location within the melt pools. Reconstruction of the parent grains from EBSD maps indicates a microstructural refinement due to in situ reaustenitization of parts of the previous consolidated layers, where these heat-affected zones are harder and present larger amounts of retained austenite. After aging, as-built samples were harder and more resistant to overaging than annealed or wrought counterparts. Transmission electron microscopy reveals a large amount of nanometric crystalline silicon-oxide inclusions, indexed as cristobalite. The combination of fine-grained martensite, coherent Cu-rich clusters, nanometric oxide particles, and retained austenite makes LPBF-processed 15-5PH stainless steel a very promising material for high-end structural applications.

© 2020 Elsevier B.V.Strain-induced α′-martensite and austenite reversion in a cold rolled UNS S32304 lean duplex steel were tracked by means of magnetic measurements, with emphasis on both Ms (saturation magnetization) and Hc (coercive field) parameters. Grain-averaged quality metrics derived from EBSD (electron backscatter diffraction) analysis were also used to distinguish the phases during austenite reversion. The material was cold rolled to a true strain (ε) of 1.61 and subjected to isothermal and continuous annealing, the latter conducted in the presence of an external magnetic field. The evolution of the α′-martensite fraction upon straining and after isothermal annealing was monitored by coupling the Ms values and thermodynamic simulations, as well as from EBSD analysis. For the isothermally annealed material (ε = 1.61), the overall behavior of Ms and hardness displayed similar trends with a strong decrease for temperatures higher than 500 °C, suggesting austenite reversion. Results confirmed the occurrence of austenite reversion for the temperature interval investigated here. At 800 °C, austenite reversion is complete, and the steel is fully recrystallized. Besides, from the EBSD analysis, evidence of ferrite transformation into austenite was rather noticeable, in accordance with thermodynamic simulations and magnetic probing. Complementary electron channeling contrast imaging (ECCI) revealed that precipitation reactions mainly occur in the recrystallized austenite at 700 and 800 °C. The Hc behavior of both, the strained and annealed conditions was inferred to be mostly driven by microstructural changes in ferrite.

© 2020 Trans Tech Publications Ltd, Switzerland.In this work, the consolidation of blended elemental powders of iron, manganese and aluminum (Fe-25Mn-15Al wt.%) was performed by Equal Channel Angular Pressing (ECAP). Samples were consolidated at room temperature in a Φ = 120° die by a single pass and a second pass in route A. Both samples were heat treated at 650 °C and water cooled. Prior to heat treatment, samples presented a dense but chemically inhomogeneous structure. Fe and Al particles were highly deformed, whereas, Mn was almost undeformed. Mn particles were partially shattered by friction with Fe and Al particles. After heat treatment, the samples were characterized by SEM-EDX and presented substantial interdiffusion along the particles interfaces. It is believed that higher deformations by ECAP may improve the sinterability of consolidated samples in order to densify and chemically homogenize it.

© 2019 Elsevier B.V.A computer program was employed to reconstruct the parent microstructure from electron backscatter diffraction maps taken from martensite. The reconstruction is based on a given user-selected orientation relationship. Two reduced-activation ferritic-martensitic Eurofer steels were austenitized for several times and cooled down at different rates. Two parameters are proposed to assess the quality of the reconstruction: the relative frequency of orientations in a determined sub-portion of the Euler space and the distribution of the angular deviation from a given theoretical orientation relationship. The number of active martensitic orientation variants during the transformation depends on grain size. Coarser grains enable a greater number of active variants improving the reconstruction quality. The distributions of angular deviations reveal that the Greninger-Troiano orientation relationship is the one that best describes the martensitic transformation in both steel grades.

© 2019 Universidade Federal de Sao Carlos. All rights reserved.Equal channel angular pressing (ECAP) is one of the severe plastic deformation processes that can also be used for metallic powder consolidation. Consolidation of blended elemental powders of iron, chromium, nickel, and manganese (Fe-25Cr-20Ni-2Mn wt. %) was performed at room temperature in a Φ= 120° die by 1 and 2 passes. SEM micrographs indicated that single pass ECAP consolidated sample presented close to full densification. Additional pass of ECAP led to hardness increase and to an apparent better mixing between the different particles. SEM/EDX analysis made before and after heat treatment of the samples showed that effective diffusion only took place after heat treatment and especially in the sample subjected to 2 ECAP passes. Results indicate that alloying by ECAP consolidation and posterior heat treatment is feasible, especially for systems that cannot be processed by conventional means, as well as mechanical alloying.

© 2017 Acta Materialia Inc.We characterized the morphology, substructure and crystallography of lenticular martensite in a Fe-Ni-C alloy by means of electron backscatter diffraction and scanning electron microscopy. Electron backscatter diffraction maps were used to determine the orientation relationship between austenite and martensite across large regions of the microstructure. We employed orientation distribution functions as a statistical representation method for the observed orientation relationships. High-resolution point-to-point scans were used to normalize the effects of the orientation changes in the austenite caused by the plastic deformation during the formation of lenticular martensite. The analysis revealed that most of the transformation in this material follows an orientation relationship close to the one proposed by Greninger and Troiano.

A [211]-oriented niobium single crystal was deformed by equal channel angular pressing (ECAP) at room temperature using the route Bc to a total strain of 9.2. A sharp cube texture develops after ECAP processing. The deformed samples were annealed in vacuum from 400ºC (673 K) to 900ºC (1173 K) for 1 h to evaluate their microstructural stability. Scanning electron microscopy (SEM) was used to image the microstructures of as-deformed and annealed specimens. Electron backscatter diffraction (EBSD) was employed to determine the respective microtextures before and after annealing. Coarsening of the microstructure occurs at a maximum rate at 550ºC (823 K) due to discontinuous recrystallization. Normal grain growth replaces discontinuous recrystallization as the main coarsening mechanism above 700ºC (973 K).

© 2017 Elsevier B.V.Strain partitioning and texture evolution of AISI 201 austenitic stainless steel were investigated upon cold rolling up to a true strain of ε = 0.92. ε-martensite formation is the main work hardening mechanism at low strains (ε = 0.11). With increasing strain, the volume fraction of α’-martensite increases with a sigmoidal-like behavior. Remaining untransformed austenite is intensely fragmented by mechanical microtwins. The in-grain misorientation increases for all phases up ε = 0.51 and then levels off for further strain. Strain partitions evenly between austenite and α’-martensite during cold rolling. X-ray texture measurements revealed that austenite develops Goss, Brass and S texture components up to the largest investigated strain. The presence of Brass component at the highest deformation seems to be assisted by mechanical twinning. The texture components of α’-martensite belong to the α- and γ- fibers. Texture evolution of ε-martensite was followed by electron backscatter diffraction data and results show that texture evolves up to ε = 0.51 and remains nearly unchanged at larger strains, similarly as observed for austenite and α’-martensite.

© 2017 Elsevier B.V.Oxide-dispersion strengthened materials are important candidates for several high-temperature structural applications in advanced nuclear power plants. Most of the desirable mechanical properties presented by these materials are due to the dispersion of stable nanoparticles in the matrix. Samples of ODS-Eurofer steel were annealed for 4320 h (6 months) at 800 °C. The material was characterized using atom probe tomography in both conditions (prior and after heat treatment). The particles number density, size distribution, and chemical compositions were determined. No significant changes were observed between the two conditions indicating a high thermal stability of the Y-rich nanoparticles at 800 °C.

© 2017, ASM International.Reduced-activation ferritic-martensitic (RAFM) steels are potential candidates for structural applications in future nuclear fusion power plants. A Ta-containing Fe-based commercial thermodynamic database was employed to calculate the phase volume fractions and their chemical compositions in Eurofer-97 RAFM steel. Results of the calculations were compared to those obtained from transmission electron microscopy, atom probe tomography and dilatometric experiments performed on short-term annealed samples. Despite minor discrepancies between experimental and calculation data, our findings suggest that the employed database is effective for calculating the phase equilibrium fields for Ta-containing steels.

© 2014 Elsevier B.V. All rights reserved.(Figure Presented). Reduced-activation ferritic-martensitic Eurofer-97 and ODS-Eurofer steels are potential candidates for structural applications in advanced nuclear reactors. Samples of both steel grades in the as-tempered condition were austenitized in vacuum for 1 h from 900 °C to 1300 °C followed by air cooling to room temperature. The microstructure was characterized by dilatometry, electron backscatter diffraction (EBSD), and X-ray diffraction (XRD). Thermodynamic calculations provided by Thermo-Calc software were used to determine their transformation temperatures. Even having similar chemical composition, important changes were observed after martensitic transformation in these steels. Significant austenitic grain growth was observed in Eurofer-97 steel leading to the development of coarser martensitic packets. Contrastingly, austenitic grain growth was prevented in ODS-Eurofer steel due to fine and stable dispersion of Y-based particles.

Oxide-dispersion strengthened ferritic martensitic steels such as ODS-Eurofer grade are good candidates for structural applications in future fusion power reactors. Long-term annealing treatments in vacuum were carried out in cold-rolled samples (80% reduction in thickness) from 1 h up to 4320 h (6 months) at 800 °C, i.e. the maximum temperature in the ferritic phase field, to follow its softening behavior. The microstructural stability of this steel was mapped using several characterization techniques including scanning electron microscopy, transmission electron microscopy, electron backscatter diffraction, Vickers microhardness testing, X-ray diffraction texture measurements, low-temperature electrical resistivity, and magnetic coercive field measurements. ODS-Eurofer steel displays good microstructural stability. Discontinuous recrystallization occurs at the early stages of annealing resulting in a low volume fraction of recrystallized grains. Extended recovery is the predominant softening mechanism at this temperature for longer times. © 2014 Elsevier B.V. All rights reserved.

Pore-boundary interaction plays an important role in densification during solid-state sintering. This paper reports the evolution of porosity and grain size in niobium sintered at 2073 and 2273 K for different sintering times. The densification curves show a decrease in porosity up to 8 and 4 vol.% after 10,800 s for the samples sintered at 2073 and 2273 K, respectively. Grain growth is observed to take place together with this decrease in porosity. A new model for grain growth inhibition during sintering is proposed for connected porosity. This model considers that the moving grain boundaries and the outer surface of cylindrical pores remain in contact during grain growth and that energy dissipation takes place owing to the fact that the grain boundary is moving relative to the porosity. Our mechanism is akin to a friction between the grain boundary and the connected porosity at their contact region. In contrast to the traditional particle-grain boundary bypassing mechanisms, the present model is not a purely geometrical relationship but is material dependent. The model gives agrees well with experimental results obtained in this paper for sintered niobium as well as for other sintered materials reported in the literature. Our model is a novel approach to treating grain growth inhibition by pores during the sintering stage in which the porosity becomes interconnected. © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.