A new steel was designed for high-performance applications under extreme conditions by combining a martensitic microstructure and the co-precipitation of nano-sized MC and B2-NiAl precipitates, along with the ability to generate a protective Al-rich oxide scale. This study focuses solely on the long-term stability of this alloy during tempering at 550 and 650 °C for holding times exceeding 1000 h. At 550 °C, very fast precipitation of fine B2-NiAl particles occurred, providing remarkable strengthening even after annealing for 1100 h, while preventing the microstructural coarsening of the martensite blocks. In contrast, tempering at 650 °C induced the rapid coarsening of the B2-NiAl precipitates and the formation of precipitate-free zones. This accelerated microstructural evolution led to a more pronounced decrease in hardness compared to samples treated at 550 °C though the hierarchical martensitic microstructure was also retained. Nevertheless, it is observed that at 650 °C, (Cr, V)23C6 carbides formed instead of the MC particles, in accordance with kinetic calculations carried out. The enhanced durability at temperatures below 650 °C suggests that this novel alumina-forming martensitic steel could be a suitable candidate for applications requiring long-term thermal stability under harsh environments.
Two alumina-forming martensitic (AFM) steels containing less than 8 wt.% Cr were exposed for over 1000 h at 550 degrees C and 650 degrees C in static liquid Pb with controlled oxygen concentration to evaluate the formation of an alumina oxide scale and its protective capacity against corrosion. The AFM-1 steel (3.6 wt.% Al, 7.8 wt.% Cr) formed a continuous, protective oxide scale that effectively resisted Pb penetration under all conditions, particularly at 650 degrees C, where performance improved due to the dissolution of B2-NiAl precipitates during prolonged exposure, releasing Al that migrated to the surface and enabled the formation of an Al-rich oxide layer, ensuring sustained protection and mitigating the localized nodular oxidation observed at 550 degrees C. In contrast, the AFM-2 steel (2.9 wt.%Al, 7.5 wt.% Cr) failed to develop a complete protective oxide layer, allowing molten Pb to penetrate and react with the substrate even at 650 degrees C, causing severe oxidation. These results demonstrate that, beyond a high Ni content (12 wt.%), achieving excellent corrosion resistance in liquid Pb requires a synergistic combination of an optimal Al/Cr balance, dissolution of B2-NiAl precipitates as an Al source, and enhanced atomic diffusion facilitated by the high density of subgrain boundaries in the martensitic microstructure.
Although retained austenite is present in minor amounts in as-built additively manufactured-maraging steels, its evolution during ageing is key to controlling the final microstructure. This study investigates the relationship between austenite reversion and precipitation evolution during ageing, particularly whether these processes compete or cooperate. Using Scanning/Transmission Electron Microscopy, Atom Probe Tomography and Thermo-Calc (R) PRISMA simulations, the presence and evolution of retained austenite, Ni3Ti and Fe7Mo6 inter-metallic phases was characterised across different ageing conditions. Experimental results revealed the presence of non-enriched austenite in the as-built condition. Nevertheless, with increasing ageing temperature, Ni and Mo segregation became evident. High-Resolution Transmission Electron Microscopy revealed that Ni3Ti precipitation primarily occurred within the martensitic matrix, while Fe7Mo6 nucleated preferentially at the austenitemartensite interface. PRISMA simulations indicated early and rapid precipitation in solute-enriched areas (i.e., intercellular regions), with Ni3Ti forming prior to Fe7Mo6. Both experimental and simulation results suggested Ni diffusion controls retained austenite growth, while Ti and Mo drive Ni3Ti and Fe7Mo6 precipitation, respectively. The evidence reported in this work supports a both collaborative and independent phase transformation mechanism, where austenite reversion and precipitation co-evolve.
Solute distribution during the laser-based powder bed fusion of metals process is highly complex because of solidification. This study builds on a previous investigation of how solute heterogeneities across different scales influence phase distribution and aging physical phenomena in a Fe-18Ni-9Co-5Mo-Ti maraging steel (Santana et al. in Addit Manuf 104494, 2024). Previous work using energy-dispersive X-ray spectroscopy revealed heterogeneous Ni and Mo enrichment at intercellular regions. Using X-ray diffraction, 8 ± 3
The Laser Powder Bed Fusion process involves complex thermodynamic and heat transfer mechanisms which results in a complicated understanding of the material's microstructure and phase transformation processes. In the case of additive manufacturing maraging steels, these present heterogeneous structures which mainly consist of Body-Centred Tetragonal (BCT) martensite and retained austenite (Face-Centred Cubic (FCC) phase structure), unlike conventionally processed material. Research has already been done on the competitive or collaborative nature of austenite growth/reversion and precipitation in these materials. However, for Laser Powder Bed Fusion maraging steels, studies have focused on either the effect of the heterogeneous structures on austenite reversion kinetics or the formation, evolution and behaviour of precipitation. Still, no comprehensive research exists that covers in detail the relation between solute heterogeneity from the meso- to the nanoscale and its influence on both phase distribution and ageing physical phenomena. To do so, multiscale chemical analyses and microstructural characterisation techniques were used to investigate a maraging steel M300 in different transformed conditions: as-built, aged at 480 and 540 degrees C. The results showed that competing mechanisms during printing caused segregation at the mesoscale, which remains in aged samples. Vaporisation led to Cr segregation, while melt convections caused Ni and Ti depletion at melt pool boundaries. Retained austenite location was found at melt pool boundaries and away from them on the as-built structure. Its preferential location remains unclear. Dissimilarities from conventional material were identified in nanosized clustering and precipitates on aged samples.
There is a need worldwide to develop materials for advanced power plants with steam temperatures of 700°C and above that will achieve long-term creep-rupture strength and low CO2 emissions. The creep resistance of actual 9-12Cr steels is not enough to fulfil the engineering requirements above 600°C. In this paper, the authors report their advances in the improvement of creep properties of this type of steels by the microstructural optimization through nano-precipitation using two methodologies. 1) Applying a high temperature austenitization cycle followed by an ausforming step (thermomechanical treatment, TMT) to G91 steel, to increase the martensite dislocation density and, thus, the number density of MX precipitates (M = V,Nb; X = C,N) but at the expense of deteriorating the ductility. 2) Compositional adjustments, guided by computational thermodynamics, combined with a conventional heat treatment (no TMT), to design novel steels with a good ductility while still possessing a high number density of MX precipitates, similar to the one obtained after the TMT in G91. The microstructures have been characterized by optical, scanning and transmission electron microscopy, EBSD and atom probe tomography. The creep behaviour at 700°C has been evaluated under a load of 200 N using small punch creep tests.
In this work, a high-performance maraging steel M300 was processed by laser powder bed fusion, where the layer thickness and the laser emission mode were modified. As-built microstructures were studied by considering the metallurgical phenomena taking place during printing: melting of the material deposited over previous layers; rapid solidification of the melt pool; and martensite-to-austenite reversion and precipitation of intermetallic phases induced by the combined effects of repeated heating and cooling cycles in the process. After printed, parts were subjected to ageing treatments at temperatures ranging from 480 to 540 & DEG;C. Microstructural characterization results evidenced the importance of layer thickness as a key parameter to modify the solidification cell size of the as-built samples. Two different phases were identified from the X-ray diffraction patterns in the microstructure: BCT martensite and FCC austenite. It was found that the tetragonality of martensite remained constant across different layers for all as-built conditions regardless of the successive reheating cycles, which are experienced during subsequent melting passes. No significant effect of the studied printing parameters was observed on the evo-lution of the microstructure during ageing. Finally, it was observed that the hardness of aged microstructures is comparable to that obtained by conventional manufacturing methods.& COPY; 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Grade 316 L is one of the most versatile austenitic stainless-steel products whose potential in laser powder bed fusion has been recently evaluated. A way of improving its properties is to add reinforcements, such as TiC nanoparticles, to promote dispersion hardening. However, it is often difficult to assess microstructure-mechanical property relationships, since particle inoculation promotes heterogeneous nucleation of equiaxed grains during rapid solidification. In this work, two 316 L samples were manufactured by laser powder bed fusion, where the powder of one of them was inoculated with TiC nanoparticles. The effect of inoculants on the microstructure and its high temperature behavior was assessed. Electron Probe Micro Analyzer proved that inoculants did not get dissolved during the printing process and they predominately lay in the intercellular regions, which were solute enriched. Advanced characterization proved that inoculation did not affect the solidification structure, which remained cellular and with a similar size, or the grain size, although it did modify the bulk texture. Finally, the effect of dispersion hardening on the behavior at high temperature of a 316 L steel was evaluated by small punch tests, which proved that the addition of TiC improves all, ductility, yield strength and ultimate tensile strength at high temperature. Moreover, samples processed by LPBF showed high temperature behavior and superior strength and ductility, as compared to the ones obtained in a reference annealed steel, even though the grain size obtained in the former case was at least 50 times larger than the one obtained for the reference condition.
Among the materials that might be manufactured with laser powder bed fusion (LPBF), one can highlight maraging steels, with excellent weldability, strength and fracture toughness. However, the effects of the processing parameters and the mechanisms governing the as-built texture are not clear yet. A recent publication showed a low texture index in the prior austenite, in contrast to other alloys subjected to LPBF with the same strategy. Authors suggested several hypotheses, although no conclusions were drawn. This work aims to investigate these findings by using a 300 maraging steel processed under different conditions, i.e. different printer, powder layer thickness and laser emission mode. To do so, X-Ray Diffraction, Electron Backscattered Diffraction and Scanning Electron Microscopy have been used. Results show that the heat treatment intrinsic to the LPBF process does not affect the prior austenite grains, whose texture and morphology remain unchanged throughout the process. Also, for the studied ranges, the microstructure texture is not related to the powder layer thickness or to the laser emission mode, although it could be affected by the laser power or the scan strategy. Finally, a low degree of variant selection has been observed, where the selected variants are those that contribute to a martensite cubic rotated texture.
The latest progress in machine learning (ML) algorithms enabled to predict some steel physical properties previously modelled by linear regression (LR), such as the Ms temperature. Authors claimed that the performance given by ML models could improve the one of previous LR models, although they did not include fair comparisons. In this work, a large database was used to train different ML algorithms, whose Ms temperature predictions were compared to the ones of previous literature empirical models. ML methods were proved to require longer computational times and wider knowledge, while leading to similar results. Therefore, we recommend that ML methods are not always considered as the first option when trying to solve easy problems that can be modelled by LR techniques.
The increasing trend of high strength low alloy steel application in the shipbuilding industry dictates the necessity for an investigation of their welds with conventional high strength steels. In this study, conventional and high strength low alloy naval steel plates 12 mm thick, were joined together in a butt joint configuration, using the metal cored arc welding technique and low heat input (1.0 kJ/mm). The weld was examined in terms of microhardness, microstructure, and tensile performance. The effect of multiple thermal cycles on the formation of primary and secondary microstructures was also discussed. The results revealed a smooth distribution of the microhardness across the different weld regions. Inside the heat affected zones (HAZs) and the weld metal various constituents were revealed, with ferrite in various forms (lath-like, acicular, semi-equiaxed, polygonal) appearing as the predominant phase, alongside martensite and austenite grains, and pearlite (lamellar and degenerated). The tensile testing indicated the base metal of the conventional high strength steel to be the weakest link of the weld, which was mainly attributed to its ferritic-pearlitic microstructure and the coarse grain size. The overall tensile performance of the weld remained at high levels, with a simultaneous reduction in the elongation after fracture in comparison to the base metals.
In this work, different heat treatments were performed in order to study two different bainite morphologies, granular and lath-like, obtained at different cooling rates in a low carbon microalloyed steel. For that purpose, advanced crystallographic characterization and quantitative metallography using SEM, EBSD and TEM were carried out. The evolution of the volume percentage, size, aspect ratio, retained austenite volume percentage and crystallography of the M/A constituents was studied as a function of the cooling rate and classified according to a machine learning algorithm. For the characterization of the crystallography and morphology of the bainitic ferrite matrix, two microstructures were selected as representative of granular and lath-like bainite. The results show that the main differences between granular and lath-like bainite are the size and shape of the M/A constituents, that change progressively from a mixture of large grains, coarse blocks and fine roughly equiaxed grains at low cooling rates to short and long films at high cooling rates. The crystallographic and morphological differences between both microstructures can be explained based on the different driving force and amount of bainitic ferrite formed at the different temperature ranges. These results confirm that the mechanisms by which granular bainite forms are not different from the transformation mechanisms of lath-like bainite.
There is a worldwide need to develop materials for advanced power plants with steam temperatures of 700°C and above which have the capacity to achieve high efficiency and low CO2 emissions. This request involves the development of new grades of 9-12Cr heat-resistant steels, with a nanostructured martensite, mainly focusing on the long-term creep rupture strength of base metal and welded joints, creep-fatigue properties, and microstructure evolution during exposure at such elevated temperatures. The main shortcomings of actual 9-12Cr high-chromium steels are that the creep resistance is not enough to fulfill the engineering requirements at temperatures higher than 600°C and the material undergoes a cyclic softening. Creep strength at high temperature could be improved by a microstructural optimization through nano-precipitation, guided by computational thermodynamics, and thermomechanical control process optimization.
In this work, the creep strengthening nanoprecipitation in novel heat resistant steels strengthened by a high density of stable nanoprecipitates has been studied. The results show that the high number density of MX nanoprecipitates within the martensitic laths in these steels comes from the great amount of MX former elements present in their chemical compositions and the high dislocation density generated by the martensitic transformation that takes place during cooling after austenitization. These dislocations act as nucleation sites for these nanoprecipitates during the tempering applied after the austenitization and quenching. Atom probe tomography measurements show that these nanoprecipitates are rich in Nb, V, Cr and N for the HDSN1 and HDSN2 steels and V, Cr and N for the HDSN3 steel. The distribution of the nanoprecipitates within the martensitic laths suggests that the creep strengthening produced by the Nb, V, Cr and N nanoprecipitates in the HDSN1 and HDSN2 steels is more effective at pinning dislocations at high temperature than that obtained in the HDSN3 steel by the V, Cr and N nanoprecipitates. However, the high amount of W in the HDSN3 steel enhances the solid solution strengthening at high temperatures, resulting in a similar high temperature strength for all HDSN steels.
Advance High Strength Steels (AHSS) have been widely used in the automotive industry during the last decades due to their excellent combination of strength and ductility and competitive cost. Current investigations focus on the development of a 3rd generation of AHSS with higher levels of strength and ductility and excellent formability while maintaining a competitive cost. This goal can be achieved by microstructural optimization through an appropriate thermomechanical treatment and chemical composition design. In this work, the effect of deformation and alloying elements on the continuous cooling phase transformations and final microstructures after different thermomechanical and heat treatments has been studied using different experimental techniques in three advance high strength steels microalloyed with Ti-Nb, Ti-Nb-Mo and Ti-Nb-Mo-V.
This paper reports on hardness, tensile properties and notch impact bending toughness values of an Fe20Cr4.5Al oxide dispersion strengthened (ODS) alloy specifically processed to achieved different preferential orientations: random, <100>, <110> and <111> parallel to the bar axis. In spite of the differences in the grain size, it was found for <100>, <111> and random orientations that the mean hardness values on the transverse cross sections is not remarkably sensitive to the texture. On the other hand, a significantly different mean hardness value for the material having the <110> crystalline orientation was found. Regarding the yield strength, it was found for random, <100> and <111> orientations that the yield strength is proportional to the Taylor’s factor. The difference between experimental and predicted yield strength values for <110> orientation was attributed to the offset effect induced by the dislocation cell size. The variation of the cleavage fracture strength with the texture was analyzed in the basis of two criteria: one based on the Normal Stress Law (macroscopic nature), and the other based on the assumption that fracture occurs from the propagation of a microcrack-like defect (microscopic nature). In this sense, it was concluded from the fractographic evidences that random and <100> orientations follow a mechanism where the fracture kinks along of the cleavage plane from a penny shaped microcrack nucleated in a second phase particle, meanwhile in the <110> and <111> orientations the fracture propagation arises from a penny shaped defect on the cleavage plane. Finally, the lower shelf values determined for the conditions studied are the same regardless of the texture and microstructure. The effect of texture on the notch toughness was noted where plastic flow predominates, i.e., in the ductile to brittle transition temperature and in the upper shelf energy.
Small Punch Creep technique was used as a screening procedure to evaluate the creep properties of different microstructures developed in a thermomechanical simulator. The goal seek was to generate alternative microstructures in a conventional ferriticmartensitic G91 steel grade which boost thermal stability at temperatures as high as 700 oC. The developed microstructures allow studying the effect of the austenitization temperature optimized by thermodynamic calculations and the ausforming on the creep strength and ductility. The improvement in creep strength recorded was attributable to a higher number density of MX precipitates. By contrast, these microstructures showed an important reduction in creep ductility.
In this work, differences and similarities between bainitic and martensitic structures obtained by isothermal heat treatments such as austempering, quench and partitioning (Q&P) and quench and tempering (Q&T), are investigated by multiple techniques including X-ray diffraction, electron backscatter diffraction, scanning and transmission electron microscopy and atom probe tomography. Results reveal that analogous lath-like ferritic structures with similar austenite content can be achieved by adjusting the isothermal holding temperature. However, certain variability in hardness is recorded, which is consistent with differences on the precipitation state revealed by the nano-scale examination of the structure, and with dissimilar crystallographic size distribution of ferritic grains.