Selective laser melting (SLM), taking advantage of its inherent rapid cooling rates and near-net-shape forming ability, has been employed to fabricate bulk metallic glasses (BMGs). However, crystallization is frequently triggered during the SLM process, which results in the loss of advantageous properties of BMGs, such as extremely high hardness and near-theoretical yield strength. Although many studies have been conducted to investigate SLM of BMGs, there is still a lack of knowledge about the microstructural and compositional evolution during the laser beam processing, particularly the micromechanical property response upon crystallization. In the present work, a systematic investigation is performed to gain a much better understanding about the evolution of microstructure and composition as well as the corresponding micromechanical property change during multiple laser beam melting. The material used in this study is an industrial-grade Zr-based BMG Zr59.3Cu28.8Al10.4Nb1.5 (AMZ4) with two different oxygen levels. AMZ4 demonstrates its good thermal stability by the fact that observable crystalline structure appears around the melt pool only after more than once laser beam treatment. The compositional stability of AMZ4 is manifested by the homogeneous elemental distribution on the melt pool area after even twenty-five laser beam remelting. The laser-metal interaction, melting and subsequent solidification are not effectively influenced by the emerging and expanding of crystallization zone (or heat affected zone, HAZ). Higher oxygen content results in not only a larger HAZ but also more quenched-in nuclei at the melt pool bottom. The HAZ does not exhibit a fully crystallized structure, but rather has a mixture of amorphous and crystalline phases. Crystallization of AMZ4 leads to an increase in hardness and Young's modulus of the material. © 2022 Elsevier B.V.

The gradient microstructures of surface layer in single crystal nickel-based superalloy were produced by creep-feed grinding. The mechanical properties (i.e., hardness, elastic modulus) and room-temperature (RT) creep behavior of such structures were evaluated using a nano-indentation technique. Results show that the gradient structures along depth from ground surface consisted of nanograins, submicron grains and lamellar-shape structures, and dislocation structures. Furthermore, it was found that the hardness and elastic modulus of gradient structures were higher by 8–10% than that of bulk material on average. However, the regions containing nanograins showed a remarkable increase in creep depth compared to bulk material, implying that the creep behavior of ground layer was changed unfavorably. The obtained stress exponents of gradient structures suggested that dislocation activities were the main mechanism for indentation creep deformation. © 2021 Elsevier B.V.

The service performance of the turbine blade root of an aero-engine depends on the microstructures in its superficial layer. This work investigated the surface deformation structures of turbine blade root of single crystal nickel-based superalloy produced under different creep feed grinding conditions. Gradient microstructures in the superficial layer were clarified and composed of a severely deformed layer (DFL) with nano-sized grains (48-67 nm) at the topmost surface, a DFL with submicron-sized grains (66-158 nm) and micron-sized laminated structures at the subsurface, and a dislocation accumulated layer extending to the bulk material. The formation of such gradient microstructures was found to be related to the graded variations in the plastic strain and strain rate induced in the creep feed grinding process, which were as high as 6.67 and 8.17 × 107 s-1, respectively. In the current study, the evolution of surface gradient microstructures was essentially a transition process from a coarse single crystal to nano-sized grains and, simultaneously, from one orientation of a single crystal to random orientations of polycrystals, during which the dislocation slips dominated the creep feed grinding induced microstructure deformation of single crystal nickel-based superalloy. © 2021 IOP Publishing Ltd.

A new wrought CrCoNi-based medium-entropy superalloy (MESA) was designed by changing the composition of a commercial superalloy of type C-263, which is used for stationary components in gas turbines. ∼5 at.% Cr and 0.85 at.% Ti + Al were added at the expense of Ni while the Ti/Al ratio was decreased. Owing to these modifications, the brittle η phase, which is stable in C-263 below 900 °C is no longer observed in C-264. Besides, the solvus temperature and volume fraction of the γ′ phase in the peak-aged state are larger in C-264 (∼935 °C, 13.5%) compared to C-263 (∼890 °C, 12.8%), resulting in superior tensile and creep properties. The stress and temperature dependencies of the creep rates were described by power-law and Arrhenius relationships. The stress exponents were between 4 and 5, while the apparent activation energies were 550 and 400 kJ/mol for C-264 and C-263, respectively. During creep at 880 °C in air, internal nitridation in both MESAs resulted in the formation of TiN precipitates, with C-264 being slightly more affected due to its higher nitrogen solubility. Due to its superior creep resistance, good malleability and machinability, the C-264 MESA is currently commercially available from VDM Metals International. © 2021 The Authors

Heavy plate steels with bainitic microstructures are widely used in industry due to their good combination of strength and toughness. However, obtaining optimal mechanical properties is often challenging due to the complex bainitic microstructures and multiple phase constitutions caused by different cooling rates through the plate thickness. Here, both conventional and advanced microstructural characterization techniques which bridge the meso- and atomic-scales were applied to investigate how microstructure/mechanical property-relationships of a low-carbon low-alloyed steel are affected by phase transformations during continuous cooling. Mechanical tests show that the yield strength increases monotonically when cooling rates increase up to 90 K/s. The present study shows that this is associated with a decrease in the volume fraction of polygonal ferrite (PF) and a refinement of the substructure of degenerated upper bainite (DUB). The fine DUB substructures feature C-rich retained austenite/martensite-austenite (RA/M-A) constitutes which decorate the elongated micrograin boundaries in ferrite. A further increase in strength is observed when needle-shaped cementite precipitates form during water quenching within elongated micrograins. Pure martensite islands on the elongated micrograin boundaries lead to a decreased ductility. The implications for thick section plate processing are discussed based on the findings of the present work. © 2021, The Author(s).

Tempered martensite ferritic steels (TMFSs) have been and are being used for critical components in high temperature plant operating in the 600 °C range. They are exposed to creep conditions for long time periods, exceeding 100,000 h. In the present study we investigate a 12% Cr TMFS, after creep-testing at 550 °C at 120 MPa for 139,000 h. We had previously investigated this material in the TEM using thin foils. We now use an extraction replica technique to analyze four particle families: M23C6, MX, Laves-phase and Z-phase, considering statistically relevant numbers of particles (between 120 and 720). We show how EELS mapping can help in identifying Z-phase particles and use Cr-V-maps to differentiate between the four particle families. The chemical evolution of particles is investigated. The experimental results are discussed in the light of previous thin foil data and with respect to predictions from computational thermodynamics. The strength and weakness of thin foil and replica procedures are compared. Improvements for thermodynamic databases are suggested. © 2021

Abstract: The present work shows that thermal expansion experiments can be used to measure the γʼ-solvus temperatures of four Ni-base single-crystal superalloys (SX), one with Re and three Re-free variants. In the case of CMSX-4, experimental results are in good agreement with numerical thermodynamic results obtained using ThermoCalc. For three experimental Re-free alloys, the experimental and calculated results are close. Transmission electron microscopy shows that the chemical compositions of the γ- and the γʼ-phases can be reasonably well predicted. We also use resonant ultrasound spectroscopy (RUS) to show how elastic coefficients depend on chemical composition and temperature. The results are discussed in the light of previous results reported in the literature. Areas in need of further work are highlighted. Graphical abstract: [Figure not available: see fulltext.] © 2021, The Author(s).

The present work contributes to a better understanding of the basic assumptions and principles behind the design of Ni-based single crystal superalloys (SXs). For this purpose, we cast and heat-treat four Ni-based single crystal superalloys (SXs) and compare their creep performances: ERBO/1 (with Re) and three ERBO/15 variants (no Re but increased levels of Ti, Mo and W). We show that Re can be replaced by other elements without losing creep strength. To come to this conclusion one has to consider both, alloy composition and microstructure. We analyze the mechanical, microstructural and chemical results (creep rates, γʼ-volume fractions, average γʼ-particle sizes, average γ-channel widths and the chemistry of γ- and γʼ-phases) obtained for ERBO/15 and its two leaner variants (less Mo: ERBO/15-Mo and less W: ERBO/15-W). ERBO/15-Mo and ERBO/15-W show higher creep rates than ERBO/15, because they exhibit lower Mo and W concentrations in the γ-channels. This results in higher diffusion rates, accelerated rafting and faster dislocation climb at γ/γʼ-interfaces. © 2020 The Authors

Collective interstitial ordering is at the core of martensite formation in Fe–C-based alloys, laying the foundation for high-strength steels. Even though this ordering has been studied extensively for more than a century, some fundamental mechanisms remain elusive. Here, we show the unexpected effects of two correlated phenomena on the ordering mechanism: anharmonicity and segregation. The local anharmonicity in the strain fields induced by interstitials substantially reduces the critical concentration for interstitial ordering, up to a factor of three. Further, the competition between interstitial ordering and segregation results in an effective decrease of interstitial segregation into extended defects for high interstitial concentrations. The mechanism and corresponding impact on interstitial ordering identified here enrich the theory of phase transitions in materials and constitute a crucial step in the design of ultra-high-performance alloys. © 2020, The Author(s), under exclusive licence to Springer Nature Limited.

Combining high-resolution transmission electron microscopy (HR-TEM) and 3-dimensional atom probe tomography (3D-APT), the early stages of nucleation and growth of vanadium carbonitrides (VCN) were revealed. VCN nucleation starts with locally distorted body-centered cubic (bcc) lattices due to a substitution of Fe atoms by V atoms, which results in the formation of an intermediate coherent crystal structure within the ferrite matrix. Misfit strain self-accommodation leads to twining within the VCN particles. As the particles grow, the precipitates gradually lose coherency and grow into discs or plates. Simultaneously, the intermediate crystal structure of the nucleus transforms into the equilibrium VCN-structure. © 2020

This research paper presents the attempt at ultrashort pulsed laser shock peening with absence of absorptive layer and confining medium which could enhance surface microhardness and the abrasion property of NiTi shape memory alloy. The average roughness values of NiTi specimen were measured on the surface, because the roughness would affect the friction resistance. The microhardness and Young's modulus were investigated at different position of single laser spot by nanoindentation technique. The pin-on-plate sliding abrasion testing were performed with different load-force (0.5 N and 2 N) for different testing time. Results showed that ultrashort pulsed laser shock peening treatment would cause a significant improvement on friction coefficient and abrasion property, which was attributed to the change of surface modification, such as roughness, microhardness, microstructure and titanium oxide layer, but the ultrashort pulsed laser shock peening treatment did not enhance its tensile strength during present research. © 2020 Elsevier B.V.

The microalloying of low-alloyed steels with Nb can improve the strength-to-toughness balance. Such an effect of Nb is usually ascribed to the refinement of the grain structure occurring in the austenite regime during hot forming. In the present work, we report that Nb enhances the impact toughness of a low-alloyed Cr–Mo steel by a mechanism which has not been appreciated so far. The lower impact toughness in the Nb-free Cr–Mo steel is due to segregation of Mo to boundaries, which facilitates the formation of fine Mo-rich ξ-phase carbides lining up along the boundaries. This further promotes the nucleation and propagation of microcracks. The addition of Nb leads to the formation of Mo-enriched NbC particles. The interfaces between these particles and the matrix supply new preferential sites for precipitation of Mo-rich ξ-phase carbides upon subsequent tempering. In this way, Nb additions result in a decrease of Mo segregation to boundaries, significantly reducing the precipitation of ξ-phase carbides on grain boundaries, thus leading to improved impact toughness. In addition to the classical microstructural explanation (grain size effect), this chemical role of Nb sheds new light on the design strategies of advanced low-alloyed steels with optimized strength-to-toughness ratios. © 2019, Springer Science+Business Media, LLC, part of Springer Nature.

In the present work, we study the effect of HIP rejuvenation treatments on the creep behavior and residual life of a pre-crept single crystal Ni-base superalloy of type CMSX-4. The present work combines miniature creep experiments of precisely oriented [001]tensile creep specimens with HIP treatments and quantitative analysis of scanning and transmission electron micrographs. A HIP-rejuvenation treatment after 5.0% creep pre-strain significantly improves creep strength. However, the microstructural damage induced by the creep pre-deformation could not be fully removed. In a series of sequential creep/HIP/creep-experiments, increasing levels of pre-deformation result in increasing levels of creep rates even after identical HIP-rejuvenation treatments. The memory effect, which causes this phenomenon, is related to an accumulation of permanent microstructural damage, which is not associated with rafting or cavitation. The mechanical results obtained in the present work are interpreted based on microstructural results on the γ/γʼ-microstructure (γ-channel widths and γʼ-size), on the pore population (number density of pores, pore size distributions and pore area fractions)and dislocation substructures which have formed during creep. The results are discussed in the light of previous results reported in the literature. © 2019 The Authors

The strength and toughness of low alloyed ferritic/bainitic steels depend on their microstructure, which evolves during thermo-mechanical treatments along the processing chain. Chromium-molybdenum steel microstructures are complex. Therefore, only a limited number of attempts have been made to fully characterize carbide populations in such steels. In the present work, analytical transmission electron microscopy is employed to study the microstructure of a low alloyed chromium-molybdenum steel, which features ferritic (F, mainly α-iron and niobium-carbides) and bainitic (B, α-phase, dislocation, grain/subgrain boundaries, various MxCy carbides) regions. The crystal structure and chemical nature of more than 200 carbides are determined and their distributions in the two microstructural regions are analyzed. The present work shows how particles can be identified in an effective manner and how the microstructural findings can be interpreted on the basis of thermodynamic calculations. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

An ex situ approach combining fast quenching experiments in a dilatometer and postmortem microstructural observation in transmission electron microscopy (TEM) has been used to observe the dynamic microstructure change during differential scanning calorimetry (DSC) ramping of an Fe–10Cr–0.15C (wt%) alloy fabricated from high-purity components. The DSC measurements reveal two exothermic events at temperatures about 270 and 600 °C in a heating process. The two events were discerned by TEM investigations on specimens interrupted during thermal ramping in a dilatometer. It is found that precipitation and growth of M3C carbide occurred first in a temperature range between 200 and 400 °C, following the Bagaryatskii orientation relationship. Subsequently, M7C3 carbides precipitate on prior martensitic laths boundaries in a temperature range between 500 and 700 °C at the expense of M3C. M23C6 carbides were found precipitating on the interface between M7C3 and matrix at approximately the same time with the precipitation of M7C3. The obtained results are also compared with an in situ TEM heating experiment, and differences between the two approaches are discussed. © 2018, Springer Science+Business Media, LLC, part of Springer Nature.

Steels belong to one of the best established materials, however, the mechanisms of various phase transformations down to the nano length scale are still not fully clear. In this work, high-resolution transmission electron microscopy is combined with atomistic simulations to study the nanoscale carbide precipitation in a Fe–Cr–C alloy. We identify a cooperative growth mechanism that connects host lattice reconstruction and interstitial segregation at the growing interface front, which leads to a preferential growth of cementite (Fe3C) nanoprecipitates along a particular direction. This insight significantly improves our understanding of the mechanisms of nanoscale precipitation in interstitial alloys, and paves the way for engineering nanostructures to enhance the mechanical performance of alloys. © 2018, The Author(s).

The process and kinetics of carbide precipitation upon tempering of an Fe-10Cr-0.15C (wt.%) alloy fabricated from high-purity components has been studied. Differential scanning calorimetry reveals three exotherms in a temperature range of 100-700°C. Using advanced electron microscopy and Kissinger analysis, the exothermic processes have been interpreted. Cementite precipitated first upon tempering at temperatures as low as 200°C; M7C3 and M23C6 appear at higher temperatures, precipitating at approximately the same time but on different sites (M7C3 within grains and laths and M23C6 on grain and lath boundaries). Subsequently, the more stable M23C6 coarsens at the expense of M7C3, which dissolves. The first exotherm was interpreted as being related to the precipitation of cementite whilst the other two overlapping exotherms were interpreted as relating to the concurrent precipitation and coarsening of M7C3 and M23C6, respectively. In-situ SEM and TEM observation is being conducted in order to obtain a more precise understanding and further validate the interpretation of the DSC results. © 2015 Materials Research Society.

Manganese sulfide is often referred to as one of important inhibitors in grain-oriented electrical steels, which is of great importance to yield strong Goss texture. However, the early stage of nucleation for such inhibitors and their evolution during the processing has not been well understood. In present work we selected a Fe—3.12wt.%Si—0.11wt.%Mn—0.021wt.%S model system and used FE-SEM and atom probe tomography (APT) to investigate the precipitation behavior of MnS inhibitors at near atomic scale. It was found that the Si—S enriched clusters with sizes of 5—15 nm were formed close to the MnS particles. The density of inhibitors decreased after large pseudo-plane-strain compression because of the effect of dislocation motion, and then slightly increased again when sample was aged at 200°C for 48 h. The dislocations and grain boundaries can act as fast diffusion paths and assist the reemergence of Si—S enriched clusters. © 2016, Higher Education Press and Springer-Verlag Berlin Heidelberg.

Nano-crystalline (NC) 316L austenitic stainless steel sample was prepared by means of High Pressure Torsion (HPT) and post-deformation annealing. Uniaxial tensile tests at room temperature showed the nano-crystalline sample exhibits extreme high yield strength up to 2230. MPa, which is the highest ever reported in the literature. © 2012 Elsevier B.V.

SUS 304 austenitic stainless steel (ASS) was deformed by high pressure torsion (HPT) to obtain 100% volume fraction of martensite (α') from a fully austenitic (γ) matrix. Deformation caused an increase in hardness (Hv) from 1.6 GPa in the as annealed state to 6.4 GPa after HPT. Deformed samples were then annealed in the range 200 - 600°C and peak hardness of 7.8 GPa was observed after annealing at 400°C for 1 hour. Differential scanning calorimetry (DSC) and electrical resistivity tests showed that the deformed alloy undergoes a two stage phase transformation on heating from room temperature up to 700°C. The first stage of transformation was associated with hardening behavior while the second one which is reverse α' → γ transformation resulted in a reduction in hardness. Annealing at 400°C after deformation was found to increase the magnetization saturation (Msat) values.

SUS316L austenitic stainless steel was subjected to severe plastic deformation (SPD) by the method of high pressure torsion (HPT). From a fully austenitic matrix (γ), HPT resulted in phase transformation from γ→α'. The largest volume fraction of 70% α' was obtained at 0.2 revolutions per minute (rpm) while was limited to 3% at 5rpm. Pre-straining of g by HPT at 5rpm decreases the volume fraction of α' obtained by HPT at 0.2rpm. By HPT at 5rpm, α'→γ reverse transformation was observed for α' produced by HPT at 0.2rpm. © (2011) Trans Tech Publications.