The isothermal high‐temperature oxidation behavior of the equiatomic CrFeNi medium‐entropy alloy is a key issue that determines whether this material is suited for high‐temperature application. In this view, the understanding of the long‐term behavior is even more crucial than short‐term corrosion effects. Herein, a single‐phase CrFeNi alloy of the face‐centered‐cubic structure is exposed to synthetic air at 1000, 1050, and 1100 °C for 24, 100, and 1000 h and its oxidation behavior is systematically compared to that of 316L steel, which shows a surprising initial oxidation stabilization during early stages. The oxidation rate of CrFeNi is parabolic at 1000 °C (with a parabolic constant k p = 1.4·10 −5 mg −2 cm −4 s −1 ) and 1050 °C ( k p = 2.7·10 −5 mg −2 cm −4 s −1 ), but breakaway oxidation occurs at 1100 °C after 4 h of exposure. In all cases, the oxide scales are found to (at least) partially spall off. Chromium diffuses outward to form a Cr 2 O 3 layer at the gas/oxide interface, and a thin layer of (Cr, Fe, Ni) 3 O 4 is identified at the oxide/alloy interface. Unlike the 316L alloy, which contains more Mn and Fe, the CrFeNi alloy does not show any catastrophic oxidation behavior at the investigated conditions.

The gamma phases of CoNi-base superalloys are disordered solid solutions whose chemical complexity is similar to that of medium-entropy alloys. This study aims to investigate how compositional variations affect their thermal stability. As a starting point, the gamma composition (Co55.5Ni23Al3.1Cr11.5W5Ti1Ta0.2Si0.7Hf0.03 in at.%) of a precipitation hardened gamma/gamma' CoNi-base superalloy (ERBOCo-1), determined by atom probe tomography, was prepared as a bulk alloy. Nine alloys were then derived from this composition. First, four derivatives were designed by reducing the concentrations of one of the major elements (Co,Ni,Cr,W) by similar to 5 at.% and compensating by increasing the concentrations of the other major elements, while keeping the contents of the minor elements (Al,Ti,Si,Ta,Hf) constant. In another set of five alloys, the compositions of the reference alloy and the first four derivatives were simplified to quaternary or ternary alloys of the Cr-Co-Ni-W system so that the ratios between the major elements remained the same. The alloys were cast, homogenized, cold-worked, and annealed for up to 1500 h followed by microstructural and chemical investigations. The results provide a better understanding of the effect of individual elements on the stability of geometrically (chi) and topologically close-packed phases (C14 laves and G) in CoNi-base medium-entropy alloys. The chi phase proved to be the most common secondary phase, which stability and compositional range are strongly underestimated in some current thermodynamic databases (e.g. TCNI10). Therefore, the present study provides new data that may help in their further development for CoNi-base superalloys and medium-entropy alloys.

This work aims to predict the microstructure of recrystallized medium and high-entropy alloys (MEAs and HEAs) with a face-centered cubic structure, in particular the density of annealing twins and their thickness. Eight MEAs and five HEAs from the Cr-Mn-Fe-Co-Ni system are considered, which have been cast, homogenized, cold-worked and recrystallized to obtain different grain sizes. This work thus provides a database that could be used for data mining to take twin boundary engineering for alloy development to the next level. Since the stacking fault energy is known to strongly affect recrystallized microstructures, the latter was determined at 293 K using the weak beam dark-field technique and compared with ab initio simulations, which additionally allowed to calculate its temperature dependence. Finally, we show that all these data can be rationalized based on theories and empirical relationships that were proposed for pure metals and binary Cu-based alloys.

A two-step processing route including cold working (primary hardening) followed by annealing-induced (secondary) hardening is proposed to strengthen single-phase face-centered cubic CrCoNi-based medium-entropy alloys (MEAs). Here, we investigate two compositions (in at.%): Cr33.3Co33.3Ni33.3 and Cr27.3Co33.3Ni33.3Mo6. The former has received considerable interest and is now regarded as a model MEA. The latter was designed to investigate how replacing 6 at.% Cr with Mo affects mechanical properties and annealing-induced hardening. It is worth mentioning that this latter composition is similar to that of the industrial MP35N alloy (Cr22.9Co35.4Ni35.5Mo6.2), which is well-known to exhibit a strong annealing-induced hardening, but Cr27.3Co33.3Ni33.3Mo6 is outside its specification. In MP35N, it has long been thought that Mo segregation at planar defects is responsible for annealing-induced hardening. In the present work, we show that the strength of both Cr33.3Co33.3Ni33.3 and Cr27.3Co33.3Ni33.3Mo6 can be increased by ∼25% after post-deformation annealing, thus demonstrating that Mo is not essential to cause annealing-induced hardening. Either another element, which could be Cr as revealed by atom probe tomography, is able to segregate at planar defects and induce annealing-induced hardening, or different mechanisms produce a similar strengthening effect. Based on these results, we discuss different models that can be used to quantify annealing-induced hardening in CrCoNi-based MEAs.

The high-temperature corrosion behaviors of the equimolar CrCoNi medium-entropy alloy and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H 2 O, 2% O 2 , 0.5% SO 2 , and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc with a mean grain size of ~ 50 μm and a homogeneous chemical composition. The oxide layer thickness of CrMnFeCoNi increased linearly with exposure time while it remained constant at ~ 1 μm for CrCoNi. A Cr 2 O 3 layer and minor amounts of (Co,Ni)Cr 2 O 4 developed on the latter while three oxide layers were detected on the former, i.e., a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr) 3 O 4 layer in the center and a thick and porous layer of Mn 3 O 4 and MnSO 4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations.

In the binary Fe-rich Fe-Ni system, martensite start temperatures MS decrease from 500 to 200 K when Ni concentrations increase from 20 to 30 at.%. It is well known that alloys with Ni concentrations below 28.5 at.% exhibit lath martensite (LM) microstructures (athermal transformation, small crystals, accommodation by dislocations). Above this concentration, plate martensite (PM) forms (burst-like transformation, large crystals, accommodation by twins). The present work is based on a combination of (i) ingot metallurgy for the manufacturing of Fe-Ni alloys with varying Ni-concentrations, (ii) thermal analysis to measure phase transformation temperatures with a special focus on MS, and (iii) analytical orientation imaging scanning electron microscopy for a quantitative description of microstructures and crystallographic features. For Ni-concentrations close to 28.5 at.%, the descending MS-curve shows a local maximum, which has been overlooked in prior works. Beyond the local maximum, MS temperatures decrease again and follow the overall trend. The local maximum is associated with the formation of transition martensite (TM) microstructure, which exhibits LM and PM features. TM forms at higher MS temperatures, as it is accommodated by simultaneous twinning and dislocation slip. An adopted version of the Clausius-Clapeyron equation explains the correlation between simultaneous accommodation and increased transformation temperatures.

Multi-principal element alloys (MPEAs) of low stacking fault energies (SFEs) often exhibit outstanding damage tolerance. In contrast to the well-understood monotonic deformation behaviors, fatigue deformation mechanisms of the low-SFE MPEAs remain fundamental questions. Using TEM, this work demonstrated two main dislocation configurations cooperating in an exemplary low-SFE CoCrNi MPEA, namely slip bands and veins/walls/cells, which are usually formed in materials with low- and high-SFEs, respectively. Under low strain amplitude of 0.3%, the deformation features are found to include primary and double slip bands (dominating in & AP;71% and 29% grains, respectively). Upon increasing strain amplitude, apart from the slip bands, dislocation substructures formed (i.e., veins/walls/cells present in & AP;33% and 60% grains under strain amplitude of 0.5% and 0.7%, respectively) due to cross slip, despite the alloy's low-SFE. Moreover, the slip bands and walls/cells are found to serve more likely as geometrically necessary dislocations and statistically stored dislocations, respectively. Besides, the constraints from neighboring grains and Copley-Kear effect (rather than grain orientation) were suggested to play more important role in determining these dislocation patterns formation. Lastly, this work evidenced unexpected partial dislocations and stacking faults (in addition to usually observed screw dislocations) shuttling between the walls/cells by planar slip. This predominant planar slip behavior explains well the exceptional damage tolerance of low-SFE MPEAs. These insights can also advance the understanding of fatigue deformation of conventional alloys with low-SFEs.

The superior properties of high-entropy multi-functional materials are strongly connected with their atomic heterogeneity through many different local atomic interactions. The detailed element-specific studies on a local scale can provide insight into the primary arrangements of atoms in multicomponent systems and benefit to unravel the role of individual components in certain macroscopic properties of complex compounds. Herein, multi-edge X-ray absorption spectroscopy combined with reverse Monte Carlo simulations was used to explore a homogeneity of the local crystallographic ordering and specific structure relaxations of each constituent in the equiatomic single-phase face-centered cubic CrMnFeCoNi high-entropy alloy at room temperature. Within the considered fitting approach, all five elements of the alloy were found to be distributed at the nodes of the fcc lattice without any signatures of the additional phases at the atomic scale and exhibit very close statistically averaged interatomic distances (2.54 - 2.55 A) with their nearest-neighbors. Enlarged structural displacements were found solely for Cr atoms. The macroscopic magnetic properties probed by conventional magnetometry demonstrate no opening of the hysteresis loops at 5 K and illustrate a complex character of the long-range magnetic order after field assisted cooling in +/- 5 T. The observed magnetic behavior is assigned to effects related to structural relaxations of Cr. Besides, the advantages and limitations of the reverse Monte Carlo approach to studies of multicomponent systems like high-entropy alloys are highlighted. (c) 2022 Elsevier B.V.

We report the cyclic deformation behavior of CoCrNi at 550 degrees C under a strain amplitude of +/- 0.5% and compare it to that of CoCrFeMnNi. CoCrNi manifests cyclic hardening followed by minor softening and a near-steady state until failure. Transmission electron microscopy investigations of CoCrNi revealed that increasing the number of cycles from 10 to 2500/5000 leads to a transition of dislocation arrangements from slip bands to tangles. Compared to CoCrFeMnNi, CoCrNi exhibits higher strength, longer lifetime and persistent serrated flow. Owing to its lower stacking fault energy (even at 550 degrees C), planar slip is more pronounced in CoCrNi than CoCrFeMnNi, which additionally shows wavy slip.

High- and medium-entropy alloys (HEAs) are a quite new class of materials. They have a high potential for applications from low to high temperatures due to the excellent combination of their structural properties. Concerning their application as components; processing properties, such as machinability, have hardly been investigated so far. Hence, machinability analyses with a focus on the influence of the milling process and its basic parameters (cutting speed, feed per cutting edge) on the resulting surface integrity of specimens from an equiatomic high- (CoCrFeMnNi) and a medium- (CoCrNi) entropy alloy have been carried out. A highly innovative milling process with ultrasonic assistance (USAM) was compared to conventional milling processes. Recent studies have shown that USAM has a high potential to significantly reduce the mechanical load on the tool and workpiece surface during milling. In this study, the basic machining and ultrasonic parameters were systematically varied. After machining, the surface integrity of the alloys was analyzed in terms of topography, defects, subsurface damage, and residual stresses. It was observed that USAM reduces the cutting forces and increases the surface integrity in terms of lower tensile residual stresses and defect density near the surfaces for the CoCrFeMnNi alloy. It was shown that the cutting forces and the metallurgical influence in the sub surface region are reduced by increasing the cutting speed and reducing the feed rate per cutting edge. With the CoCrNi alloy, the tool revealed severe wear. As a result, for this alloy no influence of the parameters on the machinability could be determined.

In the present work, we use an advanced EBSD method to analyze the two prominent types of martensite microstructures that are found in the binary Fe-Ni system, lath martensite (27.5 at.% Ni) and plate martensite (29.5 at.% Ni). We modify, document, and apply an analytical EBSD procedure, which was originally proposed by Yardley and Payton, 2014. It analyzes the distributions of the three KSI-angles (ξ1, ξ2, and ξ3, KSI after Kurdjumov and Sachs), which describe small angular deviations between crystal planes in the unit cells of martensite and austenite—which are related through specific orientation relationships. The analysis of the angular distributions can be exploited to obtain high-resolution, color-coded micrographs of martensitic microstructures, which, for example, visualize the difference between lath and plate martensite and appreciate the microstructural features, like midribs in large plate martensite crystals. The differences between the two types of martensite also manifest themselves in different distributions of the KSI-angles (wider for lath and narrower for plate martensite). Finally, our experimental results prove that local distortions result in scatter, which is larger than the differences between the orientation relationships of Kurdjumov/Sachs, Nishiyama/Wassermann, and Greninger/Troiano.

We report on the low-cycle fatigue behavior of single-phase, face-centered cubic CoCrNi and CoCrFeMnNi at room temperature. Both alloys manifest cyclic hardening followed by softening and a near steady state until failure. CoCrNi exhibits higher strength, lower inelastic-strain, and longer lifetime than CoCrFeMnNi. For both alloys, microstructural investigations reveal no noticeable changes of texture, grain size and twin fraction. Nevertheless, CoCrNi exhibits planar dislocation structures, while CoCrFeMnNi shows well-defined wavy dislocation structures. This is due to CoCrNi lower stacking fault energy, which enhances planar slip and delays deformation localization leading to its superior fatigue resistance, compared to CoCrFeMnNi.

High-entropy alloys (HEAs) and compositionally complex alloys (CCAs) represent new classes of materials containing five or more alloying elements (concentration of each element ranging from 5 to 35 at. %). In the present study, HEAs are defined as single-phase solid solutions; CCAs contain at least two phases. The alloy concept of HEAs/CCAs is fundamentally different from most conventional alloys and promises interesting properties for industrial applications (e.g., to overcome the strength-ductility trade-off). To date, little attention has been paid to the weldability of HEAs/CCAs encompassing effects on the welding metallurgy. It remains open whether welding of HEAs/CCAs may lead to the formation of brittle intermetallics and promote elemental segregation at crystalline defects. The effect on the weld joint properties (strength, corrosion resistance) must be investigated. The weld metal and heat-affected zone in conventional alloys are characterized by non-equilibrium microstructural evolutions that most probably occur in HEAs/CCAs. The corresponding weldability has not yet been studied in detail in the literature, and the existing information is not documented in a comprehensive way. Therefore, this study summarizes the most important results on the welding of HEAs/CCAs and their weld joint properties, classified by HEA/CCA type (focused on CoCrFeMnNi and Al x CoCrCu y FeNi system) and welding process.

An equiatomic CrFeNi medium-entropy alloy (MEA) that constitutes a cornerstone of austenitic stainless steels and Fe-based superalloys is investigated. Anneals at various temperatures revealed that CrFeNi forms a stable face-centered cubic (FCC) solid solution above similar to 1223 K. Based on this result, this alloy was cold-worked and recrystallized between 1273 K and 1473 K to produce different grain sizes. Compression tests were carried out at 293 K to investigate grain boundary strengthening (Hall-Petch slope: 966 MPa mu m(1/2)) and this contribution was then subtracted from the overall strength to reveal the intrinsic uniaxial lattice strength (80 MPa). Additional compression and tensile tests were performed between 77 K and 873 K to study the effect of temperature on mechanical properties and deformation mechanisms. Ductility, yield and ultimate tensile strengths increased with decreasing temperature. To reveal the active deformation mechanisms in CrFeNi with the coarsest grain size (160 mu m), tensile tests at 77 K and 293 K were interrupted at different strains followed by transmission electron microscopy analyses. In all cases, the deformation was accommodated by dislocation glide at low strains, while twinning additionally occurred above a critical resolved shear stress of 165 MPa, which was roughly temperature independent. This value compares well with predictions (180 MPa) based on the Kibey's model for twin nucleation. Moreover, the fact that this value is roughly temperature-independent is also consistent with the Kibey's model since the twin nucleation barrier (unstable twin stacking fault energy) of FCC metals and alloys does not vary significantly with temperature. (c) 2020 Acta Materialia Inc. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)

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.

In the present work, interactions of nanoindentation-induced dislocations (NIDs) with a low-angle grain boundary (LAGB) are investigated in a single-crystalline CrCoNi medium-entropy alloy (MEA). Microstructural evolutions before and after nanoindentation were examined using accurate electron channeling contrast imaging (A-ECCI). In the as-grown state, the alloy microstructure consists of subgrains separated by LAGBs. After nanoindentation on the (001) plane far away from LAGBs, the load-displacement curves exhibit the typical behavior of metals and alloys with a pop-in marking the elastic-plastic transition. This pop-in is related to the nucleation of NIDs that are observed to form pile-ups on {111} planes. In contrast, when indents are performed in the vicinity of a LAGB with a low misorientation angle of 0.24 degrees and consisting of dislocations spaced similar to 60 nm apart, different micromechanical responses and deformation mechanisms are observed depending on the distance between the LAGB and the nanoindenter tip. When the distance between the LAGB and the nanoindenter tip is larger than four times the size of the indent (corresponding ratio: R > 4), the LAGB does not affect the micromechanical response nor interact with NIDs. In contrast, when the indenter comes in direct or indirect contact with the LAGB (R < 1), the load-displacement curve deviates at low loads from the elastic stage, and popins are not observed. In this case, the continuous deformation is accommodated by the movement of the preexisting LAGB dislocations. For intermediate cases with 1 < R < 4, the load of the initial pop-in is dependent on the local defect density. In this latter case, the pile-ups of NIDs directly impinge on the LAGB. Microstructural analyses reveal that the LAGB accommodates plasticity by blocking the NIDs, activating a dislocation nucleation site in the adjacent subgrain/emission of dislocation from the LAGB, and inducing slight motions of its constituent dislocations.

This work investigates interactions of nanoindentation-induced dislocations (NIDs) with a low-angle grain boundary (LAGB) in a single-crystalline CrCoNi medium entropy alloy. Microstructures before and after µN-nanoindentation were examined using accurate electron channeling contrast imaging. Initially, the microstructure consists of subgrains separated by LAGBs with an average size of 100 µm. After nanoindentation on the (001) plane in the vicinity of a LAGB with a misorientation angle of 0.24° and consisting of dislocations spaced ~60 nm apart, NIDs formed pile-ups on {111} planes. Microstructural analyses for indents near the LAGB reveal that the LAGB accommodates plasticity by blocking the NIDs, activating a dislocation nucleation site in the adjacent subgrain/emission of dislocation from the LAGB, and inducing slight motions of its constituent dislocations. For indents between 0-420 nm from the LAGB, micromechanical analyses show the absence of pop-ins which implies plasticity occurs by the motion of pre-existing dislocations. For indents at >420 nm, pop-ins were observed and plasticity was initiated by homogeneous and heterogeneous nucleation of dislocations. The LAGB is, therefore, a strong obstacle to dislocation motion and we point out areas for future research using nanoindentation in combination with advanced characterization methods to study the interaction between dislocations and LAGBs.

In the present article, we present a data compilation reflecting recrystallized microstructures and the corresponding mechanical properties of an equiatomic, single-phase face-centered cubic (FCC) CrFeNi medium-entropy alloy (MEA). For the analysis, interpretation, and discussion of the data, the reader can refer to the original research article entitled “Effects of temperature on mechanical properties and deformation mechanisms of the equiatomic CrFeNi medium-entropy alloy”, see Ref. (Schneider and Laplanche, Acta Mater. 204, 2020). The data related to recrystallized microstructures comprise raw backscatter electron (BSE) micrographs (tif-files) obtained using a scanning electron microscope (SEM) for six grain sizes in the range [10–160 µm], optical micrographs of the alloy with the largest grain size (d = 327 µm), pdf-reports and tables presenting the corresponding grain-size distributions (d, accounting for grain boundaries only) and crystallite-size distributions (c, which accounts for both grain and annealing twin boundaries), the annealing twin thicknesses (t), the average number of annealing twin boundaries per grain (n), and the average Taylor factor (M) of each recrystallized microstructure. These are benchmark datasets that may serve to develop new algorithms for the automated evaluation of microstructural parameters. Such algorithms would help to speed up the analyses of microstructures and improve their reliability. Furthermore, several groups pointed out that in addition to the mean grain size, other microstructural parameters such as the grain size distribution (Raeisinia et al., Model. Simul. Mater. Sc. 16, 2008) and the average number of twins per grain (Schneider et al., Int. J. Plasticity, 124, 2020) may affect some material properties (e.g. Hall-Petch strengthening). Therefore, an effort was made here to determine and report almost all the microstructural parameters describing recrystallized microstructures of FCC alloys. The mechanical-properties data are provided as excel-sheets in which the raw stress-strain curves can be found. Compression tests for alloys with different grain sizes were performed at room temperature. Additional compression tests and tensile tests for the grain size d = 160 µm were performed at temperatures between 77 K and 873 K. Characteristic mechanical properties, such as yield stresses at 0.2% plastic strain (σ0.2%) and Hall-Petch parameters (σ0 and ky) are given for all temperatures in the tables below. Moreover, the Hall-Petch parameters as well as the mechanical data reported in the present study could be used for data mining and implemented in programs used for alloy design.

The Cr-Co-Ni system was studied by combining experimental and computational methods to investigate phase stability and mechanical properties. Thin-film materials libraries were prepared and quenched from high temperatures up to 700 degrees C using a novel quenching technique. It could be shown that a wide Al solid solution region exists in the Cr-Co-Ni system. To validate the results obtained using thin-film materials libraries, bulk samples of selected compositions were prepared by arc melting, and the experimental data were additionally compared to results from DFT calculations. The computational results are in good agreement with the measured lattice parameters and elastic moduli. The lattice parameters increase with the addition of Co and Cr, with a more pronounced effect for the latter. The addition of similar to 20 atom % Cr results in a similar hardening effect to that of the addition of similar to 40 atom % Co.

CrCoNi exhibits the best combination of strength and ductility among all the equiatomic single-phase FCC subsets of the CrMnFeCoNi high-entropy alloy. Here, its yield strength was determined in compression as a function of grain size and temperature. Yield strength was also plotted as a function of "crystallite" size, which takes into account both annealing twin boundaries and grain boundaries. The resulting Hall-Petch slopes were straight lines but with different slopes that depend on the number of twin boundaries per grain. Scanning transmission electron microscopy of deformed specimens revealed the formation of dislocation pile-ups at grain and annealing twin boundaries indicating that the latter also act as obstacles to slip and contribute to strength. Using a simple pile-up model, the strengths of the grain and twin boundaries were estimated to lie in the range 900-1250 MPa. Assuming that they have the same strength, in the case of twin boundaries this strength corresponds roughly to the stress required to constrict Shockley partials, which suggests that dissociated dislocations have to become compact before they can cross the annealing twin boundaries.