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Manufacturing temperatures of severely cold-drawn hyper-eutectoid steel wires are sufficiently high to influence the mobility of dislocations and alloy elements, thereby affecting the materials’ mechanical properties. Herein, we describe the evolution of microstructure and tensile strength of the as-drawn 3.45 GPa steel wire during post-deformation annealing for 30 min at 150−450 °C. Annealing at 150 °C raised the strength to 3.77 GPa by age-hardening through activation of dislocations pinning by carbon, while further temperature rising up to 450 °C caused a severe loss of strength. It was proved that annealing at 300 and 450 °C destabilizes the lamellar microstructure, promoting the formation of carbon-deficient (Fe,Mn,Cr)3C-type cementite particles with preferentially rounded and partially faceted hetero-interfaces. Annealing at 450 °C yielded the accumulation of Mn and Cr at the ferrite/particle interfaces, and their concentrations at the interfaces were dependent on the interface structure; i.e., lower concentrations at rounded interfaces (formed through capillarity–driven coarsening of the spheroidized cementite), and higher concentrations at faceted interfaces (that are initially existing in the as-drawn state). Our proof-of-principle observations, supported by thermodynamic calculations and kinetic assessments, provide a pathway for understanding the changes in microstructural and tensile properties during manufacturing of the hyper-eutectoid steel wires.

The nanostructural hierarchy of γ and γ′ phases is characterized in Ni-8.5Al-5.4Ti (at.%) alloy, after double aging treatment at 1000 and 780 °C for 6 and 20 h. Using electron microscopy and atom probe tomography, disordered γ phase inside ordered γ′ precipitate was detected, which underwent plate-like growth during aging treatment. This unique hierarchical structure enabled the simultaneous study of direct (γ′ precipitates/γ matrix) and inverse (γ nanoparticles/γ′ precipitates) order-disorder interfaces in 6 and 20 h double-aged samples. It was found that the compositional interface width, δ, of direct interfaces decreased during aging treatment, whereas the thickness remained almost unaffected for inverse interfaces. The difference in thickening behavior is explained based on the change of the Gibbs-Thomson pressure for γ plates embedded in γ′ and cuboidal γ′ precipitates surrounded by the γ matrix. This inference suggests the possibility of prediction and control of δ(t) variations during heat treatment processes based on the current thermodynamic approach.

Laser-assisted atom probe tomography (APT) has commonly been performed to determine the composition of non-conductive oxide materials at the atomic scale. However, its field evaporation mechanism is still insufficiently understood due to the complexity of laser-matter interaction on the surface of oxide tips. To understand the physical mechanism underlying laser-assisted field evaporation in a bulk oxide LaAlO3 (LAO), we conducted an interrupted experiment that combines transmission electron microscopy with APT. This correlated technique visualized the shape evolution of LAO tips during laser-assisted APT. We demonstrated that the evaporation field strength of the tips depends on the APT experimental parameters including applied laser energy and base temperature. An increase in the laser energy led to a reduction in the field evaporation strength of the tips and the formation of apex asymmetries on the tips, thereby considerably influencing the mass resolution of the technique. Moreover, an increase in the base temperature caused a slight decrease in the evaporation strength but did not significantly affect the mass-resolving ability of APT. The results discussed in this work suggest that it is the employed laser energy that primarily affects APT's resolving capability and the field evaporation strength of oxide materials. Our interrupted technique provides fundamental insight into the field evaporation sequences of LAO oxide tips under laser illumination, which can be feasibly applied to the study of various metallic and oxide materials.

Order-disorder coherent interfaces determine the microstructure and mechanical properties of precipitation-hardened high-temperature alloys. The characteristics of these interfaces can be defined by a compositional width, δ, and structural width, δ′. The latter, which can be considered as the width of the ordered part of the interface, can play an important role in high-temperature mechanical behavior of precipitation-hardened alloys. This is due to the fact that diffusion in the ordered part of the interface is generally much slower than diffusion in the disordered phase, thus hindering the solid-state diffusion-based phenomena. Here, we investigate the order-disorder interface in a Ni-19Al (at.%) alloy as a model alloy for Ni-based superalloys using atomic-resolution scanning transmission electron microscopy and three-dimensional atom probe tomography. Then, we employ thermodynamic modeling to describe the interplay between the structural and compositional interface widths in binary Ni-Al and in ternary Ni-Al-Cr and Co-Al-W systems. We introduce the δ′/δ ratio as a critical parameter that varies significantly in different alloys. Our findings offer a general pathway to control the δ′/δ ratio of interfaces, which in turn affect the high-temperature properties of precipitation-hardened alloys.

The present study aims at unveiling the influence of trace amounts of phosphorus on the macro-scale delamination in a ferritic steel. Two different steels with trace amounts of phosphorus were examined to reveal the cause: One was made by long-time high temperature holding to maximize the phosphorus segregation, and the other one was made by short-time high temperature holding to minimize the phosphorus segregation. The atom probe results at the grain boundaries ahead of the delamination-related cracks provide a strong evidence that phosphorus-enrichment and carbon-depletion for the long-time high temperature holding induces a larger degree of delamination as compared to the short-time high temperature holding. Reasons for the different segregation tendency were discussed by correlating the isothermal holding time at high temperature and the competitive segregation between phosphorus and carbon.

A new class of materials called high-entropy alloys (HEAs) constitutes multiple principal elements in similar compositional fractions. The equiatomic Fe20Mn20Cr20Co20Ni20 (at%) HEA shows attractive mechanical properties, particularly under cryogenic conditions. Yet, it lacks sufficient yield and ultimate tensile strengths at room temperature. To strengthen these materials, various strategies have been proposed mainly by tuning the composition of the bulk material while no efforts have been made to decorate and strengthen the grain boundaries. Here, we introduce a new HEA design approach that is based on compositionally conditioning the grain boundaries instead of the bulk. We found that as little as 30 ppm of boron doping in single-phase HEAs, more specific in an equiatomic FeMnCrCoNi and in a non-equiatomic Fe40Mn40Cr10Co10 (at%), improves dramatically their mechanical properties, increasing their yield strength by more than 100% and ultimate tensile strength by ∼40% at comparable or even better ductility. Boron decorates the grain boundaries and acts twofold, through interface strengthening and grain size reduction. These effects enhance grain boundary cohesion and retard capillary driven grain coarsening, thereby qualifying boron-induced grain boundary engineering as an ideal strategy for the development of advanced HEAs.

The passive films on typical stainless steels (SS) and on a newly developed high-Cr (17 wt%)-added 18 wt%-Mn steel (HCr-HMnS) were compared by Cs-corrected scanning transmission electron microscopy and atom probe tomography. Although the passive films of all samples having similar Cr contents had the same thickness, unprecedented hexagonal wurtzite MnO inside the passive film of HCr-HMnS specimen was susceptible to corrosion cracking; this was not observed in the SS samples. This MnO caused crack formation during potentiodynamic polarization test, suggesting that reducing the harmful MnO by adding Mo and Ni facilitates the development of high-Mn base SS materials . Furthermore, higher MoO2 composition of the passive films on 316 type austenitic SS than 304 type series might would result in primarily the improved pitting resistance.

WC-Co coatings with low degree of WC decomposition were deposited from electroless Ni-plated micro- and nano-structured feedstock powders using high velocity oxygen fuel (HVOF) spraying. Dry sliding friction and wear behavior of the resultant coatings, referred to as Ni/mc-WC and Ni/nc-WC, were investigated by using sintered alumina (Al2O3) as the mating material at 700 °C. For the purpose of comparison, similar experiments were carried out on conventional micro- and nano-structured coatings, denoted as mc-WC and nc-WC. The worn scars were examined by field emission scanning electron microscopy (FESEM) equipped with energy dispersive spectroscopy (EDS). The wear resistance of Ni/mc-WC and Ni/nc-WC coatings at 700 °C was found to be 45% and 72% greater than that of mc-WC and nc-WC coatings, respectively. Moreover, Ni/mc-WC and Ni/nc-WC coatings exhibited a significantly lower friction coefficient with negligible fluctuations as compared to mc-WC and nc-WC. The microscopic analyses of mc-WC and nc-WC worn surface revealed the presence of plastically deformed and discontinuous tribofilms, made up of a mixture of MWO4/WO3 (M = Co) and Al2O3, severe cracking and delamination especially at the interface of tribofilm and the underlying surface. In contrast, examination of Ni/mc-WC and Ni/nc-WC substantiated that a large area of the coatings surface is covered by a dense and adhered MWO4-type oxide layer (M = Co, Ni), which provides a more protection against wear at elevated temperature.

In this study, we addressed the effects of Ni-plating and nanostructuring of WC-Co powders on the microstructure-property relations and WC decarburization of WC-Co composite coatings. By high velocity oxygen fuel (HVOF) spraying, the coating materials were produced from four different powders, referred to as microstructured WC-Co (mc-WC), nanostructured WC-Co (nc-WC), Ni-plated microstructured WC-Co (Ni/mc-WC) and Ni-plated nanostructured WC-Co (Ni/nc-WC). We found that the coatings, deposited from Ni-free powders, undergo a high level of decarburization, thereby yielding W 2 C phase formation in brittle amorphous W-rich Co matrix that could be preferential site for crack propagation. On the contrary, the Ni-plating treatment could reduce the amount of decarburization of the coatings, resulting in the uniform distribution of WC phase in the W-depleted Co matrix. Consequently, we revealed the underlying mechanisms responsible for WC decarburization in the coatings, and further suggested that the coating deposited from Ni-plated and nanostructured powders exhibits a superior combination of hardness and fracture toughness as compared to other coatings.

An array of amorphous tin oxide (a-SnOx) nanohelixes (NHs) was fabricated on copper foil as an electrode for Na-ion batteries via the oblique angle deposition method, a solution- and surfactant-free process. The combination of the amorphous phase SnOx with a low oxidation number and its vertically aligned NH geometry with a large surface area and high porosity, which facilitate Na-ion dynamics and accommodate the volume changes, enabled a reversible capacity of up to 915 mA h g–1 after 50 cycles, fast rate capability with 48.1% retention at 2 A g–1, and high stability, which are superior to those of crystalline nanoparticle-based electrodes.

High temperature oxidation of WC-based cermet coatings deposited from electroless Ni-coated micro- and nanostructured WC-Co powders (Ni/mc-WC and Ni/nc-WC) was studied. High velocity oxygen fuel (HVOF) spraying was employed for coating deposition, and thermo-gravimetry analysis (TGA) was carried out to examine the oxidation kinetics at 600–800 °C. For comparison, the same experiments were performed on conventional micro/nanostructured WC-Co coatings (mc-WC and nc-WC). Oxidation resistance of Ni/mc-WC and Ni/nc-WC coatings at 800 °C was improved by 88.5% and 89.3% compared to mc-WC and nc-WC coatings, respectively. Linear kinetics with activation energies of 90.4 and 78.9 kJ/mol were obtained for mc-WC and nc-WC, respectively, while oxidation kinetics of Ni/mc-WC and Ni/nc-WC coatings obeyed the parabolic law with greater activation energies of 212 and 197.5 kJ/mol.

In the present study, the effects of microstructure, chemical composition on the transformation behavior and mechanical stability of individual retained austenite (RA) with the different sizes and morphology in TRIP steels were intensively investigated. In order to characterize the property of the individual RA, various analytical techniques including atom probe tomography (APT), step-wise straining EBSD and nano-indentation were applied. The blocky type RA as we categorized have many defects and lower carbon contents (~25%) compared to film type RA. And also, step-wise straining EBSD and nano-indentation results revealed that the mechanical stability of blocky type RA was lower than that of film type RA which means blocky type RA would be easily transformed into martensite. It is considered that many defects existing in blocky type RA could work as the nucleation site of martensite transformation. In contrast, high carbon contents and hard phases enclosing film type RA would increase the resistance to shear transformation resulting in the inhibition of transformation of RA to martensite.

Manipulating structure, defects and composition of a material at the atomic scale for enhancing its physical or mechanical properties is referred to as nanostructuring. Here, by combining advanced microscopy techniques, we unveil how formation of highly regular nano-arrays of nanoparticles doubles the strength of an Fe-based alloy, doped with Ti, Mo, and V, from 500 MPa to 1 GPa, upon prolonged heat treatment. The nanoparticles form at moving heterophase interfaces during cooling from the high-temperature face-centered cubic austenite to the body-centered cubic ferrite phase. We observe MoC and TiC nanoparticles at early precipitation stages as well as core-shell nanoparticles with a Ti-C rich core and a Mo-V rich shell at later precipitation stages. The core-shell structure hampers particle coarsening, enhancing the material’s strength. Designing such highly organized metallic core-shell nanoparticle arrays provides a new pathway for developing a wide range of stable nano-architectured engineering metallic alloys with drastically enhanced properties.