Search Results (61)

The (AlFeCoNi)C high-entropy alloy carbide films (HECFs) with tunable carbon contents were fabricated by magnetron sputtering to investigate the carbon-driven structural evolution and its coupling effects on mechanical and chemical properties. With increasing carbon incorporation (0–47.6 at.%), the HECFs formed a composite structure of amorphous phase and BCC nanocrystalline phase, as evidenced by XRD and TEM. Atom probe tomography (APT) reveals Al segregation in the film. Remarkably, the wear rate decreases exponentially from 4.8 × 10⁻⁵ to 6.7 × 10⁻⁶ mm³/N·m, attributed to the amorphous carbon phase acting as solid lubricant. Simultaneously, the corrosion current density reduces by two orders of magnitude (7.2 × 10⁻⁸ A/cm² in 3.5% NaCl), benefiting from the amorphous network inhibiting ion diffusion pathways. This work establishes a carbon-content–property correlation paradigm for designing multifunctional HEA films in extreme environments. Full article

This study presents the design and microstructural investigation of a single-crystal (SX) Re-bearing high-entropy superalloy (HESA-X1) featuring a thermally stable γ–γ′–γ hierarchical microstructure. The alloy exhibits FCC γ nanoparticles embedded within L1₂-ordered γ′ precipitates, themselves distributed in a γ matrix, with the suppression of detrimental topologically close-packed (TCP) phases. To elucidate solidification behavior and phase stability, Scheil–Gulliver and TC-PRISMA simulations were conducted alongside SEM and XRD analyses. Near-atomic scale analysis in 3D using Atom Probe Tomography (APT) revealed pronounced elemental partitioning, with Re strongly segregating to the γ matrix, while Al and Ti were preferentially enriched in the γ′ phase. Notably, Re demonstrated a unique partitioning behavior compared to conventional superalloys, facilitating the formation and stabilization of γ nanoparticles during two-step aging (Ag-2). These γ nanoparticles significantly contribute to improved mechanical properties. Long-term aging (up to 200 h) at 750–850 °C confirmed exceptional phase stability, with minimal coarsening of γ′ and retention of γ nanoparticles. The coarsening rate constant K of γ′ at 750 °C was significantly lower than that of Re-free HESA, confirming the diffusion-suppressing effect of Re. These findings highlight critical roles of Re in enhancing microstructural stability by reducing atomic mobility, enabling the development of next-generation HESAs with superior thermal and mechanical properties for high-temperature applications. Full article

A novel ultrahigh-strength steel with Co and strengthened through nanoscale precipitation was developed. We found that the Co element had a synergistic effect on the precipitation process. The simulation results indicate that adding Co to steel can suppress the tracer diffusion coefficients of all the elements in the steel, hindering the atomic self-diffusion rate and long-range diffusion effect. A decrease in the atomic diffusion rate of precipitations will affect the nucleation, distribution, and growth of precipitations. The Atom probe tomography (APT) results indicate that the Co element not only dispersed uniformly in the matrix itself but also induced the uniform distribution of the precipitation phases. During the nucleation process of the precipitation, the rejected Co atoms formed small regions of high Co concentrations around the precipitation, inhibiting the coarsening of the precipitation. Under the synergistic effect of Co, the high number density of nanoscale NiAl and M₂C enhanced the strength of the steel. Full article

Severe plastic deformation and subsequent heat treatments yield nanostructured commercially pure (CP) titanium Grade 4 with average grain size of about 100 nm and exceptional strength. To elucidate the underlying strengthening mechanisms in this nanotitanium (nanoTi), this study uses atom probe tomography (APT) to analyze the atomic structure of grain boundaries and assess impurity segregation. Results reveal the formation of grain boundary segregations, primarily composed of iron (Fe) atoms, reaching concentrations up to 3.3 ± 0.2 at% in localized regions. The average width of these segregation layers is 6.13 ± 0.45 nm. The paper considers a mechanism for forming these segregations and discusses relevant theoretical models describing their contribution to the material’s enhanced strength. Full article

The high-temperature performance of 10CrNi2Mo3Cu2V steel is critically governed by the distribution of Cu-rich phases. This study systematically investigated the evolution of solute redistribution, Cu-rich phase precipitation, microstructural transformations, and mechanical properties in 10CrNi2Mo3Cu2V alloy under varying aging temperatures. Advanced characterization techniques, including atom probe tomography (APT) and transmission electron microscopy (TEM), were employed to analyze microstructural features and phase formation in both as-built and heat-treated specimens. The key findings reveal that copper atom segregation initiates at a tempering temperature of 350 °C. Upon increasing the temperature to 450 °C, extensive precipitation of nanoscale copper clusters is observed. Temperatures exceeding 450 °C trigger the formation of ε-Cu phases, which undergo subsequent coarsening. Notably, these copper clusters and Cu-rich precipitates act as dislocation pinning sites, promoting crack nucleation and propagation, thereby markedly degrading the alloy’s impact energy absorption capacity. The critical diameter for Orowan mechanism-governed strengthening by Cu-rich phases is determined to be ~6 nm, while the average diameter of matrix-penetrating Cu-rich particles is approximately 1.46 nm. Quantitative analysis demonstrated that the combined contributions of the Orowan bypass mechanism and particle-cutting mechanism yield a strength enhancement of ~219 MPa, which exhibits excellent agreement with experimentally measured strength increments. These results provide critical insights into the interplay between microstructural evolution and mechanical degradation in precipitation-strengthened steels under thermal exposure. Full article

Liquid metal embrittlement (LME) in Zn-coated advanced high-strength steels (AHSSs) is an increasing concern, particularly in automotive assembly, where it can cause early failure and reduce ductility during resistance spot welding (RSW). This study explores the impact of adding 0.2 wt% Mo on the LME susceptibility of 0.2C-2Mn-1.5Si AHSS through hot tensile testing, RSW, and advanced microstructural analyses, including atom probe tomography (APT) and transmission electron microscopy (TEM). The results suggest that Mo enhances resistance to LME, as evidenced by the increased tensile stroke from 2 mm in the case of the 0 Mo alloy and to 2.75 mm in the case of the 0.2 Mo sample. Also, the average crack length in the shoulder of the welded samples decreased from 109 ± 7 μm to 28 ± 3 μm by adding 0.2 wt% Mo to the base alloy. APT analysis revealed that, in the presence of Mo, there is increased boron (B) segregation at austenite grain boundaries, improving cohesion, while TEM suggested more diffusion of Zn into the substrate, facilitating the formation of Zn-ferrite. These findings highlight Mo’s potential to reduce LME susceptibility of AHSS for automotive applications. Full article

Ultra-low-carbon, high-strength steels have gained significant attention due to their exceptional mechanical properties. To enhance the performance of the steel, understanding the precipitation behavior of strengthening precipitates is crucial. In this study, the precipitation behavior of ultra-low-carbon high-strength steel strengthened by nanoscale copper (Cu)-rich precipitates (CRPs) and carbonitride (CN) atomic clusters was characterized using atom-probe tomography after tempering at 400, 450, 600, and 650 °C for 2 h. The results revealed that the nanoscale copper CRPs and the CN atomic clusters were the main strengthening precipitates. The CRPs, enriched only in Cu, were observed at 400 °C. Segregation of nickel (Ni) and manganese (Mn) to the CRPs occurred at 450 °C, and the number densities of CRPs achieved the maximum value, leading to the highest strengthening effects. The size of the CRPs increased with increasing temperature; however, the size of the clusters of the carbide-forming atoms remained at almost ~1.6 nm. At 650 °C, the concentration of Cu, Ni, and Mn atoms in the CRPs was about 85.4, 4.5, and 4 at.%, respectively; however, that of Fe decreased significantly. In the lath boundaries, the size of 10% C and 0.4% C iso-surfaces was relatively larger than that in the matrix. In a reverted austenite region at 600 °C, the concentration of Ni in the reverted austenite, CRPs, and matrix was about 15, 2.5, and 2.5 at.%, respectively. Full article

Nanoparticles are essential for energy storage, catalysis, and medical applications, emphasizing their accurate chemical characterization. However, atom probe tomography (APT) of nanoparticles sandwiched at the interface between an encapsulating film and a substrate poses difficulties. Poor adhesion at the film-substrate interface can cause specimen fracture during APT, while impurities may introduce additional peaks in the mass spectra. We demonstrate preparing APT specimens with strong adhesion between nanoparticles and film/substrate matrices for successful analysis. Copper nanoparticles were encapsulated at the interface between nickel film and cobalt substrate using electrodeposition. Cobalt and nickel were chosen to match their evaporation fields with copper, minimizing peak overlaps and aiding nanoparticle localization. Copper nanoparticles were deposited via magnetron sputter inert gas condensation with varying deposition times to yield suitable surface coverages, followed by encapsulation with the nickel film. In-plane and cross-plane APT specimens were prepared by femtosecond laser ablation and focused ion beam milling. Longer deposition times resulted in agglomerated nanoparticles as well as pores and voids, causing poor adhesion and specimen failure. In contrast, shorter deposition times provided sufficient surface coverage, ensuring strong adhesion and reducing void formation. This study emphasizes controlled surface coverage for reliable APT analysis, offering insights into nanoparticle chemistry. Full article

Nanostructured ferritic alloys (NFAs), such as oxide-dispersion strengthened (ODS) alloys, play a vital role in advanced fission and fusion reactors, offering superior properties when incorporating nanoparticles under irradiation. Despite their importance, the high cost of mass-producing NFAs through mechanical milling presents a challenge. This study delves into the microstructure-mechanical property correlations of three NFAs produced using a novel, cost-effective approach combining severe plastic deformation (SPD) with the continuous thermomechanical processing (CTMP) method. Analysis using scanning electron microscopy (SEM)-electron backscatter diffraction (EBSD) revealed nano-grain structures and phases, while scanning transmission electron microscopy (STEM)-energy dispersive X-ray spectroscopy (EDS) quantified the size and density of Ti-N, Y-O, and Cr-O fine particles. Atom probe tomography (APT) further confirmed the absence of finer Y-O particles and characterized the chemical composition of the particles, suggesting possible nitride dispersion strengthening. Correlation of microstructure and mechanical testing results revealed that CTMP alloys, despite having lower nanoparticle densities, exhibit strength and ductility comparable to mechanically milled ODS alloys, likely due to their fine grain structure. However, higher nanoparticle densities may be necessary to prevent cavity swelling under high-temperature irradiation and helium gas production. Further enhancements in uniform nanoparticle distribution and increased sink strength are recommended to mitigate cavity swelling, advancing their suitability for nuclear applications. Full article

The reactor pressure vessel (RPV) is a critical barrier in nuclear power plants, but its embrittlement during service poses a significant safety challenge. This study investigated the effects of Cu-enriched clusters on the mechanical and magnetic properties of Fe-0.9 wt.%Cu model alloys through thermal aging. Using Vickers hardness tests, Magnetic Barkhausen Noise (MBN) detection, and Atom Probe Tomography (APT), the study aimed to establish a quantitative correlation between MBN signals, Vickers hardness, and Cu-enriched clusters, facilitating the non-destructive testing of RPV embrittlement. Experimental results showed that the hardness and MBN parameters (RMS and V_pp values) changed significantly with aging time. The hardness increased rapidly in the early stage (under-aged), followed by a plateau and then a decreasing trend (over-aged). In contrast, MBN parameters decreased initially and then increased. APT analysis revealed that Cu-enriched clusters increase in size to 4.60 nm and coalesced during aging, with their number density peaking to 3.76 × 10²³ m⁻³ before declining. An inverse linear correlation was found between MBN signals and the combined factor N_d²R_g (product of the number density squared and the mean radius of Cu-enriched clusters). This correlation was consistent across both under-aged and over-aged states, suggesting that MBN signals can serve as applicable indicators for the non-destructive evaluation of RPV steel embrittlement. Full article

Copper alloys containing chromium and hafnium combine elevated mechanical strength and high electrical and thermal conductivity. For the simultaneous enhancement of both material properties, precipitation hardening is the utilized mechanism. Therefore, the aim is to analyze the influence of chromium and hafnium in binary and ternary low-alloyed copper alloys and to compare the precipitation processes during temperature exposure. Atom probe tomography (APT) and differential scanning calorimetry (DSC) measurements enable to understand the precipitation sequence in detail. CuCr0.7 starts to precipitate directly, whereas CuHf0.7 is highly influenced by prior diffusion facilitating cold rolling. Within the ternary alloy, hafnium atoms accumulate at the shell of mainly Cr-containing precipitates. Increasing the local hafnium concentration results in the formation of intermetallic CuHf precipitates at the sites of mainly Cr-containing precipitates. Indirect methods are utilized to investigate the materials’ properties and show the impact of cold rolling prior to an aging treatment on binary alloys CuCr and CuHf. Finally, ternary alloys combine the benefits of facilitated precipitation processes and decelerated growing and coarsening, which classifies the alloys to be applicable for usage at elevated temperatures. Full article

In this work, the nanostructure of oxide dispersion-strengthened steels was studied by small-angle neutron scattering (SANS), transmission electron microscopy (TEM), and atom probe tomography (APT). The steels under study have different alloying systems differing in their contents of Cr, V, Ti, Al, and Zr. The methods of local analysis of TEM and APT revealed a significant number of nanosized oxide particles and clusters. Their sizes, number densities, and compositions were determined. A calculation of hardness from SANS data collected without an external magnetic field, or under a 1.1 T field, showed good agreement with the microhardness of the materials. The importance of taking into account two types of inclusions (oxides and clusters) and both nuclear and magnetic scattering was shown by the analysis of the scattering data. Full article

In order to increase the strength of Al-Zr alloys, which are promisingly used for heat-resistant conductors, the coupling effect of Mn addition (0.16 wt.% and 0.88 wt.%) and deformation on the precipitation, mechanical, and electrical properties of an Al-0.18wt.% Zr alloy was studied using transmission electron microscopy (TEM), atom probe tomography (APT), hardness testing, and electrical conductivity measurement, respectively. Results showed that the Mn addition fully suppresses the Al₃Zr precipitation in both hot-deformed and undeformed cases, which is mainly due to a strong Mn-vacancy bonding, in which Mn atoms seize vacancies and hence reduce the available vacancies for Al₃Zr nucleation. Minor 0.16 wt.% Mn addition causes a simultaneous decrease in hardness and electrical conductivity, regardless of whether there is deformation. The higher 0.88 wt.% Mn addition, however, significantly increases the hardness by over 40%, especially in combination with deformation. Possible influencing factors such as grain size, dislocations, intergranular/intragranular precipitation, and solute clusters are comparatively discussed in terms of microstructural features and mechanical/electrical properties that are tuned by Mn addition and/or deformation. It is found that the Mn addition can make remarkable contributions to the hardness and thermal stability of the Al-Zr alloys when coupled with deformation. Full article

Austenitic stainless steel D9 is a candidate for Generation IV nuclear reactor structural materials due to its enhanced irradiation tolerance and high-temperature creep strength compared to conventional 300-series stainless steels. But, like other austenitic steels, D9 is susceptible to irradiation-induced clustering of Ni and Si, the mechanism for which is not well understood. This study utilizes atom probe tomography (APT) to characterize the chemistry and morphology of Ni–Si nanoclusters in D9 following neutron or proton irradiation to doses ranging from 5–9 displacements per atom (dpa) and temperatures ranging from 430–683 °C. Nanoclusters form only after neutron irradiation and exhibit classical coarsening with increasing dose and temperature. The nanoclusters have Ni₃Si stoichiometry in a Ni core–Si shell structure. This core–shell structure provides insight into a potentially unique nucleation and growth mechanism—nanocluster cores may nucleate through local, spinodal-like compositional fluctuations in Ni, with subsequent growth driven by rapid Si diffusion. This study underscores how APT can shed light on an unusual irradiation-induced nanocluster nucleation mechanism active in the ubiquitous class of austenitic stainless steels. Full article

A novel procedure for the application of atom probe tomography (APT) to the structural analysis of biological systems, has been recently proposed, whereby the specimen is embedded by a silica matrix and ablated by a pulsed laser source. Such a technique, requires that the silica primer be properly inert and bio-compatible, keeping the native structural features of the system at hand, while condensing into an amorphous, glass-like coating. In this work, we propose a molecular dynamics protocol, aimed at depicting and characterizing the earliest stages of the embedding process of small biomolecules in a solution of water and orthosilicic acid, here, taken as a precursor of the silica matrix. Overall, we observe a negligible influence of orthosilicic acid on the behavior of stable folded systems (such as ubiquitin). Conversely, intrinsically disordered and unstable peptides are affected by the coating, the latter seemingly inhibiting the fluctuations of flexible moieties. While further scrutiny is in order, our assessment offers a first mechanistic insight of the effects of orthosilicic acid, thereby validating its use in the proposed innovative application of APT to the structural resolution of protein molecules. Full article