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At least 109 records · Page 6

Effects of HCP/BCC element ratios on the room-temperature tensile properties of Ti-Zr-Hf-Nb-Ta refractory high-entropy alloys

Equiatomic and non-equiatomic Ti-Zr-Hf-Nb-Ta refractory high-entropy alloys (RHEAs) were arc melted, homogenized, cold rolled, and recrystallized to produce single-phase, body-centered cubic (BCC), microstructures with weak texture and equiaxed grains 76–199 μm in size. Here, the non-equiatomic alloys had either a 60:40 or 80:20 atomic ratio of hexagonal close-packed (HCP) elements (Ti + Zr + Hf) to BCC elements (Nb + Ta). Alloy compositions were measured after thermomechanical processing to determine the concentrations of the major (substitutional) and minor (interstitial) elements. We investigated how elastic constants and uniaxial tensile properties were affected by changes in the relative concentrations of the constituent elements at fixed HCP:BCC ratios. Yield strengths ranged from 801 to 922 MPa and ultimate tensile strengths from 815 to 933 MPa. Good agreement is obtained between the experimental yield strengths and those predicted by a strength theory based on edge dislocations indicating that the observed compositional effects are due to their effects on shear modulus and volume misfit. Fracture occurred by dimpled rupture with fracture strains of 19.4%–25.7%, but uniform strains were an order of magnitude lower at 1.1%–3.2%, calling into question the useable ductility (prior to necking) of RHEAs considered to be ductile based on their fracture strain. Contrary to predictions in the literature that HCP elements promote ductility, our present results show that increasing the HCP:BCC ratio decreases both the total strain and the uniform strain. Similar trends were not evident in the yield or ultimate strengths; rather, strengths were affected mainly by shear modulus and volume misfit.

BCC high-entropy alloys↗

The Ductility of 49Fe-49Co-2V Soft Magnetic Alloy Bar: Surface Effects and Test Methods

The tensile ductility of 49Fe-49Co-2V (Hiperco® 50A) bar was investigated in both as-received and heat-treated conditions. The as-received/machined specimens exhibit very low ductility compared to samples where heat treatment was the final step prior to testing. Microstructural characterization showed that internal residual strain from bar processing and, most importantly, surface machining damage, cause lower elongation in the as-received material. Because fracture of this intermetallic alloy initiates at the surface, it is particularly susceptible to surface machining damage, i.e., the near-surface region has already exhausted most of its ability to accumulate tensile strain. During heat treatment, the internal residual strain and near-surface machining damage are eliminated and ductility is improved, despite a higher degree of crystallographic ordering in the heat-treated condition (which typically lowers ductility). Furthermore, if machining is again performed after heat treatment, the material again exhibits brittle behavior, even with only light touch-up machining passes. Here, in this work, methods of tensile strain measurement were investigated, namely conventional knife-edge extensometry and noncontact digital image correlation (DIC) on heat-treated material. For clip-on knife-edge extensometry, the range of failure strain was 2.5-5.5% for heat-treated Hiperco. For noncontact methods, ductility up to 7% was observed. The results highlight the tendency for the alloy to fail at surface imperfections, even those produced by application of the extensometer itself. Noncontact laser extensometry is recommended for determining the intrinsic ductility of the alloy. A method of laser surface modification was developed which increased ductility by ~ 100% compared to unmodified samples. The high cooling rates achieved during laser surface processing can bypass the ordering reaction and produce a ductile disordered structure at the surface that exhibits ductile fracture characteristics.

EBSD↗

Impact of annealing at 1000°C in flowing He with low O 2 concentration on the room temperature tensile properties of Mo alloys

NorthStar is developing an accelerator-based technology to produce the medical isotope Mo-99. A previous ORNL report (ORNL/SPR-2022/2490) studied the oxidation behavior of Mo in flowing He with low oxygen content at 800°C and 1000°C and it was shown that an O 2 concentration lower than ~5ppm (μ1/1) is required to achieve acceptable oxidation rates for wrought or powder metallurgy (PM) Mo. Oxidation may also impact the mechanical properties of Mo and this report summarizes tensile results at room temperature on wrought and PM Mo before and after exposure at 1000°C in flowing He with O 2 concentration varying from 1 to 15 ppm O 2 . It was found that oxidation at 1000°C results in a significant decrease of Mo strength and ductility with brittle intergranular fracture surfaces, likely due to the segregation of oxygen at grain boundaries. For the PM Mo material, the decrease in strength and ductility was also observed after annealing in vacuum at 1000°C, indicating that the diffusion of the oxygen trapped in the material pores to grain boundaries after 20-100h at 1000°C is sufficient to embrittle the material. Finally, initial results on actual aMo and high-density disks provided by NorthStar revealed the lack of ductility of the materials due to the specific disk microstructure.

36 MATERIALS SCIENCE↗

Effect of aging on failure mechanism of Alloy 709 at various temperatures

Alloy 709 is a novel austenitic stainless steel with high temperature creep strength, weldability, and corrosion resistance. These properties make the material suitable for applications in the structure of next-generation nuclear power plants. Enduring high temperatures for an extended period of time in the harsh environments of a nuclear power plant results in thermal aging of the material. Therefore, it is imperative to study the effect of thermal aging on the microstructure and mechanical properties of Alloy 709 before its application in the next generation power plants. In this study, hot-processed (forged + rolled), annealed and quenched ingots of Alloy 709 are aged at 650 °C for 2000 h in air and then tested at various temperatures up to 850 °C in an in-situ heating-loading Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectroscopy (EDS) and Electron Backscatter Diffraction (EBSD). The effect of testing temperature and aging on microstructural evolutions during tensile testing of as-received and aged samples are studied. Furthermore, both as-received and aged samples displayed serrations and drop in ductility at elevated temperatures, due to the effect of dynamic strain aging (DSA). The occurrence of DSA activity was found within temperatures range of 500 °C–750 °C in as-received and 550 °C - 650 °C in aged samples. The aged samples showed less elongation accompanied by shallower dimples on the fractured surface, indicating less ductile failure mechanism compared to as-received samples. Failure mechanism observations on the fracture surface using SEM fractography are correlated to the observations made on the sample surface using in-situ SEM to achieve a complementary set of information to better understand the failure mechanism of this novel alloy.

36 MATERIALS SCIENCE↗

Understanding the effect of friction stir processing on electrical steel: Microstructural changes and mechanical transformations

Raising Si beyond 3.5 wt% reduces core loss but embrittles electrical steels, constraining processing and application. Here we assess friction stir processing (FSP) as a solid‑state route to enable Fe–4.0 wt% Si with improved mechanical performance. Temperature‑controlled FSP with a PcBN tool produced a defect‑free processed zone. SEM/EBSD revealed dynamic recrystallization and grain refinement from an average 110 μm in the base material to ∼20 μm in the processed region, with ∼ 80% of grains < 40 μm and a reduction in high‑angle boundary fraction to ∼65% (vs >85% in the base). Comparative mechanical property analysis shows a moderate increase in yield strength in FSP samples relative to the base material, with a significant improvement in ductility (∼35–50%). Post‑fracture EBSD identified 60° twin boundaries in the base while sub-grain formation with elevated KAM in the FSP sample. Fractography revealed a shift from quasi‑cleavage in the Base-faceted planes with river patterns, steps, and occasional secondary cracks—to ductile micro void coalescence after FSP. Following FSP, the material retains soft‑magnetic behavior, with modest shifts in saturation magnetization consistent with grain refinement and stored strain, accompanied by a clear gain in formability. These results indicate that FSP provides a viable route to deploy higher‑Si electrical steels with concurrent gains in strength and ductility.

Electrical steel↗

Microstructure and fracture toughness characterization of three 9Cr ODS EUROFER steels with different thermo-mechanical treatments

Ferritic martensitic ODS steels are one of the candidate structural materials for future Gen-IV nuclear fission and fusion reactors. Here, the dependence of fracture toughness on microstructure was investigated by comparing three 9Cr ODS EUROFER steels manufactured through different thermo-mechanical processing routes. Quasi-static fracture toughness testing was performed with sub-sized C(T) specimens and microstructural characterization was carried out using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy. It was found that at lower test temperatures (-100 – 22 °C), the fracture toughness was primarily controlled by crack initiation at sub-micron particles and by production of secondary cracks during fracture. At higher temperatures (above 100 °C), fracture toughness was predominantly controlled by the matrix ductility and the grain boundary strength with a relatively ductile coarse-grained alloy demonstrating higher fracture toughness compared to high-strength fine-grained alloys. These results and discussion show that variations in thermomechanical treatments can produce significant differences in microstructure and fracture toughness behavior of ferritic martensitic ODS steels.

36 MATERIALS SCIENCE↗

Exceptional strength and wear resistance in an AA7075/TiB 2 composite fabricated via friction consolidation

The friction consolidation method successfully reinforced aluminum 7075 alloy (AA7075) with high-volume fractions (12 and 24 vol%) of titanium diboride (TiB 2 ) by high pressure and severe plastic deformation at elevated temperatures. The consolidated AMCs have a uniform dispersion of submicron- and micron-sized TiB 2 particles in the AA7075 matrix, with significant refinement of the matrix grain size and the particles. The addition of TiB 2 significantly increases hardness by up to 50 %, Young’s modulus by up to 62 %, and ultimate tensile strength by up to 28 % to 672 MPa, while reducing ductility by 80 %. Wear resistance of 7075/24 vol% TiB 2 improves seven-fold compared to baseline, making it comparable to that of carburized steels. Microstructure-based finite element modeling provided a theoretical strength limit of ~730 MPa for the composites and indicated that high triaxiality in conjunction with severe equivalent plastic strain in a narrow area between the TiB 2 particles led to early fracture initiations, limiting the ductility.

36 MATERIALS SCIENCE↗

Assessment of a Grade 91 Steel Forging and Seamless Pipe Section After 141,000-Hours of Operation in a Superheat Outlet Header

In this work, two unique heats of 9Cr creep strength enhanced ferritic (CSEF) steels extracted from a retired superheat outlet header after 141,000 hours of service were evaluated. These two CSEF steels were a forging manufactured to SA-182 F91 (F91) reducer and a seamless pipe produced to SA-335 P91 (P91) pipe. Their creep deformation and fracture behavior were assessed using a lever arm creep frame integrated with in-situ high-temperature digital image correlation (DIC) system. Critical metallurgical and microstructure factors, including composition, service damage, grain matrix degradation, precipitates, and inclusions were quantitatively characterized to link the performance of the two service aged F91 and P91 CSEF steels. The creep test results show the F91 and P91 steels exhibit a large variation in creep strength and creep ductility. The F91 steel fractured at 572 hours while P91 steel fractured at 1,901 hours when subjected to a test condition of 650 °C and 100 MPa. The nominal creep strains at fracture were 12.5% (F91) and 14.5% (P91), respectively. The high-resolution DIC strain measurements reveal the local creep strain in F91 was about 50% while the local creep strain in P91 was >80%. The characterization results show that the F91 steel possessed pre-existing creep damage from its time in service, a higher fraction of inclusions, and a faster matrix grain coarsening rate. These features contribute to the observed reduction in performance for the F91 steel. The context for these findings, and the importance of metallurgical risk in an integrated life management approach will be emphasized.

Wang, Yiyu↗

CONSTRAINT-INDEPENDENT CONSTANT CTOA DETERMINATION FOR DUCTILE STABLE CRACK GROWTH

Crack tip opening angle (CTOA) has been used as a reliable fracture toughness parameter for decades to characterize stable ductile crack growth for thin-walled aerospace structures in the low-constraint conditions. Recently, the CTOA parameter was also applied to the pipeline industry, and a CTOA test standard ASTM E3039 was thus developed for testing a critical constant CTOA. Research showed that the constant CTOA can reasonably describe fracture toughness required to arrest a dynamic crack propagation for a modern gas pipeline. However, the CTOA fracture criterion requires constraint-independent CTOA toughness against stable ductile crack growth. ASTM E3039 recommends a drop weight tearing test (DWTT) specimen for CTOA testing. Since a shallow crack is used, DWTT measured CTOA may depend on constraint level at the crack tip. To understand if it is the case, this paper evaluates the critical CTOA for a set of fracture toughness tests on single edge notched bend (SENB) specimens with shallow and deep cracks based on four CTOA estimation models. In which, the Ln(P)-LLD linear fit model is similar to that used by ASTM E3039 in the CTOA calculation. Fracture test data for X80 pipeline steel and HY80 structural steel are considered in the CTOA evaluation. The results show that the four CTOA models can determine a crack size-independent constant CTOA over stable ductile crack growth for the SENB specimens. As a result, CTOA determined by ASTM E3039 is constraint&#x2;independent and transferable to use for an actual crack propagating in a gas pipeline.

Zhu, Xian-Kui↗

Constraint-dependent CTOA determination for stable ductile crack growth

The crack tip opening angle (CTOA) has been used as a reliable fracture toughness to characterize stable crack growth for thin-wall structures in low-constraint conditions. Recently, it is found that CTOA can also be utilized as a robust fracture parameter to describe the arrest fracture toughness for gas transmission pipelines in ductile steels. For better understanding the concept of CTOA, this paper presents a brief review on the CTOA definitions and its test methods. And then, four CTOA models are developed for determining the CTOA toughness using conventional single edge notched bend (SENB) specimens, including the load–displacement linear fit model, the logarithmic load–displacement linear fit model, the stable tearing energy model, and the J-differentiation model. Here fracture test data from SENB specimens in A285 carbon steel are employed to evaluate the proposed CTOA models. The results show that these CTOA models can determine either identical or comparable critical CTOA values for stable ductile crack growth using the SENB specimens. A constraint-corrected CTOA resistance curve and a constraint-corrected critical CTOA equation are also obtained for A285 carbon steel.

42 ENGINEERING↗

Utilizing machine learning to predict tensile ductility and yield strength of CoNiV-based multi-principal elements alloys

This study explores the use of machine learning (ML) as a computational tool to accelerate the design of multi-principal element alloys (MPEAs) with improved tensile elongation. An ML model was trained using available experimental data from the literature along with theoretically derived features to predict yield strength (YS) and ductility. A subset of ML-predicted compositions—CoNiVFe, CoNiVTi, CoNiVTiFe, and CoCrNiVTi—was synthesized and evaluated through tensile testing. The ML model underpredicted YS by approximately 20–30 % and overpredicted ductility by 60–70 % for Ti-containing alloys. Microstructural analysis revealed that Ti segregation at interdendritic regions contributed to early fracture, leading to discrepancies in ductility predictions. Ti segregation at these regions likely drives the increased YS due to segregation strengthening. In contrast, the CoNiVFe alloy showed good agreement with both experimental YS and elongation, with prediction errors of ∼10.2 % and ∼20.7 %, respectively. Microstructural characterization revealed minimal segregation in this alloy, suggesting that the ML model can reliably predict the properties of alloys with little to no segregation. These findings highlight the capability of ML in predicting YS with good accuracy but underscore its limitations in capturing defect-driven failure mechanisms such as segregation-induced embrittlement.

36 MATERIALS SCIENCE↗

The effect of Ni doping on the mechanical behavior of tungsten

The effect of nickel (Ni) on activated sintering of tungsten has been known and investigated for decades. However, there are few reports on the mechanical properties of tungsten when Ni is added as a low alloying additive with less than 1 wt%. In this work, the mechanical behaviors of tungsten doped with 0.2–1.0 wt% nickel from room temperature up to 400 °C were investigated. The results show that the compression ductility of as-sintered Ni doped tungsten is drastically higher than that of as-sintered pure tungsten at all tested temperatures including room temperature, and the fracture toughness at room temperature is increased by 92%. The results suggest that the ductile-to-brittle transition temperature (DBTT) of tungsten can be reduced substantially by doping with Ni.

36 MATERIALS SCIENCE↗

ATF Cladding Mechanical Properties Report: Capability Demonstration

This report documents mechanical testing capability demonstration activities performed in fiscal year (FY)2025 at Oak Ridge National Laboratory(ORNL)on chromium-coated (Cr-coated) and uncoated advanced zirconium alloy claddings irradiated in the High Flux Isotope Reactor (HFIR) to approximately 4 displacements per atom (dpa), corresponding to ~13GWd/t burnup. Specimens were prepared in axial tension (ATT) and ring tension (RTT) geometries, and passive silicon carbide(SiC)thermometry (TM) was employed to determine irradiation temperatures, which averaged 38–43 °C below the 330 °C design target. Mechanical testing at ambient temperature demonstrated the expected irradiation-induced hardening, with yield strength(YS)and ultimate tensile strength(UTS)values increasing substantially relative to unirradiated counterparts. However, this strengthening was accompanied by a reduction in ductility, as indicated by lower uniform and total elongations(UE and TE). Both coated and uncoated claddings exhibited similar mechanical response, though Cr-coated specimens showed surface cracking perpendicular to the loading direction, attributable to the hardness mismatch between the coating and substrate. Fracture in all cases remained ductile, and no coating spallation was observed following HFIR irradiation. Complementary efforts were directed toward the fabrication of test specimens from commercially irradiated cladding (rod 47I, ~31.1 GWd/t average burnup). Axial sectioning and computer numerical control(CNC)machining successfully produced ATT geometries suitable for benchmarking against HFIR-irradiated specimens. This capability enables direct comparison of cladding behavior between test reactor and commercial reactor environments, thereby supporting the validation of HFIR as a surrogate irradiation platform for accident tolerant fuel (ATF) development. Once HFIR irradiations are completed in FY26,the relevant comparison tests will be completed. Collectively, the FY 2025 PIE campaign has provided mechanical performance data for irradiated advanced claddings The demonstrated capabilities support the framework for mechanical testing and further evaluations in subsequent years. These efforts will represent an important contribution toward the licensing and deployment of Cr-coated zirconium alloy cladding as a near-term ATF solution.

36 MATERIALS SCIENCE↗

Toughening materials: enhancing resistance to fracture

It has been said that ‘God invented plasticity, but the Devil invented fracture!’ Both mechanisms represent the two prime modes of structural failure, respectively, plastic collapse and the rupture/breaking of a component, but the concept of developing materials with enhanced resistance to fracture can be difficult. This is because fracture resistance invariably involves a compromise—between strength and ductility, between strength and toughness—fundamentally leading to a ‘conflict’ between nano-/micro-structural damage and the mechanisms of toughening. Here, we examine the two major classes of such toughening: (i) intrinsic toughening, which occurs ahead of a crack tip and is motivated by plasticity—this is the principal mode of fracture resistance in ductile materials, and (ii) extrinsic toughening, which occurs at, or in the wake of, a crack tip and is associated with crack-tip shielding—this is generally the sole mode of fracture resistance in brittle materials. We briefly examine how these distinct mechanistic processes have been used to toughen synthetic materials—intrinsically in gradient materials and in multiple principal-element metallic alloys with the example of metallic glasses and high-entropy alloys, and extrinsically in ceramics with the example of ceramic-matrix composites—in comparison to Nature which has been especially adept in creating biological/natural materials which are toughened by one or both mechanistic classes, despite often consisting of constituents with meagre mechanical properties. The success of Nature has been driven by its ability to cultivate the development of materials with multiple length-scale hierarchical structures that display ingenious gradients and structural adaptability, a philosophy which we need to emulate and more importantly learn to synthesize to make structural materials of the future with unprecedented combinations of mechanical properties.

36 MATERIALS SCIENCE↗

Fracture resistance of vintage cast iron in gaseous hydrogen

In an effort to decarbonize legacy energy systems, several projects around the world are exploring alternatives to natural gas. Gaseous hydrogen is proposed as a carbon-free fuel to displace natural gas in existing legacy natural gas distribution systems, some of which continue to operate after 100 years (or more) in service. These systems, particularly in older industrial centers, contain cast iron pipe. However, the fracture resistance of most metals is degraded in gaseous hydrogen environments. This study evaluated the fracture resistance of several legacy cast iron pipe materials while exposed to gaseous hydrogen. Measurements were performed in three environments: air, a gas mixture with hydrogen partial pressure of 1 bar and pure hydrogen with a partial pressure of 34 bar. Although cast iron is generally considered a low ductility metal, elastic-plastic fracture methods are needed to assess the fracture resistance of the relatively small specimens that can be extracted from legacy pipe. Hydrogen reduced the fracture resistance of these cast iron materials by 10-40%. In air, the fracture resistance was determined to be as high as 21 MPa m 1/2 , whereas in gaseous hydrogen at pressure of about 1 bar the fracture resistance was as low as 13 MPa m 1/2 . Additional modest degradation of the fracture resistance was assessed at higher partial pressure (as low as 12 MPa m 1/2 ).

08 HYDROGEN↗

Ultra-grain refinement creates FCC pure cobalt with high strength and high ductility

Although pure cobalt is generally known to have a hexagonal close-packed (HCP) structure at room temperature, we show that its high-temperature face-centered cubic (FCC) phase can be strongly stabilized through grain refinement, resulting in FCC pure cobalt at room temperature. Ultrafine-grained (UFG) FCC cobalt exhibits a hierarchical microstructure consisting of dense stacking fault (SF) networks in the dominant FCC grains and numerous SFs and thin FCC layers within a few HCP plates. This unique microstructure leads to a high tensile strength exceeding 1 GPa, together with a tensile elongation of over 35%, thereby surpassing the well-known strength–ductility trade-off of pure metals. In-situ synchrotron X-ray diffraction revealed that the UFG FCC cobalt exhibited a markedly enhanced deformation-induced FCC→HCP martensitic transformation, which provided sustained strain hardening through the transformation-induced plasticity (TRIP) effect. Furthermore, ultra-grain refinement dramatically suppressed premature void and crack formation, causing a transition in the fracture mode from brittle to ductile. These findings advance the fundamental understanding of the phase stability and TRIP-assisted deformation in elemental cobalt and offer new guidelines for the microstructure-driven design of high-performance cobalt-based structural alloys.

Metastability↗

Deformation and fracture characteristics of zirconium plate produced via ultrasonic additive manufacturing

Abstract The microstructural evolution, deformation modes, and fracture mechanisms of zirconium plate produced using ultrasonic additive manufacturing (UAM) are presented. In addition to conventional tensile testing techniques, digital image correlation captured highly variable strain accumulation in specimens loaded perpendicular or parallel to the build height (Z). When tested in parallel to Z, delamination at prior foil/foil interfaces creates strain localization noticeable in strain rate maps, whereas specimens loaded perpendicular to Z illustrate conventional strain hardening until necking accelerates delamination. Although bond strengths are statistically and spatially variable, in situ electron backscattering diffraction tests illustrate the ability for grains near interfaces to accommodate strain with twinning and slip modes consistent with conventionally produced zirconium alloys. Finally, mixtures of ductile and delamination-induced fracture highlight the interface-driven failure modes of UAM zirconium plate in the as-built condition. Graphic abstract

36 MATERIALS SCIENCE↗