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At least 1,009 records · Page 56

Identifying microstructures susceptible to pulverization in commercially irradiated high burnup UO2 under LOCA conditions

High burnup fuel fragmentation (HBFF) has been a concern in the nuclear industry for many years. When UO2 reaches and exceeds pellet average burnups around 55 GWd/tU, microstructural changes in the fuel pellet begin to occur that render the pellet susceptible to fine fragmentation under loss-of-coolant accident (LOCA) conditions. During a LOCA event, the cladding balloons and bursts, potentially releasing part of these fine fuel fragments into the reactor pressure vessel. This process is known as fuel fragmentation, relocation, and dispersal (FFRD). Presently, the US nuclear industry is developing a safety basis for FFRD with the goal of increasing burnups and pressurized water reactor cycle lengths. Increased cycle lengths would push the burnup limits of the fuel rods past the known threshold for HBFF susceptibility. In this work, the microstructural impact on HBFF was investigated by comparing the microstructures of as-irradiated rod segments to their post-LOCA tested counterparts. This investigation found that varied operational histories result in different microstructural evolutions across the pellet radius, which impacts the fragmentation behavior and radial location of the fragmentation. It is noted that regions with a high bubble density and a high density of grain boundaries fragment under LOCA-relevant conditions. In addition to the fragmentation that has been previously reported at the periphery of the fuel, fragmentation was also noted in the dark zone toward the fuel center. Analysis of the power histories of the fuel samples suggests that the dark zone forms in the central regions of the pellet between temperatures of approximately 740 and 960 °C.

McKinney, Casey [ORNL] (ORCID:0000000335383614)↗

Formation and mechanism of nanocrystalline AZ91 powders during HDDR processing

Grain sizes of AZ91 alloy powders were markedly refined to about 15 nm from 100 to 160 μm by an optimized hydrogenation-disproportionation-desorption-recombination (HDDR) process. The effect of temperature, hydrogen pressure and processing time on phase and microstructure evolution of AZ91 alloy powders during HDDR process was investigated systematically by X-ray diffraction, optical microscopy, scanning electron microscopy and transmission electron microscopy, respectively. The optimal HDDR process for preparing nanocrystalline Mg alloy powders is hydriding at temperature of 350 °C under 4 MPa hydrogen pressure for 12 h and dehydriding at 350 °C for 3 h in vacuum. A modified unreacted core model was introduced to describe the mechanism of grain refinement of during HDDR process. - Highlights: • Grain size of the AZ91 alloy powders was significantly refined from 100 μm to 15 nm. • The optimal HDDR technology for nano Mg alloy powders is obtained. • A modified unreacted core model of grain refinement mechanism was proposed.

36 MATERIALS SCIENCE↗

Pre-processing related recrystallization behavior in β annealing of a near-β Ti-5Al-5Mo-5V-3Cr-1Zr titanium alloy

Highlights: • Recrystallization behavior of Ti-55531 alloy in β annealing under four typical pre-processing conditions is studied. • Recrystallization nucleation mode is governed by the size and distribution of substructures. • The sequence of phase transformation and β recrystallization significantly affects recrystallized grain size. • The uniform substructures produce a higher fraction of low angle grain boundaries after full recrystallization. - Abstract: Recrystallization behavior of Ti-55531 alloy in β annealing is explored for grain refinement during primary hot working. Four typical pre-processing conditions were adopted to characterize the diverse processing routes of primary hot working: deformation and annealing in the two-phase region, deformation of globularized structure in two-phase region, deformation of lamellar structure in two-phase region and deformation in single β region. The microstructure evolution in β annealing was quantified by Optical Microscopy (OM), Electron Backscattered Diffraction (EBSD), X-ray diffraction (XRD) and quantitative metallography. The results indicate that the nucleation mode of static recrystallization is determined by the size and distribution of substructures prior to annealing which is related to pre-processing route. The uniform substructures in as-deformed globularized structure produce a higher fraction of low angle grain boundaries after full recrystallization. Fine β recrystallized structure can be obtained when β recrystallization is accompanied by α-to-β phase transformation.

36 MATERIALS SCIENCE↗

Microstructural investigation of oxide dispersion strengthened alloy 617 after creep rupture at high temperature

Highlights: • The creep related microstructural evolution of ODS-617 at 950 °C under 25 MPa was investigated. • Dispersion of nanoscale Y-Al-O particles contributed to the superior creep properties of the ODS-617. • The creep mechanism of the ODS-617 at 950 °C under 25 MPa was Coble creep. • Cracks preferentially developed around the large rod-like AlN particles, resulting in the brittle creep fracture mode. - Abstract: Oxide dispersion strengthened (ODS) alloys have been widely considered as candidate structural materials for advanced nuclear reactors because of their good high temperature properties and irradiation resistance. In this study, the creep properties of oxide dispersion strengthened Alloy 617 (ODS-617) was examined at 950 °C under 25 MPa in the air. Conventional Alloy 617 tested under the same conditions was included for comparison. The ODS-617 exhibited superior creep resistance, including a much longer rupture life of 8533 h and a steady-state creep rate of 8.9 × 10{sup −8} (1/s), which was two orders of magnitude lower than that of the conventional alloy. The lower steady-state creep rate was related to the dispersion of nano-sized Y-Al-O particles, which may impede grain boundary diffusion. It seems that cracks preferentially developed near some large rod-like AlN particles, resulting in the brittle creep fracture mode.

36 MATERIALS SCIENCE↗

Formation of omega phase induced by laser shock peening in Ti-17 alloy

Synchrotron-based high-energy X-ray diffraction and transmission electron microscopy were used to study the in-depth compressive residual strains and microstructure evolution in Ti-17 alloy subjected to two-sided laser shock peening (LSP). A noticeable difference was observed in the lattice strains and extents of peak broadening on the two sides of the sample. The compressive residual strain was smaller and the peak broadening was more pronounced on the bottom surface in comparison to the top surface. This is due to the β → ω phase transformation induced by LSP on the bottom surface. It was determined that the ω phase with fine particle morphology and incommensurate structure is located mainly in the 15 μm-thick layer under the bottom surface. The formation of the LSP-induced ω phase on the bottom surface can be attributed to the adiabatic increase in temperature due to the higher shock peak pressure on the bottom surface, and can result in the relaxation of the accumulated residual compressive strain in the original phases.

36 MATERIALS SCIENCE↗

Tracking nickel oxide reduction in solid oxide cells via ex-situ ptychographic nano-tomography

In solid oxide cell (SOC) electrodes, nickel oxide reduction is a fundamental step occurring during the initial stages of cell operation. The reduction procedure is considered to be crucial in producing the final fuel electrode microstructure. This work studies the reduction reaction occurring in a SOC fuel electrode by means of X-ray ptychographic nanotomography. The same microstructure is analyzed in its pristine state and after 1 h of reduction at 850 °C, in dry hydrogen. The microstructure evolution is discussed in terms of changes in volume fractions, surface areas, and connectivity of the different constituent materials. The pore network in the unreduced cermet is revealed to be fully isolated, implying that reduction proceeds inwards from the edges of the sample towards the center. For the given experimental conditions we report that reduction is complete after 1 h of treatment but the resulting nickel network is not yet percolated and detached from the yttria-stabilized zirconia.

25 ENERGY STORAGE↗

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↗

Tracking Dendritic Growth in Hydrogen-Based Hematite Reduction via Computer Vision

The reduction of hematite to metallic iron using hydrogen (H2) as a reducing agent presents a promising pathway for decarbonizing steel production. In this study, we employ a combination of in situ confocal scanning laser microscopy (CSLM) and advanced computer vision techniques to quantitatively analyze dendritic growth of ferrite during H2-based reduction of iron oxide at high temperatures. A workflow integrating Watershed Image Segmentation (WIS) and Lucas-Kanade Optical Flow (LKOF) is developed to extract both global and local kinetic information from time-resolved micrograph sequences. H2 reduction experiments conducted at 1400 degrees C and 1500 degrees C demonstrate a clear correlation between temperature and reduction rate, as evidenced by accuracy of fitted Johnson-Mehl-Avrami-Kolmogorov (JMAK) parameters. Optical flow analysis further elucidates the anisotropic and branched nature of dendritic growth, providing spatially resolved velocity fields that correlate well with global transformation kinetics. The proposed methodology demonstrates strong agreement with experimental measurements and literature values, offering a robust framework for automated image-based analysis to study kinetics through microstructural evolution in the reduction of iron ore, and likely other reaction-diffusion phenomena.

08 HYDROGEN↗

Cooling dynamics of two titanium alloys during laser powder bed fusion probed with in situ X-ray imaging and diffraction

Metal parts produced by laser powder bed fusion (LPBF) additive manufacturing exhibit characteristic microstructures comparable to those observed in laser welding. The primary cause of this characteristic microstructure is rapid, localized heating and cooling cycles, which result in extreme thermal gradients where material solidification is followed by fast cooling in the solid state. The final microstructure and mechanical performance are also influenced by pore formation caused by melt pool fluid dynamics. Here, we use high speed, in situ X-ray diffraction to probe the kinetics of cooling and solid-solid phase transitions after laser melting in two aerospace titanium alloys: Ti-6Al-4V, an α + β alloy; and Ti-5Al-5V-5Mo-3Cr, a near-β alloy. We complement these diffraction studies with in situ X-ray imaging to probe melt pool dynamics and pore formation. From these two complementary probes, we quantify pore formation during melting and the subsequent microstructural evolution as the material rapidly cools after solidification. These results are critical for understanding defect formation and residual stress development in different titanium alloys under LPBF conditions and can help inform process models to predict final part performance.

36 MATERIALS SCIENCE↗

Extrusion of Unhomogenized Castings of 7075 Aluminum via ShAPE

Extrusion of unhomogenized castings of 7075 aluminum (Al) alloy has been accomplished using shear assisted processing and extrusion (ShAPE). The simultaneous plastic deformation and heat generation during ShAPE rapidly fracture and dissolve interdendritic and intragranular secondary phases of Al-Zn-Mg-Cu, accomplishing homogenization in seconds rather than many hours in a furnace prior to extrusion. ShAPE thereby eliminates the energy-intensive and time-consuming homogenization step required to prepare as-cast microstructures for conventional extrusion. Concurrently, extensive grain refinement occurs due to gradient activation of dynamic recrystallization during ShAPE, which facilitates a threefold increase in extrusion speed compared to the conventional extrusion method. Evident enhancement of the mechanical properties of ShAPE+T6 samples is achieved, compared to the ASTM standard values for conventional extrusion products. The microstructural evolution pathway, involving the processes of grain refinement and secondary particle dissolution, is explained using scanning and transmission electron microscopy.

36 MATERIALS SCIENCE↗

Thermal cycling-driven microstructural changes of eutectic Al–Si phase change materials in SS304 containers revealed by multi-modal imaging

Aluminum-based Al–Si alloys are widely used as phase change materials (PCMs) in thermal energy storage (TES) systems owing to their high volumetric latent heat and superior thermal conductivity. However, their long-term reliability is limited by degradation processes that remain insufficiently understood. In this work, we employ a multimodal, correlative characterization framework to systematically resolve the degradation behavior of eutectic Al–Si PCMs in contact with SS304 containers under repeated thermal cycling. By integrating high-resolution electron microscopy, three-dimensional X-ray fluorescence (3D XRF) imaging, and differential scanning calorimetry (DSC), we directly link spatially resolved compositional and microstructural evolution to changes in thermophysical properties. The correlative analysis reveals that elemental leaching of Fe, Cr, and Ni from the stainless-steel container into the PCM drives the formation of intermetallic compounds (IMCs) both at the interface and within the bulk PCM, leading to pronounced compositional heterogeneity. These interfacial reactions and diffusion-induced transformations progressively destabilize the Al–Si eutectic, reducing the effective phase-transforming fraction. Consistent with these observations, DSC measurements show a decrease in melting temperature and latent heat of fusion with thermal cycling. These results underscore the critical influence of interfacial reactions and material compatibility on the stability, durability, and overall performance of Al–Si-based TES systems.

25 ENERGY STORAGE↗

In situ studies on heavy ion irradiation and partial oxidation induced stacking faults and nanograins in tungsten nanolaminates

Understanding the microstructural evolution of tungsten (W) under extreme irradiation environments is critical for its application as a plasma-facing material in future fusion reactors. Heavy ion irradiation study offers expedited damage accumulation and thus allows irradiation tolerance property prediction in a short period of time. In this study we explore in situ Kr ion irradiation of W nanolaminates at 800 °C and uncover a complex interplay of irradiation-induced transformations, including the emergence of stacking faults, nanograin formation, and generation of thickened grain boundaries defined as GB regions with the thickness of up to 15 nm. High-resolution transmission electron microscopy studies reveal the formation of extended planar faults and a metastable hexagonal close-packed (hcp) phase within the body-centered cubic (bcc) matrix. These structural transitions are facilitated by irradiation-induced shear. They are further stabilized by the presence of oxygen, which promotes stacking fault formation and vacancy trapping. Elevated temperatures enhance defect mobility, enabling dynamic recrystallization into ultrafine grains and the thickening of GBs due to defect absorption and impurity segregation. These findings unravel non-equilibrium phase transformation pathways in heavy ion irradiated W and highlight the critical role of impurity-mediated defect dynamics in governing its radiation tolerance properties.

Wazeer, Adil [Purdue University]↗

New large-strain FFT-based formulation and its application to model strain localization in nano-metallic laminates and other strongly anisotropic crystalline materials

This paper presents a new robust large-strain (LS) elasto-viscoplastic (EVP) formulation based on Fast Fourier Transforms (FFTs) for the prediction of the micro-mechanical response and microstructure evolution of polycrystalline and multiphase materials, with emphasis on the effect of strong crystallographic and/or morphologic anisotropy on localization of plastic deformation. In this work, the novel LS-EVPFFT formulation allows treatment of complex initial geometries and large deformations considering three grids of material points: a regular grid in the reference configuration, where FFTs can be performed; an irregular grid in the initial configuration, created by applying a stress-free displacement field to the reference regular grid; and an irregular grid in the current configuration, undergoing large strains and rotations as the material is loaded. Further numerical stability of the new formulation also required the use of a novel expression for the discrete modified Green’s operator, which reduces spurious field oscillations. After presenting and validating the new formulation by comparison with preexisting implementations and analytical solutions, LS-EVPFFT is applied to the prediction of slip and kink bands formation in polycrystalline columnar ice, and kink bands in single crystal zinc wires, showing good agreement with classic experiments. Finally, the model is used to study kink band formation during compression of Cu–Nb nano-metallic laminates (NMLs), in which accurate treatment of the complex geometry associated with the tortuosity of interfaces and large deformations become critical, showing consistency with corresponding micropillar experiments.

36 MATERIALS SCIENCE↗

Hot deformation characteristics of AZ80 magnesium alloy: Work hardening effect and processing parameter sensitivities

Isothermal compression experiment of AZ80 magnesium alloy was conducted by Gleeble thermo-mechanical simulator in order to quantitatively investigate the work hardening (WH), strain rate sensitivity (SRS) and temperature sensitivity (TS) during hot processing of magnesium alloys. The WH, SRS and TS were described by Zener-Hollomon parameter (Z) coupling of deformation parameters. The relationships between WH rate and true strain as well as true stress were derived from Kocks-Mecking dislocation model and validated by our measurement data. The slope defined through the linear relationship of WH rate and true stress was only related to the annihilation coefficient Ω. Obvious WH behavior could be exhibited at a higher Z condition. Furthermore, we have identified the correlation between the microstructural evolution including β-Mg17Al12 precipitation and the SRS and TS variations. Intensive dynamic recrystallization and homogeneous distribution of β-Mg17Al12 precipitates resulted in greater SRS coefficient at higher temperature. The deformation heat effect and β-Mg17Al12 precipitate content can be regarded as the major factors determining the TS behavior. At low Z condition, the SRS becomes stronger, in contrast to the variation of TS. The optimum hot processing window was validated based on the established SRS and TS values distribution maps for AZ80 magnesium alloy.

36 MATERIALS SCIENCE↗

A brittle fracture mechanism in thermally aged duplex stainless steels revealed by in situ high-energy X-ray diffraction

A direct relationship between the microstructural evolution and macroscopic fracture behaviors of a thermally aged (at 475 °C for 400 h) duplex stainless steel (DSS) has been established with experimental results from atom probe tomography (APT), nanoindentation and in situ synchrotron-based high-energy X-ray diffraction (HE-XRD). Furthermore, the APT experiments demonstrate that ferrite in DSS spinodally decomposes into Cr-enriched and Cr-depleted domains during thermal aging, which leads to a severe hardening effect in ferrite. The lattice strain development during deformation acquired with the in situ HE-XRD measurements confirms the cleavage fracture of α{110} and α{200} ferrite grains aligned perpendicular to loading direction. The thermally aged DSS can be readily fractured by connecting the cleavage cracks in ferrite. Conclusively, the spinodal-decomposition-induced hardening in ferrite and the premature failure of ferrite control the final brittle fracture in the aged DSS.

36 MATERIALS SCIENCE↗

Cryogenic mechanical behaviors of CrMnFeCoNi high-entropy alloy

The CrMnFeCoNi high-entropy alloy (HEA) exhibits higher yield strength, ultimate strength and ductility at lower temperature. To further clarify the effect of the testing temperature on microstructure evolution, in this study in-situ synchrotron-based high-energy X-ray diffraction tensile tests were carried out from 298 K down to 123 K. The enhanced yield strength of the alloy at cryogenic temperatures can be attributed to the greater lattice distortion prior to plastic deformation. Higher strain hardening rate leads to the simultaneously enhanced strength and ductility of the studied HEA below room temperature. Both dynamic Hall-Petch hardening (twinning) and dislocation hardening provide high work hardening capacity for this alloy during the plastic deformation at cryogenic temperatures. The increased dislocation density and nano-twins at cryogenic temperatures can be attributed to the decrease in the stacking fault energy as the deformation temperature decreases. These studies could provide an in-depth understanding for the strengthening mechanisms of the HEA in different temperature conditions and guide the exploration of HEAs with superb mechanical properties at cryogenic environments.

36 MATERIALS SCIENCE↗

In situ investigation of the deformation behaviors of Fe 20 Co 30 Cr 25 Ni 25 and Fe 20 Co 30 Cr 30 Ni 20 high entropy alloys by high-energy X-ray diffraction

In situ synchrotron-based high-energy X-ray diffraction (HE-XRD) technique was employed to investigate the mechanical behaviors and microstructural evolution of face-centered cubic (FCC) Fe 20 Co 30 Cr 25 Ni 25 and Fe 20 Co 30 Cr 30 Ni 20 high entropy alloys (HEAs) during tensile deformation. Fe 20 Co 30 Cr 30 Ni 20 HEA has a good combination of strength (ultimate tensile strength of 864 ± 35 MPa) and ductility (elongation of 0.627 ± 0.021). The HE-XRD investigation reveals that Fe 20 Co 30 Cr 30 Ni 20 HEA has the transformation-induced plasticity (TRIP) effect, which starts at a critical stress of ~555 MPa. Furthermore, transmission electron microscopy confirmed this deformation-induced new phase is hexagonal-close-packed structured ε-martensite, which follows an orientation relationship of {111} γ //(0001) ε , and (110) γ //[11 2 ¯ 0] ε with the FCC γ matrix. The observation of deformation twins in the deformed samples of the two studied HEAs proves that twinning-induced plasticity (TWIP) effect occurs in both HEAs. The combination of TRIP and TWIP effects lead to the high strength, large ductility and improved strain hardening behavior of Fe 20 Co 30 Cr 30 Ni 20 HEA.

36 MATERIALS SCIENCE↗

Transformation and twinning induced plasticity in metastable Ti-Mo alloys under high strain rate deformation

The development of metastable titanium (Ti) alloys provides an unprecedented opportunity to expand their use in plasticity and damage critical applications like protective structures. However, such applications require knowledge of quasi-static to dynamic mechanical behavior, which is currently lacking. Here we perform in-situ, ultrafast synchrotron x-ray diffraction during high strain rate (Kolsky) pressure bar testing in tension and post-mortem electron microscopy to study TRansformation Induced Plasticity (TRIP) and TWinning Induced Plasticity (TWIP) in metastable Ti-Mo alloys. Two alloys, namely Ti-12Mo and Ti-15Mo (wt.%), were selected for study having different β -phase chemical stabilities. TWIP was observed in both Ti-12Mo and Ti-15Mo by in-situ synchrotron diffraction during high strain rate testing. Post-mortem microstructural characterization also revealed the presence of TRIP in Ti-12Mo. TWIP in Ti-15Mo was found to under-perform in terms of total elongation compared to TRIP/TWIP in Ti-12Mo. Ti-12Mo exhibited an average elongation of 17% compared to only 12% for Ti-15Mo with deformation at 1000 s -1 . In conclusion, TRIP resulted in significantly finer microstructure evolution and alleviated local strain accumulations in Ti-12Mo, suggesting TRIP can be used to tune available strength/ductility combinations in metastable Ti alloys under high strain rate deformation conditions.

36 MATERIALS SCIENCE↗