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At least 1,621 records · Page 90

Biaxial deformation in high purity aluminum

The convergence of multiple characterization tools has been applied to investigate the relationship of microstructure on damage evolution in high purity aluminum. The extremely coarse grain size of the disc-shaped sample provided a quasi-two dimensional structure from which the location of surface-measured features could be inferred. In particular, the role of pre-existing defects on damage growth was accessible due to the presence of casting porosity in the aluminum. Micro tomography, electron backscatter diffraction, and digital image correlation were applied to interrogate the sample in three dimensions. Recently micro-bulge testing apparatus was used to deform the pre-characterized disc of aluminum in biaxial tension, and related analysis techniques were applied to map local strain fields. Subsequent post-mortem characterization of the failed sample was performed to correlate structure to damaged regions. We determined that strain localization and associated damage was most strongly correlated with grain boundary intersections and plastic anisotropy gradients between grains. Pre-existing voids played less of an apparent role than was perhaps initially expected. Finally, these combined techniques provide insight to the mechanism of damage initiation, propagation, and failure, along with a test bed for predictive damage models incorporating anisotropic microstructural effects.

36 MATERIALS SCIENCE↗

Development of a mechanistic thermal aging model for Grade 91

This report provides a summary on understanding and predicting the effects of long-term thermal aging on microstructure and tensile properties of G91 to corroborate the ASME Code rules in strength reduction due to elevated temperature service. The research is to support the design and long-term operation of G91 structural components in sodium-cooled fast reactors (SFRs). The report is a Level 2 deliverable in FY18 (M2NT-18AN050502061), under the Work Package NT-18AN05050206, “G91 Code Extension Testing” performed by the Argonne National Laboratory (ANL), as part of the Advanced Materials Development Program for Fast Reactors. The thermal aging study of G91 involves three types of thermally-aged specimens: (1) specimens machined from two heats of G91, G91-H1 and H30176 that have been tested for the Advanced Materials Development Programs in the past years. These specimens were aged at 550, 600, and 650°C for times up to ~64,000 h; (2) specimens fabricated from the heads of the archived crept specimens (13 in total) of six heats of G91, H5349, H30394, H30383, H10148, H30176. These specimens were aged at 427 - 538°C and for times up to 132,647 h; (3) specimens made from a tube removed from the Kingston coal-fired power plant after exposure for 155,000 h at 550°C. These three sets of specimens provide a comprehensive data set for understanding and predicting the effect of long-term thermal aging on microstructure and tensile properties of G91. Microstructural analysis of the thermally-aged G91 revealed that thermal aging causes significant microstructural changes: (1) the tempered martensite formed during tempering is unstable, and suffers significant recovery during aging, manifested by an increase in subgrain width, a decrease in subgrain length, and a decrease in subgrain aspect ratio (i.e. subgrains become more equiaxed) as the aging temperature and time increase. The subgrain recovery is facilitated by the reduction of dislocation density within subgrains; (2) M23C6 carbides in the as-received G91 are distributed along grain and subgrain boundaries and play an important role as pinning obstacles against subgrain coarsening. M23C6 carbides coarsen during aging, and the coarsening of M23C6 carbides reduces the pinning force on the boundaries; (3) MX carbonitrides in the as-received G91 are distributed uniformly within subgrains, providing the precipitation hardening effect. They coarsen with increasing aging temperature and time, but the coarsening rate is low; (3) a new phase, the Laves phase intermetallic forms during aging. The formation of the Laves phase removes the Mo solutes from the matrix, reducing the solid solution strengthening effect. The Laves phase particles grow rapidly once they are nucleated, and they precipitate primarily along boundaries. They may have a pinning effect on boundaries, but should provide little to the alloy strength. The evolution of each microstructural constituent during thermal aging can be well described by individual microstructural models. The estimated activation energy for MX coarsening was 175 kJ/mol, equivalent to the activation energy for boundary and core diffusion in a-Fe, while the estimated activation energy for subgrain coarsening was significantly lower, ~96 kJ/mol. Thermal aging of G91 results in the reduction in the yield stress and the ultimate tensile strength but has an insignificant effect on the uniform and total elongations. The reduction in tensile strength is more pronounced as the aging temperature and time increases. The in situ tensile tests with high-energy X-rays revealed that sub-boundary strengthening plays a dominant role, and the strengthening role of M23C6 particles may be accounted for by subgrian boundary hardening, and three strengthening mechanisms can be superimposed to describe the tensile strength of G91: subgrain boundary hardening, MX precipitation hardening, and Mo solid solution strengthening. A microstructure – strength model was establ

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Impact of krypton irradiation on a single crystal tungsten: Multi-modal X-ray imaging study

Understanding microstructural and strain evolutions induced by noble gas production in the nuclear fuel matrix or plasma-facing materials is crucial for designing next generation nuclear reactors, as they are responsible for volumetric swelling and catastrophic failure. In this paper we describe a multimodal approach combining synchrotron-based nanoscale X-ray imaging techniques with atomic-scale electron microscopy techniques for mapping chemical composition, morphology and lattice distortion in a single crystal W induced by Kr irradiation. We report that Kr-irradiated single crystal W undergoes surface deformation, forming Kr containing cavities. Furthermore, positive strain fields are observed in Kr-irradiated regions, which lead to compression of underlying W matrix.

36 MATERIALS SCIENCE↗

Twinning behaviors of a rolled AZ31 magnesium alloy under multidirectional loading

The microstructure and texture evolution of an AZ31 magnesium rolled sheet during quasi-static compression at strain rates of 10{sup −3} s{sup −1} has been investigated by in situ electron backscattered diffraction. The influence of the initial and pre-deformed texture on the predominant deformation mechanisms during compression has been examined. It has been found that extensive grain reorientation due to (10 − 12) tensile twinning appeared when compressed along transverse direction. Tensile twin variants were observed under this loading condition, and different variants will cause an effect to the following deformation. Several twinning modes occurred with continuative loading along rolling direction. - Highlights: •Twinning behaviors were investigated through in situ multidirectional compressive tests. •Deformation behavior was affected by the twin variants. •Four types of twinning behaviors were observed during deformation process.

36 MATERIALS SCIENCE↗

Microstructure and coercivity in alnico 9

Magnetic property enhancement of alnico, a rare-earth free permanent magnet, is highly dependent on both the initial microstructure and the evolution of the spinodal decomposition (SD) inside each grain during the heat treatment process. The size, shape and distribution of the magnetic FeCo-rich (α 1 ) phase embedded in continuous non-magnetic AlNi-rich (α 2 ) phase as well as a minor Cu-enriched phase residing in between are shown to be crucial in controlling coercivity. Phase and magnetic domain morphology in a commercial alnico 9 alloy was studied using a combination of structural characterization techniques, including scanning electron microscopy, electron backscatter diffraction, aberration-corrected scanning transmission electron microscopy and Lorentz microscopy. Our results showed that casting created structural nonuniformity and defects, such as porosity, TiS 2 precipitates and grain misorientation, are heterogeneously distributed, with the center section having the best crystallographic orientation and minimal defects. The optimal spinodal is a “mosaic structure”, composed of rod-shape α1 phase with {110} or {100} planar faceting and diameter of ~30–45nm. There is also a Cu-enriched phase residing at the corners of two < 110 > facets of the α1 phase. Furthermore, it was observed that grain boundary phase reverse magnetization direction at lower external magnetic field compared to the SD region inside the grain. Improving grain orientation uniformity, reducing detrimental grain boundary phase volume fraction, and the branching of the α 1 rods, as well as their diameter, are promising routes to improve energy product of alnico.

36 MATERIALS SCIENCE↗

Synthesis and behavior of bulk iron nitride soft magnets via high-pressure spark plasma sintering

Abstract In this study, dense bulk iron nitrides (Fe x N) were synthesized for the first time ever using spark plasma sintering (SPS) of Fe x N powders. The Fe 4 N phase of iron nitride in particular has significant potential to serve as a new soft magnetic material in both transformer and inductor cores and electrical machines. The density of SPSed Fe x N increased with SPS temperature and pressure. The microstructure of the consolidated bulk Fe x N was characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. XRD revealed a primary phase of Fe 4 N with secondary phases of Fe 3 N and metallic iron. Finite element analysis (FEA) was also applied to investigate and explain localized heating and temperature distribution during SPS. The effects of processing on interface bonding formation and phase evolution were investigated and discussed in detail to provide insight into fundamental phenomena and microstructural evolution in SPSed Fe x N. Graphic abstract

36 MATERIALS SCIENCE↗

Stimulating β -Series Precipitation in Mg–Nd Alloys Via Microalloying: A Comparison of Electron Microscopy and Small-Angle Scattering Techniques

The Mg–Nd alloy system is of particular interest in the development of high-strength, lightweight structural alloys due to the formation of strengthening metastable Mg–Nd β-series precipitates during heat treatment. The strengthening is primarily provided by a combination of the β''' and β 1 precipitation. It is therefore important to understand how the precipitation behavior can be enhanced by other common alloying elements. In this work, the effects of 0.2 wt pct Zn and Ca on β-series precipitation were studied. Small-angle/ultra-small-angle X-ray scattering (SAXS/USAXS) techniques in combination with scanning transmission electron microscopy (STEM) were used to study the evolution of precipitation microstructure. Here, it is found that the Zn additions refine the precipitates, leading to an increase in hardness with aging at 200 °C. On the other hand, the Ca additions result in an acceleration in the formation of larger β 1 precipitates and chains which provides less strengthening. The β 1 chains are surrounded by precipitate-free zones (PFZs) that further contribute to the decreases in hardness observed in the over-aged condition. This paper demonstrated that SAXS/USAXS provides a powerful tool for an in situ study of the early stages of precipitation in the Mg–Nd-based alloys.

36 MATERIALS SCIENCE↗

Rapid Assessment of the Ce-Co-Fe-Cu System for Permanent Magnetic Applications

Here, this work focuses on the rapid synthesis and characterization of quaternary Ce(CoFeCu) 5 alloy libraries to assess their potential viability as permanent magnets. Arrays of bulk specimens with controlled compositions were synthesized via laser engineered net shaping (LENS) by feeding different ratios of alloy powders into a melt pool created by a laser. Based on the assessment of the magnetic properties of the LENS printed samples, arc-melted and cast ingots were prepared with varying Fe (5–20 at.%) and Co (60–45 at.%) compositions while maintaining constant Ce (16 at.%) and Cu (19 at.%) content. The evolution of the microstructure and phases with varying chemical compositions and their dependence on magnetic properties are analyzed in as-cast and heat-treated samples. In both the LENS printed and cast samples, we find the best magnetic properties correspond to a predominantly single-phase Ce(CoFeCu) 5 microstructure in which high coercivity ( H c > 10 kOe) can be achieved without any microstructural refinement.

36 MATERIALS SCIENCE↗

Enhanced accuracy through ensembling of randomly initialized auto-regressive models for dynamical systems

Computational mechanics simulations using traditional finite element methods (FEM) require prohibitively expensive computational resources for real-time engineering applications, design optimization, and digital twin implementations. While machine learning (ML) surrogate models offer significant computational speedups, autoregressive ML models for time-dependent mechanical systems suffer from error accumulation that compromises long-term prediction reliability - a critical concern for engineering applications where accuracy over extended time horizons is essential for safety and performance assessments. Here, we propose a deep ensemble framework specifically designed to address this challenge in computational mechanics applications, where multiple ML surrogate models with random weight initializations are trained in parallel and their predictions aggregated during inference. This approach leverages statistical diversity to maximize information gain from a fixed set of training data and to mitigate error propagation, while maintaining the computational efficiency that makes ML surrogates attractive for engineering practice. We validate the framework on three representative problems spanning critical areas of computational mechanics: stress field evolution in heterogeneous microstructures under complex loading (relevant to advanced materials design and composite analysis), planetary-scale shallow water dynamics (applicable to environmental and geotechnical engineering), and Gray-Scott reaction-diffusion systems (relevant to mass transport and chemical process engineering). Across all test cases, the ensemble approach demonstrates consistent error reduction of 15-33% compared to individual models. The codes for this work are available on GitHub (https://github.com/Graham-Brady-Research-Group/AutoregressiveEnsemble_SpatioTemporal_Evolution).

autoregressive prediction↗

Tribological behaviors of nanotwinned Al alloys

Wear-induced damages cause significant materials loss each year. Al alloys are widely used by industry but usually have low wear resistance. Here, we compare the tribological behaviors of ultrafine grained Al, a nanoprecipitate hardened Al 7075 alloy and nanotwinned Al–Ni alloys using the nanoscratch. The nanotwinned Al–Ni alloys exhibit lower coefficient of friction and much greater wear resistance than the Al and Al 7075 alloys. Additionally, the enhanced wear properties of Al–Ni alloys arise from their high strength and the evolution of nanotwinned microstructures into gradient nanograins during wear. These findings on fundamental wear mechanisms in nanotwinned alloys may advance the discovery of wear-resistant metallic materials.

36 MATERIALS SCIENCE↗

Moisture transport and sorption in cement based materials containing slag or silica fume

This paper presents the moisture dependency of moisture transport and moisture fixation in mortars with OPC, slag and silica fume. Water vapor desorption isotherms were measured with gravimetric methods and the moisture dependency of moisture transport was investigated with cup-tests. The results show an ongoing evolution of water vapor desorption isotherms from eight months to four years. The evolution is more pronounced for mortars containing slag. The results also show that there is a significant difference in moisture dependency of the moisture transport properties above 70% relative humidity; some mortars exhibit a clear moisture dependency in moisture transport whereas others do not. At a relative humidity below 70%, the water to binder ratio is more decisive for moisture transport than the type of binder. These results are of value for service-life models, where they represent important input data, and for understanding the evolution of the microstructure at later ages.

36 MATERIALS SCIENCE↗

Degradation mechanism of lead-vanado-iodoapatite in NaCl solution

Degradation mechanism of lead-vanado-iodoapatite (IAPT) in NaCl solution at 90 °C was investigated through systematic characterization of surface morphology, microstructure and microchemistry evolution of the alteration layer. Nano-scale characterization indicated that IAPT crystals degraded from grain boundaries toward inner grains, forming ultrafine Cl-bearing crystallites. A coupled interface dissolution-reprecipitation replacement mechanism and the ion exchange between Cl - and I - across the degradation zone may together play roles in determining the nano-scale degradation behavior of IAPT. This work highlights the degradation through multiple reactions and elemental transport across the liquid-solid and solid-solid interfaces at length scales from sub-millimeter to nanoscale.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Response of unalloyed tungsten to mixed spectrum neutrons

Neutron irradiation in mixed spectrum reactors is an effective approach to investigate the synergistic effects of solid transmutations and atomic displacement damage in tungsten. In this article the findings and interpretations from a large-scale tungsten irradiation campaign conducted using the High Flux Isotope Reactor of Oak Ridge National Laboratory are summarized. The response of originally-unalloyed tungsten to mixed spectrum neutron irradiation is characterized by enormous hardening, degradation of modulus of toughness eventually leading to embrittlement, and decreased thermal conductivity. These property changes may be attributed primarily to production, segregation, and precipitation of rhenium and osmium and assisted by displacement damage. The stages describing the evolution of the microstructural development and property changes with the neutron dose and the accompanying accumulation of transmutation products are proposed.

36 MATERIALS SCIENCE↗

Influence of nanochannel structure on helium-vacancy cluster evolution and helium retention

In the fusion reactors, plasma facing materials (PFMs) will be bombarded by large amounts of energetic particles, including helium (He) atoms. These metal-insoluble He atoms are prone to self-trapping or are trapped by vacancies, dislocation cores or grain boundaries, aggregating to form high concentration He bubbles which leads to serious degradation of the PFMs’ properties. Studying the initial stages of He-defect interactions becomes increasingly important because it not only helps us understand the formation mechanism of He bubbles but also provides insight to help design new irradiation-resistant PFMs. As such, in this work we used the positron annihilation Doppler broadening spectroscopy (DBS) and secondary ion mass spectrometry (SIMS) to explore the evolutions of the interactions between vacancy-type defects and He and the retention of He in the nanochannel W film irradiated with 190 keV He + ions to different fluences under different temperatures. It is found that the presence of a nanochannel structure accelerates the release of He from the film even at low irradiation fluences, and the release of He is significantly enhanced at higher fluences, thus inhibiting or delaying the formation of large He-vacancy clusters in the nanochannel W film. Both irradiation fluence and temperature have significant influence on the formation and evolution of He-vacancy clusters, and the evolution of these microstructure also causes hardness changes.

36 MATERIALS SCIENCE↗

Small-scale mechanical testing and characterization of fuel cladding chemical interaction between HT9 cladding and advanced U-based metallic fuel alloy

Fuel cladding chemical interactions (FCCI) occurred on the interface between the nuclear metal fuel and cladding is the primary cause of cladding wastage, weakening cladding mechanical integrity, and placing fuel and cladding at risk. Although the microstructural and phase information of FCCI has been fairly understood, mechanical properties remain less studied due to limited reaction volume. Here, through a combining of advanced electron microscopy characterizations and small-scale mechanical testing techniques, including indentation and micro-tensile testing, this study investigated the microscale mechanical properties of FCCI between the ferritic/martensitic (F/M) HT9 cladding and an advanced Uranium (U)-based metallic fuel irradiated at the Advanced Test Reactor to 2.2% FIMA with peak inner cladding temperature reached to 650 °C. Mechanical testing results show significant hardening and embrittlement in the FCCI region. The brittle fracture of FCCI specimen is mainly attributed to the formation of nano-crystallized intermetallic σ-FeCr phase. Whereas mechanical softening was revealed in the unreacted HT9 matrix due to irradiation-induced microstructural and microchemical evolution, specifically, the disappearance of martensitic lath structure and the formation of Fe 2 Mo Laves phase precipitation which consumed the solid solution strengthening Mo from the F/M HT9 matrix. Due to the achieved high cladding temperature, this fuel pin is of particular significance for revealing the high-temperature irradiation effect on the mechanical properties of HT9 cladding. Therefore, the outcomes of this study are expected to contribute to the development of multi-scale mechanical behavior modeling of HT9 cladding for Generation IV reactors which requires cladding to run at higher temperature (above 600 ?).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ion irradiation study of lithium silicates for fusion blanket applications

Here, this study reports on the microstructural and compositional evolutions, deuterium release and lithium loss behavior in lithium silicates. Pellets of biphasic Li 4 SiO 4 and Li 2 SiO 3 were fabricated using hot pressing of powders. Sequential irradiation with Si + , He + and D + ions was performed up to 773 K to emulate one-year 6 Li burnup in 6 Li 4 SiO 4 inside the SlimCS DEMO. Crystalline Li 4 SiO 4 phase was not observed in the irradiated depth region of all the samples in this study. In spite of full amorphization in the near-surface region, Li 2 SiO 3 irradiated to a high dose at 773 K remained crystalline in the damage peak region, suggesting that Li 2 SiO 3 is more irradiation resistant to amorphization than Li 4 SiO 4 . Radiolysis may be primarily responsible for silicate decomposition and amorphization. Data from this study also show that D release from the pellet is very efficient during ion irradiation at 773 K, which is accompanied with a significant Li loss. Thermal annealing for 10 min at 773 K for the room-temperature irradiated pellet leads to a nearly complete D release without an observable Li loss. A concept of Ni coating on tritium breeder materials is discussed with supporting data to minimize Li loss without a significant impact on tritium diffusion and release.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Deformation textures of aluminum in a multilayered Ti/Al/Nb composite severely deformed by accumulative roll bonding

The accumulative roll bonding process was carried out to produce multilayered Ti/Al/Nb composites up to four cycles. Scanning electron microscopy, transmission electron microscopy electron backscattered diffraction and nanoindentation were employed to investigate the microstructural and texture evolution. A homogenous distribution of Ti/Nb necking layers in Al matrix was achieved after four ARB cycles. Grain refinement was observed to increase with increasing number of ARB cycles. The fraction of high-angle grain boundaries as also increased. Strong recrystallization texture appeared for high number of ARB cycles due to the adiabatic heat that occurs during ARB processing. The shear band at the Ti/Al interface reduced the intensity of the cold rolling fiber textures of Al. There was no evidence of shear component from the orientation distribution function results.

36 MATERIALS SCIENCE↗

Development of nano-Y2O3 dispersed Zr alloys synthesized by mechanical alloying and consolidated by pulse plasma sintering

Highlights: • Zr-Fe-Cr-Cu-Ti-1.0wt% nano-Y{sub 2}O{sub 3} dispersed alloys are fabricated by mechanical alloying and pulse plasma sintering. • These alloys record extremely high compressive strength, Young’s modulus, and hardness. • These mechanical properties are superior as compared to other commercially available Zr based alloys. • Dispersion of nanometric FeZr{sub 2}, Y{sub 2}Ti{sub 2}O{sub 7}, Fe{sub 2}Ti, ZrCu, Cr{sub 2}Zr, Y{sub 2}O{sub 3} leads to grain boundary pinning at elevated temperature. - Abstract: In this paper, Zr alloys are synthesized with nominal compositions: 50Zr-30Fe-10Cr-5Cu-5Ti (alloy A), and 49Zr-30Fe-10Cr-5Cu-5Ti-1Y{sub 2}O{sub 3} (alloy B), 45Zr-30Fe-10Cr-10Cu-5Ti (alloy C), 44Zr-30Fe-10Cr-10Cu-5Ti-1Y{sub 2}O{sub 3} (alloy D) (all in wt%) by mechanical alloying and consolidated by pulse plasma sintering at 1173 K (900 °C), 1223 K (950 °C) and 1273 K (1000 °C) using 75 MPa uniaxial pressure applied for 5 min and 70 kA pulsed current at 3 Hz pulse frequency. The microstructure and phase evolution during mechanical alloying and sintering has been characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM & TEM) and energy dispersive spectroscopy (EDS). Mechanical properties i.e. hardness and compressive strength were determined by using nano-indentation unit and universal testing machine. The produced alloys recorded very high levels of compressive strength (1359–2456 MPa), and hardness (7.05–10.05 GPa) which measures 1.5–2.0 times more than that of other Zr alloys (2 O{sub 3}) particles which can contribute to grain boundary pinning, and improved creep and oxidation resistance at elevated temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗