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At least 1,081 records · Page 60
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Ultrasonic evaluation of oxygen content, modulus, and microstructure changes in YBa2Cu3O(7-x) occurring during oxidation and reduction

Ultrasonic velocity measurement techniques were used to evaluate the effects of oxidation and reduction on the elastic properties, global microstructure and oxygen content of the YBa2Cu3O(7-x) ceramic superconductor for samples ranging from 70 to 90 pct of theoretical density. Bulk density, velocity, and elastic modulus generally increased with increasing oxygen content upon oxidation, and this behavior was reversible. Velocity image patterns were similar after oxidation and reduction treatments for a 90 pct. dense sample, although the velocity value at any given point on the sample was changed following the treatments. The unchanging pattern correlated with destructive measurements showing that the spatial pore distribution (fraction and size) was not measurably altered after the treatments. Changes in superconducting behavior, crystal structure, and grain structure were observed consistent with changes in oxygen content.

Roth, Don J.↗
DOE OSTI2019

Complete Status Report Documenting the Processing, Microstructure and High-Temperature Mechanical Properties of the Nanostructured Ferritic Alloy OFRAC

This report provides a summary of the new nanostructured ferritic alloy, OFRAC (Oak Ridge Fast Reactor Advanced Fuel Cladding), that was developed for the advanced sodium fast reactor fuel cladding and core internals. The composition of OFRAC, which is Fe-12Cr-1Mo-03.Ti-0.3Nb + 0.3Y2O3 (wt. %), was chosen to achieve high temperature strength as well as high temperature creep performance and swelling resistance requirements that past structural materials such as austenitic stainless steels and ferritic/martensitic steels, i.e. HT-9, are not suitable as SFR cladding materials. The mechanical alloying procedures were described for producing OFRAC and the detailed characterization studies revealed uniformly distributed, high concentration of Y-Ti-O enriched oxide particles, or nanoclusters. The Nb addition that was intended to sequester interstitial C and N that are commonly introduced as contamination during ball milling of powder was found to be very effective in forming coarse size Nb carbonitrides along with excess Ti that removes these interstitial elements from the bcc-Fe matrix of OFRAC. The tensile tests on the OFRAC in the extruded condition showed excellent balance in strength and ductility from room temperature to 800°C. Both the microstructure and tensile properties were not significantly degraded after annealing the extruded OFRAC samples for 8 h at 1050°C and 1150°C. The latter temperature is ~76% of the melting point of OFRAC. These results demonstrated the stability of the microstructure and tensile properties to extremely high temperatures. The thermal creep resistance at elevated temperatures and stresses was investigated using strain rate jump testing. The results showed that OFRAC possessed high stress exponents at high stresses and temperatures of 550°C, 600°C, 700ºC and 800°C. This thermal dependence of minimum creep rate indicates that OFRAC will show quite low creep rates at higher temperatures and stresses compared to HT-9 and stainless steels. These significant improvements indicate that the NFA OFRAC alloy is a compelling and viable choice for sodium fast reactor fuel cladding.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Spark Plasma Sintering of high-density fine-grained Y2.5Nd0.5Al5O12+SiC composite ceramics

Highlights: • YAG + (10, 20) wt.% α-SiC high-density ceramics obtained by SPS. • YAG + α-SiC ceramics have a more fine-grained structure than pure garnet. • The optimal sintering temperature of YAG + SiC ceramics is lower than that of garnet. • Introduction of α-SiC particles creates internal stress fields in garnet. • Introduction of α-SiC particles results in lower sintering activation energy of garnet. - Abstract: Spark Plasma Sintering (SPS) has been used to produce samples of fine-grained composites Y{sub 2.5}Nd{sub 0.5}Al{sub 5}O{sub 12} + x wt.% α-SiC (x = 1020) with ∼98–99% density. The microstructure of the composites has been studied, as well as the impact of α-SiC particles on the mechanical properties and kinetics of composite sintering. The introduction of the α-SiC part has been demonstrated to form a more fine-grained structure and under the given SPS conditions change the sintering mechanism in ceramics. The study has also demonstrated that introduction of α-SiC particles into garnet results in formation of internal stress fields, which, in turn, leads to a decrease in the activation energy of sintering of fine-grained composites at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Revealing the evolution of order in materials microstructures using multi-modal computer vision

The development of high-performance materials for microelectronics, energy storage, and extreme environments depends on our ability to describe and direct property-defining microstructural order. Our present understanding is typically derived from laborious manual analysis of imaging and spectroscopy data, which is difficult to scale, challenging to reproduce, and lacks the ability to reveal latent associations needed for mechanistic models. Here, we demonstrate a multi-modal machine learning (ML) approach to describe order from electron microscopy analysis of the complex oxide La 1−x Sr x FeO 3 . We construct a hybrid pipeline based on fully and semi-supervised classification, allowing us to evaluate both the characteristics of each data modality and the value each modality adds to the ensemble. We observe distinct differences in the performance of uni- and multi-modal models, from which we draw general lessons in describing crystal order using computer vision.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Formation kinetics and thermodynamic stability of the Aurivillius compounds in Bi 4 Ti 3 O 12 –BiFeO 3 system

Abstract The Aurivillius compounds in the Bi 2 O 3 –Fe 2 O 3 –TiO 2 system, combining ferroelectric, semiconducting, and ferromagnetic properties, have attracted particular interest. Formation kinetics and thermodynamic stability are the fundamental knowledge needed for modeling and predicting the temporal microstructure and property evolution during materials processing but have not yet been addressed by quantitative experimental measurement. This article focuses on the Bi n +1 Fe n –3 Ti 3 O 3 n +3 Aurivillius compounds on the Bi 4 Ti 3 O 12 –BiFeO 3 tie‐line to elucidate the mechanisms and thermodynamic controls responsible for phase formation of compounds with various perovskite‐like layers. Five high‐purity Aurivillius compounds Bi 4 Ti 3 O 12 , Bi 5 FeTi 3 O 15 , Bi 6 Fe 2 Ti 3 O 18 , Bi 7 Fe 3 Ti 3 O 21 , and Bi 8 Fe 4 Ti 3 O 24 with integer n = 3–7 values were synthesized and their phase transformation properties and enthalpies of formation were studied by X‐ray diffraction in situ, high temperature differential scanning calorimetry, and high temperature oxide melt solution calorimetry. Thermodynamic stability of the compounds decreases with increasing n , and formation kinetics gradually slow down, demonstrating the inherent difficulty to synthesize pure Aurivillius compounds with n larger than 8. This difficulty was confirmed by an impurity phase coexisting with Bi 9 Fe 5 Ti 3 O 27 .

Gong, Weiping↗
DOE OSTI2022

Cantor-derived medium-entropy alloys: bridging the gap between traditional metallic and high-entropy alloys

The year 2004 marked the beginning of a new era in the design of metallic materials, as the concept of multiple principal component alloys, commonly known as High-Entropy Alloys (HEAs), was proposed by Cantor and Yeh. The unexpected single-phase microstructure, instead of the expected brittle intermetallic compounds, was attributed to the large entropy of mixing and immediately caught the attention of the scientific community. Today, HEAs are considered important advanced materials and a broad range of alloys using nominally the same design principle have been investigated. Despite that, the CrMnFeCoNi (Cantor) alloy stands out as the most successful HEA due to its outstanding mechanical properties and microstructure. In this scenario, variants of the Cantor alloy, named medium-entropy alloys (MEAs), are gaining significant interest as they display a better industrial potential than both HEAs and traditional alloys. These variants of the Cantor alloy with only three or four main elements result in 15 possible combinations. The microstructure of these alloys is discussed in terms of advanced characterization as well as thermodynamic parameters and computational simulation. Their phase stability is addressed over a wide range of temperatures and strain rates. The mechanical properties, especially the fracture toughness, of the CrFeCoNi and CrCoNi alloys have been reported to be even superior to those of the Cantor alloy and most modern engineering alloys. This is associated with the formation of a continuous sequence of strengthening mechanisms, including hierarchical twin networks, which serve to prolong the strain hardening. The present article reviews and critically assesses, for the first time, recent advances in these Cantor-derived MEAs.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure and Three-Point Bending Fatigue Behavior of Al-Cu-Mg-Ag Alloys with Various Mg Contents

This paper presents an investigation on the influence of Mg content on the microstructures, tensile properties and three-point bending fatigue behavior of Al-Cu-Mg-Ag alloys. The results indicate that the alloy containing 0.70 wt.% Mg possesses lower tensile properties and higher fatigue performance compared to the one with 1.15 wt.% Mg. Increasing Mg content in Al-Cu-Mg-Ag alloys can enhance the nucleation and precipitation of Ω phase, as well as increase the volume fraction and number density of constituent particles. The investigation of the fatigue crack initiation and growth behavior of Al-Cu-Mg-Ag alloy using interrupted fatigue tests suggests that micro-cracks mainly nucleate on Al{sub 2}Cu constituent particles and the fatigue life is mainly associated with the density of constituent particles.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Process-Defect-Structure-Property Correlations During Laser Powder Bed Fusion of Alloy 718: Role of In Situ and Ex Situ Characterizations

Components made by laser powder bed fusion (L-PBF) additive processes require extensive trial and error optimization to minimize defects and arrive at targeted microstructure and properties. In this paper, in situ infrared thermography and ex situ surface roughness measurements were explored as methodologies to ensure Inconel ® 718-part quality. For a given laser energy of 200 Watts, prismatic samples were produced with different exposure times (80 to 110 µs) and point spacings (80 to 110 µm). The infrared intensities from laser–material interaction zones were measured spatially and temporally. The conditions leading to higher IR intensity and lowest surface roughness values correlated well with less porosity and coarse solidification grain structure. The transition from highly columnar to misoriented growth is attributed to changes in thermal gradients and liquid–solid interface velocities. Hardness measurements and electron microscopy of the as-processed and post-processed heat-treated samples show complex transitions in microstructural states including the heavily dislocated FCC matrix, reduction of dislocation density, and copious precipitation, respectively. These results show that the geometry-process-structure-property correlations are dynamic, and they cascade depending on the transitions of phase states from powder to liquid to solid, as well as phase decompositions and deformations within the solid FCC phase. Finally, validity of using analytical weld process models to describe the above phenomena is also highlighted.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Low and room temperatures tensile properties of a nanoprecipitate-strengthened (FeCoCr)40Ni40Al10Cu10 high-entropy alloy

Highlights: • We designed a (FeCoCr){sub 40}Ni{sub 40}Al{sub 10}Cu{sub 10} high entropy alloy (HEA) strengthened by exclusive L1{sub 2} nano-precipitates. • The present HEA exhibited excellent combination of tensile strength (~1200MPa) and elongation (~36%) at 233 K. • The coherent nano-precipitates, deformation twinning and immobile LC locks made a joint contribution to the optimal mechanical property. - Abstract: We report the tensile properties and microstructural evolution of a high entropy alloy (FeCoCr){sub 40}Ni{sub 40}Al{sub 10}Cu{sub 10} deformed at low temperature (233K) and room temperature (293 K). The alloy presented a superior combination of tensile strength (~1200 MPa) and elongation (~36%) at 233 K than at 293 K. Transmission electron microscopy revealed that the enhanced tensile properties at low temperature were due to deformation twinning, the formation of immobile Lomer-Cottrell dislocation locks, and the high density coherent nano-precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Hot rolling of ZK60 magnesium sheet with isotropic tensile properties from tubing made by Shear Assisted Processing and Extrusion (ShAPE)

In order to evaluate the viability of ShAPE processed Mg alloys as a feedstock for fabricating lightweight sheet material, tubes consisting of ShAPE-extruded Mg alloy ZK60 were flattened into plates and hot rolled at 450 °C to reductions of 37%, 68%, and 93%. The mechanical properties and microstructure of the rolled material were characterized through tensile testing and electron backscattered diffraction (EBSD). ZK60 specimens rolled to 68% reduction had tensile properties similar to published properties of rolled ZK60 sheets fabricated using conventional processes, and exhibited negligible tensile anisotropy referenced to the rolling direction. Additional rolling from 68% to 93% reduced the ultimate tensile stress in the rolling direction from 341.74±5.96 MPa to 260.76±22.4MPa. The yield stress and elongation to failure of the material also decreased from 292.16±1.11 MPa to 256.93±18.4 MPa and 6.95±1.94% to 3.38±0.51%, respectively, but negligible little anisotropy was observed with respect to loading direction. EBSD mapping indicated that the as-extruded ZK60 had texture rotated away from the basal direction which developed into a strong basal texture over numerous hot rolling steps. This evolution in texture has been observed after rolling for hot-rolled ZK60 fabricated through conventional extrusion processes. The initial grain structure was found to have experienced noticeable twinning from flattening the tube into plate. After hot rolling, the grain structure became more equiaxed, but the average grain diameter did not change appreciably from 5.15 ± 3.39 µm in the ShAPE extruded material, to 5.27 ± 12.44 µm in the 93% hot rolled sheet. This response to hot rolling is similar to the response of ZK60 fabricated using other methods such as Equal Channel Angular Processing (ECAP). Therefore, this work demonstrates ShAPE has the potential as an alternative method to producing feedstock for Mg alloy sheets. Modifications to the experimental procedure which could lead to improvements in observed properties are briefly discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Annular Metallic Nuclear Fuel Informatics at 50 nm Resolution

U-10wt.% Zr (U-10Zr) based metallic fuel is the leading candidate for next-generation sodium cooled fast reactor in United States. Advanced post-irradiation characterization (from sub-nanometer to micrometer) helps to understand fuel microstructure and property change during irradiation, benefiting fuel qualification for commercial application. With high velocity image data generating method, an automatic way to extract the microstructural information quantitively can better serve the needs from post irradiation characterization. A trained machine learning model, named Decision Tree, is employed to categorize pores caused by fission gas release and to aid phase identification. This work presents a showcase of this approach on different irradiated U-10Zr metallic fuels. This quantitative data offers insights into the fission product migration and potentially thermal conductivity degradation. This information from machine learning will be fed into fuel design code for better prediction of fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

A detailed study of the microstructure and thermal stability of typical SiC fibers

Highlights: • The cross-sectional microstructure and thermal stability of typical SiC fibers were characterized via SEM and TEM. • The SiC fiber with gradient microstructure has better properties than that with uniform microstructure. • The graphite exhibits straight planes on the fiber surface while they're turbostratic inside the fiber. Continuous SiC fibers have attracted increasing research interest for their significant application in aerospace and nuclear energy. Control of inhomogeneity and decrement of defects are crucial for improving the mechanical and high-temperature performance of SiC fibers. Thus an understanding of fine and detailed microstructural and microchemical distribution of SiC fibers is urgently needed. In the present work, the cross-sectional phase distributions, morphologies and defects of amorphous, non-stoichiometric and near-stoichiometric SiC fibers were well characterized. From surface to core, the amorphous and non-stoichiometric fibers exhibited uniform microstructures, but a gradient change along the radial direction was observed in the near-stoichiometric fiber. Nanosized SiC and turbostratic carbon (2–4 nm) were randomly distributed inside the amorphous fiber. A large amount of graphite surrounding SiC grains appears in the non-stoichiometric fiber which possess low strength and weak thermal stability. The near-stoichiometric fiber has transgranular fracturing, high strength and favorable thermal stability, and the graphite planes are turbostratic inside the fiber but straight on the surface. The results of both energy-dispersive X-ray spectrometry measurements and first-principles calculations demonstrate that Al atoms can occupy Si sites in the SiC grains. Our findings offer fine understanding for fabricating SiC fibers with superior properties.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

Model-informed, Adaptive Physical Vapor Deposition to Fabricate Hierarchical Binary-alloy Thin-films

Designing next generation thin films, tailor-made for specific applications, relies on the availability of robust processing-structure-property relationships. Traditional structure zone diagrams are limited to low-dimensional mappings, with machine-learning methods only recently attempting to relate multiple processing parameters to the final microstructure. Despite this progress, structure-processing relationships are unknown for processing conditions that vary during thin-film deposition, limiting the range of microstructures and properties achievable. In this project, we employed a phase-field computational model combined with a genetic algorithm (GA) to identify and design time-dependent processing protocols that achieve tailor-made microstructures. We simulate the physical vapor deposition of a binary-alloy thin film by employing a phase-field model, where deposition rates and diffusivities are controlled via the genetic algorithm. Our GA-guided protocols achieve targeted microstructures with lateral and vertical concentration modulations, as well as more complex, hierarchical microstructures previously not described in simple structure zone diagrams. Our algorithm provides insight to experimentalists looking for additional avenues to design novel thin-film microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characterization of hot-pressed von Alpen type NASICON ceramic electrolytes

The Na-ion conducting solid electrolyte NASICON is a promising solid state electrolyte (SSE) for use in Na based electrochemical systems. The effects of particle morphology and synthesis of von Alpen type NASICON via hot-pressing were investigated. Spray dried particles were shown to improve mechanical and electrochemical properties. X-ray diffraction, scanning electron microscopy, impulse excitation measurements, Vickers hardness, and impedance spectroscopy were used to correlate relationships between phase purity, microstructure, mechanical properties, and electrochemical properties. Scanning electron microscopy showed the presence of a glass phase as between 19.08% and 28.23% area percentage and a ZrO 2 phase between 0.46% and 3.51% area percentage in the hot-pressed samples. Impulse excitation showed elastic modulus varying from 83.65 to 97.65 GPa. The first values of Poisson's ratio and shear modulus of NASICON are reported as between 0.23 and 0.26 and 33.87 to 38.79 GPa, respectively. Vickers hardness and fracture toughness measurements showed Vickers hardness ranging from 4.30 to 4.68 GPa and fracture toughness ranging from 1.05 to 1.09 MPa m ½ . Impedance spectroscopy showed grain conductivities ranging from 1.023 to 1.287 mS/cm, with grain boundary resistance percentages between 73.22 and 47.5%. Total conductivities ranged from 0.292 to 0.596 mS/cm, with 0.596 mS/cm being achieved at room temperature for the spray dried powders with lower grain boundary resistance percentages.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2001

Structure-Property Correlations in Al-Li Alloy Integrally Stiffened Extrusions

The objective of this investigation was to establish the relationship between mechanical property anisotropy, microstructure and crystallographic texture in integrally 'T'-stiffened extruded panels fabricated from the Al-Li alloys 2195, 2098 and 2096. In-plane properties were measured as a function of orientation at two locations in the panels, namely mid-way between (Skin), and directly beneath (Base), the integral 'T' stiffeners. The 2195 extrusion exhibited the best combination of strength and toughness, but was the most anisotropic. The 2098 extrusion exhibited lower strength and comparable toughness, but was more isotropic than 2195. The 2096 extrusion exhibited the lowest strength and poor toughness, but was the most isotropic. All three alloys exhibited highly elongated grain structures and similar location-dependent variations in grain morphology. The textural characteristics comprised a beta + <100> fiber texture, similar to rolled product, in the Skin regions and alpha <111> + <100> fiber texture, comparable to axisymmetric extruded product, in the Base regions. In an attempt to quantitatively correlate texture with yield strength anisotropy, the original 'full constraint' Taylor model and a variant of the 'relaxed constraint' model, explored by Wert et al., were applied to the data. A comparison of the results revealed that the Wert model was consistently more accurate than the Taylor model.

Hales, Stephen J.↗
DOE OSTI2017

Effect of Ag additions on the lengthening rate of Ω plates and formation of σ phase in Al-Cu-Mg alloys during thermal exposure

Effect of Ag additions on the mechanical properties and microstructures of the peak-aged Al-Cu-Mg alloys during prolonged thermal exposure at 150 °C, was investigated by tensile testing, conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The results showed that after exposure for 500 h, > 85% of the peak strength remained. Microstructure observations indicated that increasing the Ag content from 0.14 to 0.57% promoted the precipitation of a fine and uniform Ω phase and suppressed the formation of the θ′ phase, leading to a notable improvement of the strength properties and thermal stability of the studied alloys. Quantitative TEM analysis showed that the coarsening of Ω phase was predominated by plate lengthening rather than thickening, while its lengthening rate was independent of various Ag additions during exposure at 150 °C. In addition, an increase of Ag also facilitated the formation of a cubic σ phase, which was further supported by STEM results. - Highlights: •Increasing Ag improved strength properties and thermal stability of the alloys. •After exposure for 500 h, > 85% of the peak strength remained. •The lengthening rate of Ω plates remained constant as Ag increased at 150 °C. •Increasing Ag content facilitated the formation of σ phase.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructure, electrical resistivity, and tensile properties of neutron-irradiated Cu–Cr–Nb–Zr

High strength, high conductivity copper alloys that can resist creep at high temperatures are one of the primary candidates for efficient heat exchangers in fusion reactors. Cu–Cr–Nb–Zr (CCNZ) alloys, which were designed to improve the strength and creep life of ITER Cu–Cr–Zr (CCZ) reference alloys, have been found to have comparable electrical conductivity and tensile properties to CCZ alloys. The measured creep rupture times for these improved alloys is about ten times higher than the ITER reference alloys at 90–125 MPa at 500 °C. However, the effects of neutron irradiation on these alloys, and the ensuing material properties, have not been studied; thus, their utility in a fusion reactor environment is not well understood. This study characterizes the room temperature mechanical and electrical properties of a neutron-irradiated CCNZ alloy and compares them to a neutron-irradiated ITER reference heat sink CCZ alloy. Tensile specimens were neutron irradiated in the High Flux Isotope Reactor (HFIR) to 5 dpa between 250 °C and 325 °C. Post-irradiation characterization included electrical resistivity measurements, hardness, and tensile tests. Microstructural evaluation used scanning electron microscopy, energy dispersive x-ray spectroscopy, and atom probe tomography to characterize the irradiation-produced changes in the microstructure and investigate the mechanistic processes leading to post-irradiation properties. Transmutation calculations were validated with composition measurements from atom probe data and used to calculate contributions to the increased electrical resistivity measured after irradiation. Comparisons with CCZ alloys in the same irradiation heat found that the post-irradiated CCNZ and CCZ alloys had comparable electrical resistivity. Although CCNZ alloys suffered more irradiation hardening than CCZ, the overall tensile behavior deviated very little from non-irradiated values in the temperature range studied.

36 MATERIALS SCIENCE↗