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At least 613 records · Page 34
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Microstructural and material property changes in severely deformed Eurofer-97

Severe plastic deformation changes the microstructure and properties of steels, which may be favourable for their use in structural components of nuclear reactors. In this study, high-pressure torsion (HPT) was used to refine the grain structure of Eurofer-97, a ferritic/martensitic steel. Electron microscopy and X-ray diffraction were used to characterise the microstructural changes. Following HPT at room temperature to a maximum shear strain of 230, the average grain size reduced by a factor of ~30, with a marked increase in high-angle grain boundaries. Dislocation density also increased by more than one order of magnitude. The thermal stability of the deformed material was investigated via in-situ annealing during synchrotron X-ray diffraction. This revealed substantial recovery between 450 K – 800 K. Irradiation with 20 MeV Fe-ions to ~0.1 dpa caused a 20% reduction in dislocation density compared to the as-deformed material. However, HPT deformation prior to irradiation only had a minor effect in mitigating the irradiation-induced reductions in thermal diffusivity and surface acoustic wave velocity of the material. Microstructural and material property changes are dominated by deformation compared to irradiation. In light of this, the benefits of using HPT to improve the irradiation resistance of Eurofer-97 are limited. These results provide a multi-faceted view of the changes in ferritic/martensitic steels due to severe plastic deformation, and how these changes can be used to alter material properties.

ion-irradiation↗
DOE OSTI2024

Influence of high-strain-rate compression and subsequent heat treatment on (TiNbZr) 89 (AlTa) 11 refractory high-entropy alloys: Dynamic-mechanical behavior and microstructural changes

This study explored the dynamic-mechanical behavior of a novel low-density (TiNbZr) 89 (AlTa) 11 refractory high-entropy alloy (RHEA) across strain rates ranging from 1.0×10 3 to 3.5×10 3 s –1 . A significant increase in the yield and ultimate compressive strengths with rising strain rates up to 3.0×10 3 s –1 was observed and attributed to enhanced dislocation activities and stress-induced microstructural transformations. The formation of the B2 phase and Zr 5 Al 3 precipitates was found to be crucial in bolstering the alloy strength at high strain rates. Beyond strain rates of 3.0×10 3 s –1 , a decrease in strength occurred due to thermal softening and strain localization. Microstructural analyses at 3.5×10 3 s –1 revealed grain refinement, the development of micro shear bands, and dislocation tangles, which were indicative of dynamic recrystallization. Besides, the findings also revealed that the post-dynamic compression heat treatment further enhanced the hardness and microstructural stability of the alloy. These results highlight the potential of the (TiNbZr) 89 (AlTa) 11 RHEA for applications requiring materials with high strength-to-weight ratios, particularly in dynamically loaded environments. It is expected that the results of this study will further advance our fundamental understanding of the behavior of RHEAs under extreme conditions, thereby opening new avenues for material innovation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Microstructure effects on fatigue crack growth in additively manufactured Ti–6Al–4V

In this article we investigate the relationship between the different microstructural features in additively-manufactured (AM) Direct Metal Laser Deposited Ti–6Al–4V alloys and the observed fatigue and fracture behaviors, using high resolution Digital Image Correlation experiments and microstructural imaging. Fatigue cracks in the AM specimens were observed to periodically propagate parallel to the α' laths and deflect at prior β grain boundaries. Corresponding plastic strain distributions show needle-like regions of high strain that correlated to the α' laths, suggesting significant influence of the microstructure on the plastic zone. In many cases, the fatigue cracks also propagated towards voids from unsintered powder or gas entrapment in the vicinity. In several experiments, premature failure of the AM specimens occurred under monotonic fracture or cyclic fatigue loading, which we attribute to the presence of void clusters located near the crack-tip. These fatigue and fracture characteristics were similar for AM specimens of different build-orientations.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evolution of microstructure and strength of a high entropy alloy undergoing the strain-induced martensitic transformation

In a recent work, we have reported outstanding strength and work hardening exhibited by a metastable high entropy alloy (HEA), Fe 42 Mn 28 Co 10 Cr 15 Si 5 (in at. %), undergoing the strain-induced martensitic transformation from metastable gamma austenite (γ) to stable epsilon martensite (ε). However, the alloy exhibited poor ductility, which was attributed to the presence of the brittle sigma (σ) phase in its microstructure. The present work reports the evolution of microstructure, strength, and ductility of a similar HEA, Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 (in at. %), designed to suppress the formation of σ phase. A cast and then rolled plate of the alloy was processed into four conditions by annealing for 10 and 30 min at 1100 °C and by friction stir processing (FSP) at tool rotation rates of 150 and 400 revolutions per minute (RPM) to facilitate detailed examinations of variable initial grain structures. Neutron diffraction and electron microscopy were employed to characterize the microstructure and texture evolution. The initial materials had variable grain size but nearly 100% γ structure. Diffusionless strain induced γ→ε phase transformation took place under compression with higher rate initially and slower rate at the later stages of deformation, independent on the initial grain size. The transformation facilitated part of plastic strain accommodation and rapid strain hardening owing to a transformation-induced dynamic Hall-Petch-type barrier effect, increase in dislocation density, and texture. Here, the peak strength of nearly 2 GPa was achieved under compression using the structure created by double pass FSP (150 RPM followed by 150 RPM). Remarkably, the tensile elongation exhibited by the alloy was nearly 20% with fracture surfaces featuring a combination of ductile dimples and cleavage.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Effects of rejuvenation modes on the microstructures and mechanical properties of metallic glasses

This study systematically investigates the effects of three rejuvenation modes, namely biaxial loading, thermal pressure loading, and cryogenic thermal cycling, on the microstructures and mechanical properties of Cu 64 Zr 36 metallic glasses (MGs) using molecular dynamics (MD) simulations. The simulation results demonstrate that biaxial tension application during loading results in a rejuvenated glassy state with high strength. Specifically, we find that the yield stress, Young's modulus, and shear modulus of the rejuvenated glass obtained by biaxial tensile loading decreased by 2.8%, 2.1%, and 2.7%, respectively, compared to an as-cast MG reference. We also find that MGs achieve the greatest degree of rejuvenation, at the expense of strength, with the use of thermal pressure loading. Interestingly, the application of cryogenic thermal cycling results in a rejuvenated state with a lower strength drop compared to thermal pressure loading. Furthermore, analysis of the potential energy and medium-range-order (MRO) size indicates that the microstructures of MGs achieves a high-energy ordered glass state after thermal pressure loading, but a high-energy disordered glass state after biaxial tensile loading and cryogenic thermal cycling. Furthermore, these findings provide meaningful insights into the effect of rejuvenation modes on the microstructures and mechanical properties of MGs, as well as useful guidelines for designing MGs with high strength and superior plasticity for prospective applications in industry.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Process and feedstock driven microstructure for laser powder bed fusion of 316L stainless steel

Here in the pursuit of improving additively manufactured (AM) component quality and reliability, fine-tuning critical process parameters such as laser power and scan speed is a great first step toward limiting defect formation and optimizing the microstructure. However, the synergistic effects between these process parameters, layer thickness, and feedstock attributes (e.g. powder size distribution) on part characteristics such as microstructure, density, hardness, and surface roughness are not as well-studied. In this work, we investigate 316L stainless steel density cubes built via laser powder bed fusion (L-PBF), emphasizing the significant microstructural changes that occur due to altering the volumetric energy density (VED) via laser power, scan speed, and layer thickness changes, coupled with different starting powder size distributions. This study demonstrates that there is not one ideal process set and powder size distribution for each machine. Instead, there are several combinations or feedstock/process parameter ‘recipes’ to achieve similar goals. This study also establishes that for equivalent VEDs, changing powder size can significantly alter part density, GND density, and hardness. Through proper parameter and feedstock control, part attributes such as density, grain size, texture, dislocation density, hardness, and surface roughness can be customized, thereby creating multiple high-performance regions in the AM process space.

316L stainless steel↗
DOE OSTI2025

Microstructural evolution and phase stability in Nb-containing interstitial Fe-Mn-Co-Cr-C high-entropy alloys: An in-situ synchrotron X-ray diffraction study during laser melting

The influence of Nb on phase stability and microstructural evolution in an interstitial Fe-Mn-Co-Cr-C high-entropy alloy was investigated using in-situ synchrotron X-ray diffraction (SXRD) during laser melting. Scheil-Gulliver simulations predict the formation of σ and γ-f.c.c. phases in all three alloys, along with NbC in Nb-containing compositions. SXRD confirmed the presence of most predicted phases, but the σ phase was absent. Nb promotes crystallite refinement and increases dislocation density, though excessive additions reduce refinement efficiency due to solubility limits and secondary phase formation. Furthermore, Nb addition also enhances ε-h.c.p. phase formation by reducing stacking fault energy through NbC-induced carbon depletion. Analysis of intensity peak evolution reveals that Nb alters preferred grain orientations, reducing {111} γ intensity while enhancing {220} γ , leading to a more isotropic grain distribution. Overall, Nb plays a key role in phase selection, microstructure refinement, and preferred orientation evolution, allowing the tailored microstructure of high-entropy alloys via rapid solidification.

Interstitial high entropy alloys↗
DOE OSTI2020

Laser-interference pulse number dependence of surface chemistry and sub-surface microstructure of AA2024-T3 alloy

The laser-based treatment of a metal surface is an intrinsically non-chemical technique that can alter both the topology and chemistry of surfaces. A laser-based treatment for coating and joining applications can offer alternative surface preparations to the chemically-based surface preparation techniques, which are subject to severe environmental protection and hazardous-waste management considerations. In this study, the surface chemistry and sub-surface microstructural changes are investigated for a novel surface processing method using laser interferometry produced by two beams of a pulsed Nd:YAG laser. The two-beam laser-interference allowed the structuring of the surface at length scales much less than that of the laser beam spot. Surface chemistry changes in the oxide layer of AA 2024-T3 aluminum alloy rolled sheet due to laser processing were investigated using x-ray photoelectron spectroscopy (XPS). Near surface microstructural changes have been investigated with scanning electron microscopy and energy dispersive x-ray spectroscopy (SEM/EDS), and scanning transmission electron microscopy (STEM) as a function of number of interfering laser shots. SEM microstructure pictures of the top surface shows the minimization of surface defects, as all of the sharp features from a rolled sheet surface were smoothed by laser-structuring. STEM images indicate that the laser-interference processing reduced the formation of CuMn-rich precipitates over a 500–800 nm depth from the top surface. XPS data indicated that the Al oxide layer is modified compared to that of the baseline specimen and that the oxide thickness increases with the number of shots per spot. Finally, the additional thicker oxide on Al alloys is expected to increase the corrosion resistance of the coated Al 2024.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural evolution of an aluminide coating on alloy 625 during wet air exposure at 900 °C and 1000 °C

The microstructural changes of the aluminized alloy 625 during cyclic oxidation in air + 6% H 2 O at 900 °C and 1000 °C were analyzed using optical metallography (OM), scanning electron microscopy (SEM) with energy and wave length dispersive X-ray analysis (EDX/WDX) as well as electron backscatter diffraction (EBSD). An in-house developed thermodynamic-kinetic procedure was employed to predict the microstructural evolution of aluminized alloy 625 during high temperature exposure by considering simultaneously occurring surface oxidation and interdiffusion processes. Because of the lack of mobility data for the relevant alloying elements in the σ-phase, assumptions for the mobilities were made based on the value of the mobilities in α-Cr. Despite these assumptions, the calculated results were found to be in good agreement with experimental observations. The complete depletion of β-NiAl in the coating observed during exposure at 1000 °C was correctly predicted by the model. The model was also able to infer dissolution of the precipitate phases α-Cr and σ in the interdiffusion zone during exposures at 900 °C and 1000 °C. The model was yet unable to predict the formation of the μ-phase in the alloy after 1000 h of exposure at 1000 °C. The developed modelling method offers the potential to predict microstructural changes of aluminized nickel base alloys thus reducing cost and time consuming experimental efforts.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Effect of CMAS viscosity on the infiltration depth in thermal barrier coatings of different microstructures

Calcium magnesium aluminum silicate (CMAS) is one of the leading concerns for the gas turbine industry. The effects of CMAS viscosity and the coating microstructure on CMAS infiltration depth were explored by conducting a time dependent interaction study. Three CMAS compositions were used from literature, and their viscosities predicted through FactSage viscosity module were drastically different. The interaction was carried out on three different TBCs synthesized using the solution precursor plasma spray process (SPPS): two of the TBCs were made of yttrium aluminum garnet (YAG) having different microstructures that promote different modes of CMAS infiltration, and one TBC was made of gadolinium zirconate (GZO). All samples had stress relieving vertical cracks and different intensities of horizontally banded porosity, (inter pass boundaries IPBs). A concentration of 100 mg/cm 2 of CMAS was applied on the TBCs which were then subjected to a 5-minute interaction at 1300 °C. Samples were analyzed using scanning electron microscopy (SEM), electron dispersive X-ray spectroscopy (EDXS), and transmission electron microscopy (TEM). Low viscosity CMAS readily penetrated the TBCs while more viscous CMAS showed less penetration. The depth of CMAS infiltration depended on the coating microstructure. In the YAG with IPBs, the CMAS spread horizontally in the IPBs before infiltrating deeper, resulting in reduced infiltration depth compared to other samples in spite of having wider vertical cracks. TEM and EDXS analysis were performed to investigate the phases present in the CMAS-TBC interaction region in YAG. Two regions were chosen, the top TBC surface in direct contact with the sea of CMAS, and the region at the CMAS penetration ended within the coating. Finally, the results showed that no secondary phases like apatite were observed in YAG, thus it can be concluded that the arrest of CMAS happened solely because of CMAS viscosity and the short infiltration time.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Self-Organization and Nitrogen Incorporation in Diamond-Like Carbon Microstructures Synthesized by Nonthermal Plasma

Nonthermal plasma activation of light alkanes is an encouraging decarbonization strategy to produce chemicals or fuels from abundant and/or flared carbon sources. However, prolific carbon growth on both the catalyst and electrode has limited its practicality, requiring additional knowledge of the carbon structure and growth mechanism before breakthroughs are realized. Furthermore, visual evidence is provided for nonuniform diamond-like carbon (DLC) microstructures that materialize in a coaxial dielectric barrier discharge (DBD) reactor flowing ethane and He at 278 K. Through a connection to known behaviors of DBD microdischarge patterns, the microstructure spacing was controlled by altering the applied voltage (ΔV) of the plasma or the burning voltage (U b ). Additionally, carbon valorization through nitrogen incorporation from N 2 was explored as an orthogonal solution to carbon mitigation, with N/C values >0.25 achieved and both sp 2 and sp 3 C–N bonding observed in the microstructures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Investigation of MgO additives on microstructure and properties of thin LLZO electrolytes for all-solid-state batteries

To realize high-energy density lithium lanthanum zirconate (LLZO)-based solid-state batteries (SSB), LLZO electrolytes should be fabricated with low thickness and high mechanical strength. An effective strategy for strengthening ceramic materials is to use additives. Here, we employed MgO nanopowders and fibers as additives for the thin LLZO electrolyte in order to improve the mechanical strength. The microstructure, mechanical properties, and electrochemical properties are characterized to investigate the effects of adding MgO and sintering time. The MgO remains at grain boundaries after sintering, making the microstructure of LLZO fine and uniform. The mechanical strength of the MgO-added LLZO was enhanced by more than 60% while maintaining high ionic conductivity (1 × 10 -4 S cm -1 ) at room temperature. Li symmetric cells using the MgO fiber–LLZO and MgO powder–LLZO exhibit 2 and 3 times higher critical current density (CCD) than those of pure LLZO, and a solid-state full cell exhibits stable cycling performance. Further, these results demonstrate that the use of MgO nanopowder or fiber as an additive for thin LLZO is beneficial for high-current density cycling, by improving mechanical properties and microstructure.

25 ENERGY STORAGE↗
DOE OSTI2019

A data-driven approach to construct a quantitative relationship between microstructural features of fatigue cracks and contact acoustic nonlinearity

This study demonstrates the feasibility of a data-driven approach to construct a quantitative relationship between nonlinear acoustic parameters and microstructural features of contact interfaces. The near-surface nonlinearity is measured using dynamic acousto-elastic testing (DAET) with a surface wave probe, while the microstructural features are extracted from scanning electron microscopy (SEM) images of fatigue cracks. Four aluminum alloy samples, each having a fatigue crack are prepared. Six local nonlinearity parameters are measured at different locations along the crack propagation direction. A total of 40 local measurements are acquired. A principal component analysis (PCA) reveals that all six nonlinearity parameters are correlated and hence can be replaced by one principal component (PC). Fifteen crack micro-geometrical features at each measurement point were extracted from the SEM images. Regression analysis is used to relate the PC of the nonlinearity parameters to the microstructural features at the crack interface. We compare three regression models that take variable selection into account: stepwise multiple linear regression (MLR), stepwise principal component regression (PCR), and least absolute shrinkage and selection operator (LASSO). Despite having different principles, the three predictive models identify two features as the most significant in predicting the interface nonlinearity: the crack aperture (opening) distribution and the distance to the crack tip. The differences between the three models and the physical interpretation of the data-driven predictions are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Pre-Irradiation Comparison of W-Based Alloys for the PHENIX Campaign: Microstructure, Composition, and Mechanical Properties

Tungsten is the material of choice as the plasma-facing material in future plasma-burning fusion reactors. During operation, plasma-facing materials will be simultaneously exposed to 14-MeV neutrons, low-energy D/He particles, and high heat loads. Neutron irradiation of tungsten results in bulk material damage, including knock-on damage causing loops and voids, and transmutation reactions leading to the transmutation of tungsten to rhenium and osmium. Under irradiation to high dose, Re and Os atoms can amalgamate into precipitates that drastically alter the material properties, noticeably increasing the hardness. However, the early-stage development of Re and Os precipitates under a fast neutron spectrum has not been investigated.In this work, the microstructure and hardening behavior of W-Re alloys containing 0 to 2.2 wt% Re, TiC-doped W, and powder-injection-molded W are investigated prior to neutron irradiation at 500ºC and 800ºC to ~0.1 displacement per atom in the High Flux Isotope Reactor (HFIR) to establish a baseline understanding of the starting microstructures.Transmission electron microscopy analysis indicates a dislocation-heavy microstructure, and scanning transmission electron microscopy–energy dispersive spectroscopy shows no spatial segregation of Re and W. Similarly, surface compositional studies performed with electron backscatter diffraction and X-ray photoelectron spectroscopy showed no presence of Re, indicating the Re did not segregate or form new phases during fabrication. Here, the alloys in their as-fabricated state showed no Re segregation or second-phase development, with no significant differences between their microstructures and Vickers hardness values.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructure-dependent rate theory model of defect segregation and phase stability in irradiated polycrystalline LiAlO 2

We report gamma lithium aluminate (LiAlO 2 ) is a breeder material for tritium and is one of key components in a tritium-producing burnable absorber rod (TPBAR). Dissolution and precipitation of second phases such as LiAl 5 O 8 and voids are observed in irradiated LiAlO 2 . Such microstructure changes cause the degradation of thermomechanical properties of LiAlO 2 and affect tritium retention and release kinetics, and hence, the TPBAR performance. In this work, a microstructure-dependent model of radiation-induced segregation (RIS) has been developed for investigating the accumulation of species and phase stability in polycrystalline LiAlO 2 structures under irradiation. Three sublattices (i.e. [Li, Al, V] I [O, V o ] II [Li i , Al i , O i , V i ] III ), and concentrations of six diffusive species (i.e. Li; vacancy of Li or Al at [Li, Al, V] I sublattice, O vacancy at [O, V o ] II sublattice, and Li, Al and O interstitials at [Li i , Al i , O i , V i ] III interstitial sublattices; are used to describe spatial and temporal distributions of defects and chemistry. Microstructure-dependent thermodynamic and kinetic properties including the generation, reaction, and chemical potentials of defects and defect mobility are taken into account in the model. The parametric studies demonstrated the capability of the developed RIS model to assess the effect of thermodynamic and kinetic properties of defects on the segregation and depletion of species in polycrystalline structures and to explain the phase stability observed in irradiated LiAlO 2 samples. The developed RIS model will be extended to study the precipitation of LiAl 5 O 8 and voids and tritium retention by integrating the phase-field method.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Reducing leakage current and enhancing polarization in multiferroic 3D super-nanocomposites by microstructure engineering

Abstract Multiferroic materials have generated great interest due to their potential as functional device materials. Nanocomposites have been increasingly used to design and generate new functionalities by pairing dissimilar ferroic materials, though the combination often introduces new complexity and challenges unforeseeable in single-phase counterparts. The recently developed approaches to fabricate 3D super-nanocomposites (3D‐sNC) open new avenues to control and enhance functional properties. In this work, we develop a new 3D‐sNC with CoFe 2 O 4 (CFO) short nanopillar arrays embedded in BaTiO 3 (BTO) film matrix via microstructure engineering by alternatively depositing BTO:CFO vertically-aligned nanocomposite layers and single-phase BTO layers. This microstructure engineering method allows encapsulating the relative conducting CFO phase by the insulating BTO phase, which suppress the leakage current and enhance the polarization. Our results demonstrate that microstructure engineering in 3D‐sNC offers a new bottom–up method of fabricating advanced nanostructures with a wide range of possible configurations for applications where the functional properties need to be systematically modified.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Enhanced Terahertz Emission of GaAs Microstructures

We observed the enhancement of terahertz radiation emitted from GaAs microstructures under wavelength tuned optical excitation. GaAs microstructure thin films were prepared by molecular beam epitaxy method. The peak amplitude of terahertz radiation from GaAs microstructure is more than eight times that from semi-insulating GaAs.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Fabrication of Polymer Membrane-Suspended Microstructures on Printed Circuit Boards

When microelectromechanical systems are manufactured in high densities, the necessary routing layer structures can become complex and thus expensive if executed in silicon technology. If, additionally, the microstructures are also to be fabricated suspended on membranes, complex thinning processes become necessary to form these often rather fragile membranes. Here, a novel fabrication concept is demonstrated that allows for the fabrication of membrane-suspended microstructures using standard microfabrication techniques directly integrated with printed circuit boards (PCB) by laminating polyimide (PI) films over cavities in the PCB. This results in cost-effective routing layer fabrication and direct compatibility with common electronic component standards such as SMT (surface-mount technology) and THT (through-hole technology). To illustrate the capabilities of the fabrication process, we fabricated an array of membrane suspended microheaters. Individual platinum microheater elements are suspended on PI membranes that are 25 μm thick and 500 μm in diameter. The fabricated PCB carries a 10x10 array of suspended microheaters on an area of 26,mm x 26,mm. Here, the characterization of the microheater array shows that a yield of 86% functional microheaters was achieved. An individual microheater shows an almost linear heating characteristic at least up to 200°C demonstrating the viability of the technique for creating functional membrane-suspended microstructures on a PCB. [2021-0226]

47 OTHER INSTRUMENTATION↗