SEARCH · Engineering Papers

Results for “microstructure”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 667 records · Page 37

All sources NASA NTRS DOE OSTI

DOE OSTI2022

Effect of nitriding on mechanical and microstructural properties of Direct Metal Laser Sintered 17-4PH stainless steel

In this work, the effect of the nitriding process on microstructure and mechanical properties of additively manufactured (AM) 17-4PH stainless steel is investigated. The nitriding was performed at 530 °C, 560 °C, and 580 °C for 2 h. The nitriding process improves the hardness and surface roughness of the AM 17-4PH steel. Detailed microstructural characterizations of both as-built and nitride samples are performed using an optical microscope, scanning electron microscope (SEM) equipped with energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction technique. It reveals that the nitride layer thickness increases with nitriding temperature. A distinct transition layer between the substrate and nitride layer is observed in the 560 °C and 580 °C nitride samples. The nitriding process develops almost equiaxed grain microstructure with new secondary phase precipitates, whereas in the as-built material, the grains are primarily columnar along the AM process build direction. Specifically, the nitriding process introduces γ-Fe4N, ε-Fe3N, CrN, and Ni3N precipitates. The increase in Ni- and Cu-rich precipitates with the nitriding temperature explains the observed improvement in the hardness and surface roughness. Furthermore, the nitriding process does not alter the substrate's initial weak crystallographic texture.

17-4PH steel↗

DOE OSTI2021

Quantifying the effect of hydride microstructure on zirconium alloys embrittlement using image analysis

Since hydride microstructure can significantly influence Zr alloy nuclear fuel cladding’s ductility, a new metric has been developed to quantify hydride microstructure in 2D micrographs and relate it to crack propagation. As cladding failure usually results from a hoop stress, this new metric, called the Radial Hydride Continuous Path (RHCP), is based on quantifying the continuity of brittle hydride particles along the radial direction of the cladding tube. Compared to previous metrics, this approach more closely relates to the propensity of a crack to propagate radially through the cladding tube thickness. The RHCP takes into account hydride length, orientation, and connectivity to choose the optimal path for crack propagation through the cladding thickness. The RHCP can therefore be more closely linked to hydride embrittlement of the Zr alloy material, thus creating a relationship between material structure, properties, and performance. The new definition, along with previously proposed metrics such as the Radial Hydride Fraction (RHF), the Hydride Continuity Coefficient (HCC), and the Radial Hydride Continuity Factor (RHCF), have been implemented and automated in MATLAB. These codes are made available with this publication as supplementary materials. These metrics were verified by comparing their predictions of hydride morphology against expected values in simple cases, and the implementation of the new metric was validated by comparing its predictions with manual measurements of hydride microstructure performed on ImageJ. The RHCP was also validated against experimental measurements of fracture behavior and it was shown to correlate with cladding failure better than previous metrics. The information provided by these metrics will help accurately assess cladding integrity during operation, transportation, and storage.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Microstructure-process relationships in monolithic U-10Mo fuel foil single-pass rolling: A parametric simulation study

In this work, a previously validated coupling of Kinetic Monte Carlo (KMC) Potts Model and finite element method (FEM) simulations was implemented to investigate the effects of microstructural features in as-cast and homogenized monolithic U-10Mo foils on the emergent microstructure after rolling and reheating. Parameters that could potentially affect recrystallization behavior of the rolled U-10Mo foils were considered: grain size distribution, uranium carbide (UC) size distribution, UC volume fraction, spatial distribution of UC, and rolling reduction magnitude. Grain structure and the magnitude of rolling reduction have the strongest influence on recrystallization kinetics and the fabricated grain size distribution. The UC distribution had only a weak effect on the recrystallization kinetics and final microstructures. While particle-stimulated nucleation (PSN) occurred in simulation more frequently as grain size increased, its incidence did not appear to considerably affect the recrystallization kinetics or grain size distribution.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Microstructure and phase evolution in the U-10Zr fuel investigated by in situ TEM heating experiments

The development of U-Zr metallic nuclear fuel for fast spectrum reactors is impacted by a lack of mechanistic understanding of the fuel behavior evolution under thermal irradiation conditions, despite previous works providing substantial fuel performance data. This work uses in-situ transmission electron microscopy heating experiments to study phase and microstructural evolution in several unirradiated U-10Zr specimens during rapid heating ramps (from room temperature to 1000 °C). The starting a-U + bcc-(Zr, U) eutectic microstructure began to decompose above 600 °C. The decomposition initiated from the bcc (U,Zr) phase. Similar results were observed for all specimens even when fabricated by different routes (e.g., cold rolled or annealed). As a result, the impact of observed microstructure and phase evolutions at high temperatures on fuel fabrication and in-pile fuel transient test was also discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Irradiation creep measurement and microstructural analysis of chromium nitride–coated zirconium alloy using pressurized tubes

Environmental barrier coatings for Zr-based materials are currently under development to reduce oxidation and embrittlement in light-water reactors. Chromium nitride is one such candidate for this application, particularly as accident-tolerant fuel cladding. However, quantifying the impact of coatings on the irradiation-induced creep of zircaloy (Zry) is critical as this mechanism often exceeds thermal creep rates under light-water reactor operating conditions and can be a limiting design characteristic. Additionally, examining irradiation effects in the microstructure at the coating interface is key to understanding the compatibility of the material system. Here, to accelerate the experimental measurement of irradiation creep and microstructure evolution in CrN-Zry, compact, pressurized creep tubes were fabricated and irradiated in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory. Miniature, thin-walled rodlets fabricated from annealed Zr-Sn barstock were coated with CrN using physical vapor deposition (PVD) to nominal thicknesses of 4 and 8 μm. Coated and uncoated rodlet specimens were internally pressurized and welded, generating nominal circumferential hoop stresses of 0, 90, or 180 MPa under 300°C irradiation conditions. Twelve specimens were measured diametrically prior to irradiation using a low-cost, automated, contactless laser profilometer developed for this work. Specimens were irradiated in sealed capsules for one 25-day HFIR cycle, accumulating approximately 1.8 $\times$ 10 21 n/cm 2 fast fluence (E n > 10 MeV). The irradiated samples were retrieved and remeasured using the same profilometry system in a shielded hot cell facility. Irradiation creep between specimens was compared using standard statistical tests and showed that both thicknesses of CrN coating had a negligible effect on the irradiation creep strain of the Zry material. Microstructure characterization of pre- and post-irradiated CrN-Zry specimens showed minimal changes due to irradiation but did show a substantial O-rich region at the Zry-CrN interface.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Correlating microstructure and mechanical properties of harvested high dose Zorita light water reactor internals

Here, in this study, microstructural studies and micro-mechanical testing of an ex-plant material harvested from the decommissioned pressurized water reactor (PWR) is carried out. Irradiated 304 stainless steel (SS) components were harvested by the Electric Power Research Institute, U.S. Nuclear Regulatory Commission, and members of the José Cabrera Nuclear Power Station (Zorita) in Spain. The bi-crystalline micro-tensile specimens, atom probe tomography (APT) tips, and transmission electron microscopy (TEM) lamellae were fabricated from the baffle plate materials irradiated to 0.05, 15 and 50 dpa to elucidate microstructural, microchemical, and local mechanical properties changes as a function of dose. TEM and APT studies reveal radiation induced Ni, Cr, and Si rich precipitates in the 15 dpa sample that become smaller and partially redissolve into the matrix of the 50 dpa sample (decreasing size and number density). Dislocation loop and cavity number density and size were quantified as a function of dose as well as swelling. Intergranular Ni and Si enrichments with concomitant Fe and Cr depletion were observed in the 15 dpa sample and were more pronounced in the 50 dpa sample. Micro-tensile testing performed in the scanning electron microscope (SEM) at room temperature and 300 °C shows that the material's local yield strength and ultimate tensile strength decreases with increased dose and elevated test temperature and provides further insights via localized strain mapping. Current and previous mechanical data was compared with calculated values using the dispersed barrier hardening model with inputs of dislocation loops, precipitates, and cavities from microstructural characterization.

36 MATERIALS SCIENCE↗

DOE OSTI2019

High-throughput, super-resolution 3D reconstruction of nano-structured solid oxide fuel cell electrodes and quantification of microstructure-property relationships

Nano-structuring methods are actively applied to solid oxide fuel cell electrodes to reduce the operating temperature while preserving a high electro-catalytic activity. The unique nanoscale microstructure is vital to electrochemical performance, yet not well quantified in three dimensions. Here, with a multi-stage recovering principle of distance correlation functions, the three-dimensional microstructures of La 0.8 Sr 0.2 MnO 3-δ nanoparticles infiltrated porous Y 0.16 Zr 0.84 O 2-δ electrodes are reconstructed with a dimension of 1024 × 1024 × 1024 voxels at a resolution of 7.5 nm from one two-dimensional micrograph. The key geometric characteristics, such as tortuosity factors, active surface/interface areas and three-phase boundary length, are calculated from the reconstructed three-dimensional microstructures at various loadings of La 0.8 Sr 0.2 MnO 3-δ . Combining with the analysis of distribution of relaxation times, the active three-phase boundary length is shown to be the main factor governing the electrode impedance, and is related quantitatively to the electrochemical process at high frequency. The accuracy of capturing nanoscale features is validated by the focused ion beam sectioning dataset of a Ni-Y 0.16 Zr 0.84 O 2-δ electrode at nanoscale resolution. Lastly, this work provides a promising strategy for reconstructing three-dimensional heterogeneous nanostructures from one super-resolution two-dimensional micrograph, and demonstrates a quantitative approach for uncovering processing-structure-property relationships of nanostructured electrodes and beyond.

25 ENERGY STORAGE↗

DOE OSTI2020

Correlative electron and ion beam analysis of the electrochemical performances of LiV 3 O 8 cathode films as a function of microstructures

Degradation mechanisms in LiV 3 O 8 cathode films (~500 nm) with different initial microstructures i.e., globular nanocrystals in amorphous matrix and needle-like nanocrystals, synthesized by annealing the cathodes at 150 °C and 300 °C for 6 h are studied by Transmission Electron Microscopy (TEM) and Auger Electron Spectroscopy (AES). In addition, a unique in-situ combination of TEM and Secondary Ion Mass Spectrometry (SIMS) imaging techniques, namely Parallel Ion and Electron beam Spectrometry (PIES) is carried out to measure the 3D distribution of V and Li with nanoscale resolution. These characterization studies focus on correlating the pre- and post-cycling microstructure to observed electrochemical performance. The LiV 3 O 8 cathode film with needle-like nanocrystals (300 °C) shows a higher initial capacity but it degrades rapidly compared to the film with globular nanocrystals embedded in amorphous matrix (150 °C). We observed that LiV 3 O 8 films with needle-like nanocrystals are more susceptible to cathode decohesion and vanadium dissolution than the films with globular nanocrystals embedded in amorphous matrix, explaining the differences in their electrochemical performance. The findings from this study have relevance to the development of thin film electrode microstructures for high capacity and cyclic stability.

25 ENERGY STORAGE↗

DOE OSTI2025

High spatial resolution neutron imaging of lithium-ion batteries: Correlating microstructure and lithium transport

Thick electrodes for lithium-ion batteries can increase the overall energy density, but increasing the electrode thickness introduces charge transport limitations. These limitations may be mitigated through proper electrode structuring. Here, high spatial resolution neutron imaging was used to understand the correlation between microstructure and lithium transport in lithium-ion anodes. Batteries with distinct graphite anode microstructures were produced and studied with high spatial resolution in operando neutron radiography to observe the effects of structure on transport. High spatial resolution neutron computed tomography was performed following in operando neutron radiography. X-ray computed tomography and scanning electron microscopy were used to observe the finer scale anode structure to complement neutron imaging. Solvent-free anodes containing a tightly-packed layered structure confined lithium movement close to the separator. This structure limited capacity, but supported better rate capability. Conversely, a more open pore structure in the wet cast anodes yielded higher capacity with reduced rate capability. Together, these results show that lithium distributions can be controlled by the macroscopic structure of the electrodes, the microstructural pore network, and the microscale active areas that support electrochemical reactions. Furthermore, multimodal imaging applying the complementary strengths of neutron and X-ray methods is shown as a tool for advancing battery design.

25 ENERGY STORAGE↗

DOE OSTI2018

Microstructural characterization and comparison of Ti-6Al-4V manufactured with different additive manufacturing processes

In this work, the microstructures of Ti-6Al-4V manufactured by different additive manufacturing (AM) processes have been characterized and compared. The microstructural features that were characterized are the α lath thickness, grain boundary α (GB-α) thickness, prior β grain size and α colony size. In addition, the microhardnesses were also measured and compared. The microstructure of shaped metal deposited (SMD) Ti-6Al-4V material showed the smallest variations in α lath size, whereas the material manufactured with laser metal wire deposition-0 (LMwD-0) showed the largest variation. The prior β grain size was found to be smaller in material manufactured with powder bed fusion (PBF) as compared with corresponding material manufactured with the directed energy deposition (DED) processes. Parallel bands were only observed in materials manufactured with DED processes while being non-present in material manufactured with PBF processes.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of build geometry on the microstructural development of 316L parts produced by additive manufacturing

Highlights: • Stainless steel ribs were created via direct metal laser sintering to investigate microstructural effect of part design. • EBSD confirmed the presence of large elongated grains in the center of the part, with preferred orientation. • Small grains at the rib surface were found to grow towards the center of the rib with random orientation. • By changing rib thickness and build angle varying texture was observed in the final products. • Large intragranular misorientations were observed in all samples. - Abstract: Additive manufacturing (AM) technology has shown great potential in manufacturing complex products, such as lattice structures without extensive tooling. The focus of this study was to understand the effect of the part geometry on the resulting microstructure. Direct metal laser sintering was used for fabrication of ribs with thicknesses varying between 0.2 and 3.0 mm as well as inclined ribs the with build angles of 30° and 45°. The investigation showed that grains were growing in an epitaxial manner parallel to the building direction. The large elongated grains had a preferential orientation, resulting from the temperature gradient. Additionally, it was found that small grains had formed close to the part surface which were inclined towards the center of the rib. In contrast to the elongated grains, they had a random orientations. The results also indicated that at build angles below 45°, the formed microstructure consisted of the large grains elongated in the building direction. For the used process parameters, the critical part thickness to avoid large elongated grains was found to be about 0.4 mm. These findings allowed us to establish the basics for design rules when it comes to thin wall structures.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Influence of rapid heating and cooling combined with deformation at ultrahigh strain rates on the microstructure evolution of pure titanium shaped charge liner

Highlights: • A slug prepared from pure titanium SCL was recovered after detonation deformation at an ultrahigh strain rate over 10{sup 5} s{sup −1}. • The α → β → α phase transformation occurred in Ti SCL during the ultrahigh-strain -rate deformation. • The microstructures of the recovered slug included lamellar α grains, equiaxed α grains, and jagged α grains. - Abstract: A slug prepared from pure titanium shaped charge liners was recovered after detonation deformation at an ultrahigh strain rate over 10{sup 5} s{sup −1} and high strain over 500%. Optical microscopy, electron backscattered diffraction (EBSD), and transmission electron microscopy (TEM) were employed to investigate the microstructure of the Ti shaped charged liner before and after the detonation deformation. The microstructures of the recovered slug include lamellar α grains, equiaxed α grains within localized shear bands, and jagged α grains. EBSD results indicated that the grain orientation distribution is random and no texture was observed in the slug. TEM observation revealed that the α → β → α phase transformation occurred owing to the rapid heating and cooling combined with deformation at ultrahigh strain rates in the Ti shaped charge liner. No melting phenomenon was observed during the deformation process. The deformation process consisted of the explosive detonation stage combined with rapid heating and the subsequent penetration stage combined with rapid cooling. In the explosive detonation stage, the α → β phase transformation instantaneously occurred via a martensitic mechanism. In the penetration stage, the high-temperature slug in β state was cooled rapidly and showed different deformation behaviors in three different areas.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of annealing after strip casting on microstructure, precipitates and texture in non-oriented silicon steel produced by twin-roll strip casting

Highlights: • Non-oriented silicon steel with superior magnetic properties was produced by twin-roll strip casting. • The effect of annealing after strip casting on microstructure, precipitates and texture was investigated. • Role of precipitates in microstructure and texture evolution along the entire route was explored. • High magnetic induction and strong λ-fiber texture was obtained by optimizing strip annealing process. - Abstract: A 3.1 mm thick non-oriented Fe-1.0% Si steel as-cast strip was produced by twin-roll strip casting. Samples with/without strip annealing were cold rolled to 0.5 mm and then annealed. The development of microstructure, precipitate and texture was characterized along the entire processing route. It was found that annealing after strip casting had a minor influence on the average grain size and texture of the as-cast strip. A large number of particles precipitated and coarsened during the strip annealing process. Meanwhile, precipitates hindered dislocation slip and crystal rotation such that more significant in-grain shear bands were formed in cold rolled sheets. During recrystallization annealing process, the newly formed fine precipitates in directly cold-rolled sheets consumed stored strain energy and also hindered grain growth. But the initial precipitates in the annealed strip grew further and the effect of pinning of dislocations and grain boundary was lost. Therefore, annealed sheets with strip annealing process showed homogeneous equiaxed grains and the recrystallization texture was characterized by strong λ-fiber texture, which led to high permeability.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructure characterization by X-ray tomography and EBSD of porous FeCr produced by liquid metal dealloying

Highlights: • FeCr-Ni precursors were dealloyed in a Mg bath to give FeCr-Mg bicontinuous structure. • FeCr-Mg bicontinuous structure was immersed in HNO{sub 3} solution to get porous FeCr. • (FeCr){sub x}-Ni{sub 1−x} precursors are fully FCC phase while porous FeCr are fully BCC phase. • Composition & dealloying parameters are key parameters for controlling microstructure - Abstract: Liquid metal dealloying is a promising technique to get nanoporous materials which are attractive for their excellent functional properties. From a (FeCr){sub x}-Ni{sub 1−x} precursor, it is possible to get porous FeCr with this technique. While immersing precursors in a molten Mg bath, Ni atoms selectively migrate into the Mg bath. After cooling down to room temperature, the resulting microstructure is a bi-continuous structure of FeCr and Mg (with Ni in solid solution). A final etching step removes the Mg solid-state solution phase. Precursors with different compositions were dealloyed and imaged in 3D. From X-ray tomography images, porous FeCr characteristics as solid fraction, phase size, specific surface were extracted. EBSD maps were acquired on samples before and after dealloying. We will show that precursor composition is a key parameter to control pores and grains size while dealloying parameters (time and temperature) are key parameters to control ligaments size and in fine specific surface. By controlling precursor composition and dealloying parameters it is now possible to get dealloyed nanoporous metals with desired grain and porous microstructure by liquid metal dealloying.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructural evolution and electrical resistivity of nanocrystalline W thin films grown by sputtering

Highlights: • W thin films with thicknesses of 5–40 nm were deposited by sputtering and annealed up to 400°C. • Grain size of the beta (β)-W was about 5 nm, whereas that of the alpha (α)-W was about 130 nm. • Thickness dependent electrical resistivity variations as a function of annealing temperature were presented. - Abstract: Tungsten (W) thin films and nanostructures, particularly those having a beta (β)-phase, have attracted a large amount of attention lately because an ultrathin β-phase W film attached to a ferromagnetic layer can reverse the direction of magnetization upon current injection. However, in-depth microstructural studies including the phase transformation in W films as a function of thickness and post-deposition heat treatment temperature are rare. Here, we report the microstructural evolution and the change in the electrical resistivity of W films with thicknesses of 5–40 nm. Microstructural analyses indicate that the β-W is nanocrystalline with a small grain size of about 5 nm, while the alpha (α)-W has a grain size larger than 130 nm with random crystal orientation. We present a state diagram showing the phase of the W film as functions of film thickness and annealing temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2022

Local residual stresses and microstructure within recrystallizing grains in iron

The intragranular strains and the microstructure within recrystallizing grains in single phase pure iron have been systematically studied in 3D using synchrotron micro-diffraction. In contradiction to common knowledge we observe that residual elastic strains of up to 1–2 × 10 –3 are present in the recrystallizing grains. The local strain variations within individual grains can be similar in magnitude to those between different grains. The effects of processing parameters, including rolling reduction, recrystallized volume fraction, and cooling rate, as well as microstructural parameters, including grain size, orientation and internal misorientation, on the development of local residual elastic strains and microstructure have been quantified. It is suggested that the difference in local defect density between recrystallized grains and the surrounding deformed matrix, as well as the redistribution of medium to long-range residual stresses in the deformed grains, are the main reasons for the development of such strains in the recrystallized grains. The local residual stress levels are calculated and their possible impact on the mechanical properties and recrystallization processes are discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Influence of fabrication on microstructure and heat affected zone width in weldments of nuclear reactor pressure vessel steel

Advanced manufacturing routes such as electron beam welding and powder metallurgy with hot isostatic pressing are increasingly used across energy and aerospace industries, where the reliable prediction of weld behavior and heat affected zone (HAZ) evolution is critical. This study examines how fabrication routes and post-weld heat treatments influence phase distribution, crystallite size, microstrain, and dislocation density in nuclear reactor pressure vessel steels using synchrotron X-ray diffraction (SXRD). Retained austenite occurs only in samples that did not undergo austenitization, whereas an austenitizing heat treatment fully eliminates retained austenite and produces a more uniform microstructure across the weldment in terms of phase fraction, dislocation density, and microstrain. The Rosenthal solution underestimates the HAZ width for powder metallurgy samples. A newly proposed modified Rosenthal solution, reducing density by accounting for porosity, matches the SXRD-measured HAZ width with a 0.65% error. Structure–property correlations reveal that dislocation density correlates strongly with nanohardness in homogenous microstructures, while in heterogenous weldments nanohardness is further influenced by the presence of dissimilar phase boundaries. These findings provide new insight into the thermal and microstructural response of powder metallurgy fabricated steels and offer a framework for optimizing welding procedures and heat treatments in advanced manufacturing applications.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2026

Controlling homogenization length scales and microstructure in additively manufactured Ti-Ta functionally graded materials

Materials with smooth compositional gradients or functionally grade materials (FGMs) produced via additive manufacturing (AM), enables joining dissimilar materials and optimizing multiple properties in advanced engineering applications. However, as-printed AM microstructures exhibit micro-segregation and solidification defects which, when combined with controlling macroscale gradient properties, complicates necessary post-processing. Here, we use CALPHAD-informed diffusion modelling to design post-processing heat treatments for lightweight to refractory FGMs. Ti-Ta (0 to 85 at. % Ta) FGMs were fabricated using laser-based directed energy deposition AM. Post-processing heat treatments at 1000° C and 1500° C were designed to promote homogenization across specific length scales and experimentally validated. Investigation of chemical segregation and microstructures demonstrated that the length scale of homogenization is controlled as a function of time, temperature, and local composition. Ta-rich regions exhibited incomplete homogenization compared to Ti-rich layers. Unmelted Ta particles were found to completely dissolve at 1500 °C. By controlling cooling rate (200 °C/min), martensitic structures were produced between 14–36 at. % Ta, consistent with martensite-start temperatures calculations, while furnace cooling (2 °C/min) produced α+β morphologies. This work establishes a validated predictive framework for designing post-processing to tailor microstructure and chemical architecture in AM FGMs, facilitating their deployment in demanding environments.

Materials science↗