Search NASA⌕ Search

SEARCH · Search NASA

Results for “microstructural analysis”

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.

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

At least 127 records · Page 7

ROADRUNNER MiniFuel Experiment: Irradiation Target Design and Sample Characterization

High-density uranium nitride (UN) is a fuel candidate for several advanced nuclear reactor designs currently under development. Because there are limited UN performance data relative to fuel fabrication impurity and density variation, an irradiation campaign has been developed as part of a collaborative effort among the University of Texas at San Antonio (UTSA), Westinghouse Electric Company, Oak Ridge National Laboratory (ORNL), and Los Alamos National Laboratory (LANL) under the Nuclear Science User Facilities program. This project, entitled ROADRUNNER, or Research On ADvancing the peRformance of UraNium Nitrides in Extreme enviRonments, aimsto support UN fuel qualification for advanced reactors by investigating the impact of density and impurity variations on UN performance as a function of irradiation temperature and burnup. The MiniFuel experiment vehicle developed by ORNL, which leverages the High Flux Isotope Reactor, was selected to perform this accelerated separate-effects irradiation testing. The experiment test matrix consists of six MiniFuel targets containing miniature UN fuel disks, and targets three distinct burnup levels (37.5, 60, and 75 MWd/kg U) and three distinct temperatures (600, 900, and 1200°C). Neutronics and thermal analyses were performed to determine the experimental parameters needed to meet the desired irradiation conditions and to predict the experiment components temperatures. UN pellets were fabricated at LANL with tightly controlled parameters to produce specimens with three distinct densities and three levels of carbon content. The pellets were then thinned down by UTSA to the experiment-required thickness. The pre-characterization of the specimens includes density measurements, carbon and oxygen contents, microstructure analysis, and x-ray computed tomography. The selected specimens will be assembled into the MiniFuel experiment, and the first ROADRUNNER MiniFuel targets are intended for HFIR insertion during the Fall of 2024. After irradiation, the targets will be shipped to ORNL’s hot cell facility for disassembly. The post-irradiation examination on the fuel specimens includes fission gas release measurements, visual inspection, fuel swelling measurements, gamma spectroscopy, and microstructure analysis. The data collected post-irradiation will be used to develop fuel performance models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Polytope Sector-Based Synthesis and Analysis of Microstructural Architectures With Tunable Thermal Conductivity and Expansion

The aim of this work is to (1) introduce an approach, called polytope sector-based synthesis (PSS), for synthesizing 2D or 3D microstructural architectures that exhibit a desired bulk-property directionality (e.g., isotropic, cubic, orthotropic, etc.), and (2) provide general analytical methods that can be used to rapidly optimize the geometric parameters of these architectures such that they achieve a desired combination of bulk thermal conductivity and thermal expansion properties. Although the methods introduced can be applied to general beam-based microstructural architectures, we demonstrate their utility in the context of an architecture that can be tuned to achieve a large range of extreme thermal expansion coefficients—positive, zero, and negative. The material-property-combination region that can be achieved by this architecture is determined within an Ashby-material-property plot of thermal expansion versus thermal conductivity using the analytical methods introduced. These methods are verified using finite-element analysis (FEA) and both 2D and 3D versions of the design have been fabricated using projection microstereolithography.

42 ENGINEERING↗

Microscopy and microstructure of Shuttle thermal protection system materials

Examples of the contribution of microstructural analysis to the development of the Space Shuttle tile insulation system are presented, with photographic examples of the scanning electron microscope (SEM) investigations. After the basic thermal protection system materials had been selected, it was neccessary to analyze the mechanical responses of the combined materials; which included: (1) the polymer strain isolation pad (SIP), (2) the room temperature-vulcanizing silicone rubber bond, (RTV), and (3) rigid ceramic fiber reusable surface insulation (RSI). Microstructural analysis was used to provide information on deformation and fracture mechanisms, load transfer mechanisms, and structural alterations occurring before final failure. Both quantitative and qualitative information was obtained in the open, three-dimensional fibrous structures of the ceramic tiles by means of novel techniques of encapsulation and dissolution.

Newquist, C. W.↗

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I3TEM) offers the unique ability to observe microstructural changes due to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. This work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO2.

Taylor, Caitlin↗

Survey of baffle plate samples, specimen machining, and hydrogen measurements

This report outlines preliminary results on the survey and characterization of irradiated baffle plate, baffle former, and flux thimble tube specimens as part of the ongoing investigation into irradiation-induced embrittlement in austenitic stainless steels at ambient (room temperature) conditions. The specimens originated from commercial pressurized water reactor (PWR) components, covering displacement damage doses ranging from approximately 0.065 to 75 dpa. Initial scanning electron microscopy (SEM) surveys revealed that specimen surfaces exhibited fine machining marks and in-service-formed oxide layers on the side surfaces of the analyzed specimens. The oxide layers revealed specific features resembling localized "pitting-like" corrosion. An additional set of specimens representing in-service oxidation is being preserved for future microstructure analysis work. As believed, this will provide additional insights into long-term material degradation in PRWs. Specimen machining challenges emerged due to a complex failure of the electric discharge machining (EDM) system located in hot area. Despite partial restoration, issues persist with the EDM’s secondary power supply, necessitating the exploration of alternative EDM or computer numerical control (CNC) machining approaches to facilitate tensile specimen preparation. Currently, low speed saw cutting is in progress to prepare specimens for hydrogen measurements and general microstructure analysis. The near-term goals include completing tensile specimen machining for advanced mechanical testing and characterizing fracture mechanisms, and stress-corrosion cracking testing, ultimately aiming to identify and mitigate the ambient-condition intergranular cracking through targeted post-irradiation annealing strategies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

3D Printed Ceramic Reinforced Polymer Composites Microstructure and Mechanical Properties

In Fused Filament Fabrication (FFF) 3D printing a part is made by extruding material layer by layer. Benefits of FFF are the ability to print complex shapes quickly and at a lower cost compared to other manufacturing methods. In this work, filaments composed of either silicon carbide (SiC) or zirconium silicate ceramic particulates in a polylactic-acid (PLA) matrix were used to print specimens for microstructural analysis and mechanical testing. Pure PLA samples were also printed and tested as a baseline for comparison. A Design of Experiments approach was used to test the interactions between three different parameters and their effect on ultimate strength, Young’s modulus, and yield strength. For compression test specimens, these parameters were infill percentage, number of shells, and print orientation angle. For tensile test specimens, the parameters were layer height, number of shells, and infill orientation angle. Pre- and post-compression test samples were evaluated by scanning electron microscopy for microstructural analysis. Infill percentage had the greatest effect on mechanical properties while number of shells and print orientation angle had minor effects. When changing the layer lines from perpendicular to parallel, relative to the loading direction, SiC-PLA had higher mechanical properties while pure PLA properties had decreased, and zirconium silicate-PLA had mix results.

Fused filament fabrication↗

Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffraction data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to the process and analysis can be made, and neutron diffraction can become a viable and efficient technique for gamma/alpha phase composition determination for nuclear fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Tensile Strength and Microstructural Characterization of Uncoated and Coated HPZ Ceramic Fibers

Tensile strengths of as-received HPZ fiber and those surface coated with BN, BN/SiC, and BN/Si3N4 have been determined at room temperature using a two-parameter Weibull distribution. Nominally approx. 0.4 micron BN and 0.2 micron SiC or Si3N4 coatings were deposited on the fibers by chemical vapor deposition using a continuous reactor. The average tensile strength of uncoated HPZ fiber was 2.0 +/- 0.56 GPa (290 +/- 81 ksi) with a Weibull modulus of 4.1. For the BN coated fibers, the average strength and the Weibull modulus increased to 2.39 +/- 0.44 GPa (346 +/- 64 ksi) and 6.5, respectively. The HPZ/BN/SiC fibers showed an average strength of 2.0 +/- 0.32 GPa (290 +/- 47 ksi) and Weibull modulus of 7.3. Average strength of the fibers having a dual BN/Si3N4 surface coating degraded to 1.15 +/- 0.26 GPa (166 +/- 38 ksi) with a Weibull modulus of 5.3. The chemical composition and thickness of the fiber coatings were determined using scanning Auger analysis. Microstructural analysis of the fibers and the coatings was carried out by scanning electron microscopy and transmission electron microscopy. A microporous silica-rich layer approx. 200 nm thick is present on the as-received HPZ fiber surface. The BN coatings on the fibers are amorphous to partly turbostratic and contaminated with carbon and oxygen. Silicon carbide coating was crystalline whereas the silicon nitride coating was amorphous. The silicon carbide and silicon nitride coatings are non-stoichiometric, non-uniform, and granular. Within a fiber tow, the fibers on the outside had thicker and more granular coatings than those on the inside.

Bansal, Narottam P.↗

Directed energy deposition of Haynes 282 nickel superalloy

Laser powder directed energy deposition was employed to fabricate Haynes® 282 Ni-based superalloy for high temperature creep testing. Material was heat treated using a single-step aging heat treatment of 800 °C for 4 h. Microstructural analysis was conducted in the as-deposited, solution-annealed, and age-hardened conditions. γ′ precipitates were absent in the as-deposited and annealed condition but formed during aging with an average size of 48.5 ± 12 nm. γ’ denuded zones ranging in thickness from 73 to 469 nm were observed adjacent to an effectively continuous grain boundary carbide film that covered 72.5% of the measured boundary length. The heat-treated material contained a high-volume fraction of TiC carbides ranging in size from 38 to 457 nm. Electron backscatter diffraction showed partial recrystallization, with 77-83% recrystallized area and a heterogeneous grain-size distribution. Creep testing at 750 °C at 300, 320, and 350 MPa revealed significantly inferior performance compared to wrought material, with higher strain rates, earlier tertiary onset, and shorter rupture lives. Fractography shows that failure was dominated by intergranular rupture. Post rupture microstructural analysis results suggest that the creep behavior was primarily governed by the non-equilibrium interface network rather than the bulk γ/γ’ matrix. In conclusion, the findings indicate that achieving wrought-like creep performance necessitates substantial improvements in the additive process, specifically focusing on enhanced homogenization, full recrystallization, and precise control over the morphology and distribution of carbides.

36 - MATERIALS SCIENCE↗

Voltage cycling as a dynamic operation mode for high temperature electrolysis solid oxide cells

Solid Oxide Electrolysis Cells (SOECs) have emerged as a promising technology for the efficient production of H2 via high-temperature electrolysis. However, power input from dynamic energy sources remains a significant challenge for their long-term stability. It is important to analyze the tolerance of cells under dynamic operation conditions. This study focuses on evaluating the impact of voltage cycling on the performance and durability of electrode-supported SOECs. We explore the operational limits and degradation mechanisms of SOECs subjected to various voltage conditions and find that the cells have high tolerance for dynamic voltage. Voltage cycling between 1.3 V and 1.5 V for 9000 cycles does not damage the cell. Conversely, cycling to higher voltages (≥1.7 V) results in accelerated degradation. Advanced characterization is used to screen for various degradation modes post operation. Within the oxygen electrode, XRD and STEM EDS find compositional and phase evolution in all voltage cycled samples including increased decomposition of the air electrode resulting in cation migration. Microstructural analysis of the fuel electrode from nano-CT data shows minimal change throughout the sample set and no evidence of Ni migration, indicating the fuel electrode is stable and not impacted by cycling to higher voltages within the timeframe studied.

Zhu, Zhikuan↗

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

Nb₃Sn has emerged as a leading alternative material due to its higher superconducting critical temperature (Tc) and superheating field (Hsh), promising a viable solution to the intrinsic performance limit currently faced by Nb superconducting radiofrequency (SRF) cavities. We sputter-coated Nb₃Sn inside Nb SRF cavity using a stoichiometric Nb₃Sn tube target in a DC cylindrical magnetron sputter coater. The target was fabricated by growing an estimated >20 μm thick Nb₃Sn layer on a Nb tube via Sn vapor diffusion using Jefferson Lab’s coating system. Approximately 150 nm thick Nb-Sn films were sputter-deposited onto flat Nb samples at positions representing the beam tubes and equator of a 2.6 GHz Nb cavity. Post-deposition annealing at 950 °C for 3 h resulted in the formation of Nb₃Sn. Microstructural analysis of the annealed films was carried out to investigate the morphology and structure of the Nb₃Sn films. Later, a 2.6 GHz Nb SRF cavity was coated with a ~1.2 μm thick sputtered Nb-Sn film using a stoichiometric Nb₃Sn target, followed by annealing. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, indicating the formation of Nb₃Sn. After a light Sn recoating treatment, the cavity achieved a quality factor (Q0) of 6.7E+08 at lower field at 2.0 K.

Accelerator Physics↗

Analysis of Microstructure and Sliding Wear Behavior of Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} High-Entropy Alloy

Α Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} high-entropy alloy (HEA) of the well-known family of CoCrFeNiTi has been designed using empirical parameters. The aim of this design was the production of a HEA with fcc structure that gives ductile behavior and also high strength because of the solid solution effect. The VEC calculations (8.1) supported the fcc structure while the δ factor calculations (4.97) not being out of the limit values, advised a significant lattice distortion. From the other hand, the ΔΗ{sub mix} calculations (− 9.64 kJ/mol) gave strong indications that no intermetallic would be formed. In order to investigate its potential application, the Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} HEA was prepared by vacuum arc melting and a primary assessment of its surface degradation response was conducted by means of sliding wear testing using different counterbody systems for a total sliding distance of 1000 m. An effort to correlate the alloy’s wear response with the microstructural characteristics was attempted. Finally, the wear behavior of the Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} HEA was compared with that of two commercially used wear-resistant alloys. The results obtained provided some first signs of the high-entropy alloys’ better wear performance when tested under sliding conditions against a steel ball.

36 MATERIALS SCIENCE↗

Fabrication, Analysis of Microstructure and Oxidation Resistance of Cemented C/C Composites by Laser

Cylindrical carbon–carbon composites have been cemented using a CO{sub 2} laser actuated by a raster scanning mirror system in a four-step sequence. Complete and homogenous surface cementation as well as thermal stability of the composites was sought after and achieved. The line of heat created from the laser beam impinged parallel to the axis of the pre-coated cylinder, while suspended from one end and slowly rotated. Four slurry compositions, all containing chloride salts from refractory elements, some combined with silicon, were pre-deposited by air spraying it over each specimen and then laser treated sequentially. Confined heat sublimed the chlorine ions resulting in silicide compounds that reacted with the carbon substrate to form a bonding layer. Microstructure characterization was performed using scanning electron microscopy, energy-dispersive spectroscopy and x-ray diffraction, immediately after the cementation was consolidated and after heat treated under argon. Preliminary oxidation weight loss tests were performed up to 1423 K under argon and air, revealing a 9.8 and 30.6% weight reduction, respectively, after 9 h of exposure. Cemented specimens were then coated with a glass overcoat layer that allowed them to perform moderately better against oxidation achieving up to a 28% weight loss after 20 h at 1273 K in air.

36 MATERIALS SCIENCE↗

Weld Quality Assessment in Fiber Laser Weldments of Ti-6Al-4V Alloy

Laser welding experiments are performed on Ti-6Al-4V alloy sheets by adopting fiber laser. A special kind of workpiece fixture is designed and fabricated for providing shielding gas. After experiments, penetration depth, fusion zone width and heat-affected zone size at different locations within weld bead are measured and discussed in detail. Influence of line energies on the formation of non-uniform microstructure within weld bead is explored by conducting microstructural analysis. Various kinds of microstructural morphology of martensitic structure such as α′ martensite, blocky α, massive α and basket-weave microstructure are found in fusion zone. Experimentally, it is found that beam power is the key parameter for controlling penetration depth. Higher hardness is noticed within fusion zone due to the existence of large volume of α′ martensite. Tensile strength and hardness of welded specimens are increased with decreasing line energy. Small amount of micropores are also found in solidified weld bead. However, its sizes are in acceptable range as per BSEN:4678 standard. Most favorable welding condition is identified as a combination of beam power of 800 W and welding speed of 1000 mm/min which yields full penetration, narrower bead width, small heat-affected zone, minimal defects and acceptable mechanical properties.

36 MATERIALS SCIENCE↗

A Comparative Analysis on Microstructure and Fracture Mechanism of X100 Pipeline Steel CGHAZ Between Laser Welding and Arc Welding

The objective of this study is to compare and contrast the differences in microstructure and fracture mechanism between CGHAZ of laser welding and submerged arc welding in X100 pipeline steel. The single-pass welding thermal simulation test of laser welding and submerged arc welding was carried out in MMS-200 thermal simulation test machine using self-made fixtures. The results indicated that the microstructure of laser welding CGHAZ and submerged arc welding CGHAZ was lath martensite and granular bainite, respectively. The impact energy of laser welding CGHAZ was 27 J, and the fracture mode was ductile fracture; the impact energy of submerged arc welding CGHAZ was 7.7 J, and the fracture mode was brittle fracture. The nucleation and propagation mechanism of cracks in different welding modes was established. Microcracks nucleated at the position of dislocation accumulation and remained austenite suppressed crack nucleation in laser welding CGHAZ. The nucleation site was at the M–A constituents in submerged arc welding CGHAZ. The main crack of laser welding CGHAZ was formed by one or a small number of microcracks. The main crack in submerged arc welding CGHAZ was formed by a large number of microcracks. The difference between crack nucleation and propagation mechanism is the reason why the impact energy of laser welding CGHAZ is higher than of submerged arc welding CGHAZ.

36 MATERIALS SCIENCE↗

Analysis of microstructural facet fatigue failure in ultra-fine grained powder metallurgy Ti-6Al-4V produced through hydrogen sintering

The hydrogen sintering and phase transformation (HSPT) process is a powder metallurgy method that produces Ti-6Al-4V with fatigue properties rivaling wrought processed Ti-6Al-4V. Previous fatigue work on HSPT Ti-6Al-4V has shown failure to be frequently caused by microstructural facets, which were believed to be grain boundary (GB) α phase. This belief conflicts with other reports as fatigue failure typically occurs across α colonies or primary α grains, not GB α. In this work, electron backscattered diffraction is used to identify these facets as GB α. Furthermore, a simple geometric model predicting the effective slip length of GB α is presented.

36 MATERIALS SCIENCE↗

Microstructure and high temperature properties of tungsten processed via electron beam melting additive manufacturing

There is considerable interest in the adoption of additive manufacturing for processing refractory metals. The layer-wise fabrication approach enables opportunities for producing complex geometries which cannot be otherwise be achieved via powder metallurgy. However, the processing science is still in its nascent stages and structure–property relations are relatively unexplored. Fundamental research is needed to further develop the technology and enable the fabrication of refractory metals for high temperature applications. Here we focus on the processing of pure tungsten using electron beam melting additive manufacturing. Experimentally we develop a suitable processing window for achieving high density crack free material. Microstructural analysis reveals that the microstructure generally consists of a columnar structure with a (111) build direction fiber preference, although, fiber switching was observed. Process induced deformation is believed to drive the formation of subgrains whose boundaries exhibit a high dislocation density. Additionally, high temperature tensile testing reveals that the material exhibits excellent properties closer to that of annealed tungsten. Significant mechanical anisotropy was observed to be present which is likely driven by strong crystallographic texture.

36 MATERIALS SCIENCE↗