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 361 records · Page 20

Application of Al-Cu-W-Ta graded density impactors in dynamic ramp compression experiments

Graded density impactors (GDIs) are utilized to dynamically compress materials to extreme conditions. Two modifications to a previously developed Mg-Cu-W GDI are made in this work before using it in a dynamic compression experiment: Mg is replaced with Al and a Ta disk is glued to the back. The Mg phase is replaced by Al because FCC Al remains solid to higher pressure along its Hugoniot compared to Mg. The addition of the Ta disk creates a constant particle velocity regime and facilitates a definition of peak pressure states. Microstructure analysis, profilometry, and ultrasonic C-scans of the Al-Cu-W GDI all confirm excellent uniformity. We evaluated signal variation in the radial direction of a dynamically compressed Al-LiF bilayer target to evaluate the contribution of spatial nonuniformity to errors. Velocity traces from five photon Doppler velocimetry (PDV) probes located at different radial distances from the center of the target varied at most by 1.1% with a root mean square of 0.3% during the compression ramp, demonstrating low PDV measurement error over a relatively large experimental area. The experimental PDV data additionally agrees well with 1D simulations that use inputs from predictive characterization models developed for the material properties resulting from tape casting, laminating, and powder consolidation processes. Low measurement error during quasi-isentropic compression, leading to better precision, promises a robust platform to reach extreme compression and low-temperature recovery states and facilitates discovery via synthesis, quenching, and preservation of new high-pressure phases.

36 MATERIALS SCIENCE↗

NiGa 2 O 4 interfacial layers in NiO/Ga 2 O 3 heterojunction diodes at high temperature

NiO/Ga 2 O 3 heterojunction diodes have attracted attention for high-power applications, but their high temperature performance and reliability remain underexplored. Here, we report the time evolution of the electrical properties in the widely studied p-NiO/n-Ga 2 O 3 heterojunction diodes and formation of NiGa 2 O 4 interfacial layers at high temperatures. Results of our thermal cycling experiment show an initial leakage current increase which stabilizes after sustained thermal load, due to reactions at the NiO–Ga 2 O 3 interface. High-resolution TEM microstructure analysis of the devices after thermal cycling indicates that the NiO–Ga 2 O 3 interface forms a ternary compound at high temperatures, and thermodynamic calculations suggest the formation of the spinel NiGa 2 O 4 layer between NiO and Ga 2 O 3 . First-principles defect calculations find that NiGa 2 O 4 shows low p-type intrinsic doping and hence can serve to limit electric field crowding at the interface. Vertical NiO/ Ga 2 O 3 diodes with intentionally grown 5 nm thin spinel-type NiGa 2 O 4 interfacial layers show an excellent device ON/OFF ratio of >10 10 (± 3 V), V ON of ~1.9 V, and increased breakdown voltage of ~1.2 kV for an initial unoptimized 300 lm diameter device. These p–n heterojunction diodes are promising for high-voltage, high temperature applications.

30 DIRECT ENERGY CONVERSION↗

Exhaust Gas Recirculation Cooler Fouling in Diesel Applications: Fundamental Studies Deposit Properties and Microstructure

This paper reports on the results of experimental efforts aimed at improving the understanding of the mechanisms and conditions at play in the fouling of EGR coolers. An experimental apparatus was constructed to utilize simplified surrogate heat exchanger tubes in lieu of full-size heat exchangers. The use of these surrogate tubes allowed removal of the tubes after exposure to engine exhaust for study of the deposit layer and its properties. The exhaust used for fouling the surrogate tubes was produced using a modern medium-duty diesel engine fueled with both ultra-low sulfur diesel and biodiesel blends. At long exposure times, no significant difference in the fouling rate was observed between fuel types and HC levels. Surface coatings for the tubes were also evaluated to determine their impact on deposit growth. No surface treatment or coating produced a reduction in the fouling rate or any evidence of deposit removal. In addition, microstructural analysis of the fouling layers was performed using optical and electron microscopy in order to better understand the deposition mechanism. The experimental results are consistent with thermophoretic deposition for deposit formation, and van der Waals attraction between the deposit surface and exhaust-borne particulate.

EGR↗

Be:B Amorphous Coatings and Order-Disorder Transitions

Here Be:B films were explored as a possible ablator material for use in inertial confinement fusion target capsules. It was found that Be:B forms an amorphous structure near the eutectic composition of 11 to 12 at. % B. It is believed that having an amorphous ablator should be useful in suppressing Rayleigh-Taylor instabilities during compression of the target. As the composition is moved away from the eutectic, an amorphous-to–columnar structure transition was more likely to be observed after some finite thickness of amorphous material had been deposited. Microstructural analysis indicated that this transition involved the nucleation of nanocrystal structures within the amorphous matrix. This nanocrystal nucleation is believed to be due to supersaturation of the dopant atom in the host. Finally, an efficient packing analysis is also presented in an effort to explain the most favorable amorphous composition of 11 to 12 at. % B doping observed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Cr-Be Pushered Single Shell (PSS) Capsule Development

Pushered single shell (PSS) has emerged as an alternative platform of implosion to ease the stability issue at the ablation front. The design consists of a thin inner Be layer, a 50% Cr:Be plateau region, an S-curve gradient, a low Cr (1.5%) tamper layer, and followed by a pure Be outer layer. General Atomics has developed a way to fabricate the higher-Z Cr to lower-Z Be gradients on glow discharge polymer mandrels with a designed S-shape profile for optimal implosion stability using magnetron sputtering. Microstructure analysis of the gradient coating indicated that at lower Cr concentration a short order or amorphous structure was formed. Here, these fabricated PSS capsules were subsequently built into capsule fill tube assemblies, verified to be leak tight at both ambient and cryogenic conditions, and delivered to Lawrence Livermore National Laboratory for the shots. The capsule thermal stability was demonstrated by invariable Cr profiles before and after pyrolysis. However, cracking at inner Cr layers was observed, which has been attributed to thermal stress.

Capsule↗

Composition-dependent apparent activation-energy and sluggish grain-growth in high entropy alloys

Experimental results reveal that the apparent activation-energy for grain-growth in an fcc-based Al x CoCrFeNi high entropy alloy (HEA) system increases from 179 to 486 kJ/mol when the Al content increases from x = 0.1 to 0.3. These unexpectedly high apparent activation-energy values can be potentially attributed to solute clustering within the fcc solid-solution phase that develops with increasing Al content in this HEA. Detailed microstructural analysis using atom-probe tomography and density functional theory (DFT) calculations strongly indicate the presence of such nanoscale clusters. This phenomenon can change grain-growth from a classical solute-drag regime to a much more sluggish cluster-drag based mechanism in these HEAs.

36 MATERIALS SCIENCE↗

Tungsten doped diamond shells for record neutron yield inertial confinement fusion experiments at the National Ignition Facility

We report on fabrication and characterization of layered, tungsten doped, spherical about 2 mm diameter microcrystalline diamond ablator shells for inertial confinement fusion (ICF) experiments at the National Ignition Facility. As previously reported, diamond ICF ablator shells can be fabricated by chemical vapor deposition (CVD) on solid spherical silicon mandrels using an ellipsoidal microwave plasma reactor. In the present work, we further developed these ablator shells by embedding a W -doped diamond layer sandwiched between two undoped diamond regions. W incorporation in diamond was achieved by adding tungsten hexacarbonyl to the CH 4 /H 2 CVD feed gas. We observe that the W doping concentration decreases with increasing deposition rate which, in turn, is controlled by adjusting the total gas pressure. Cross sectional microstructural analysis reveals sharp interfaces between doped and undoped regions of the diamond shell and uniform W distribution with concentrations up to about 0.3 at.%. At higher W concentrations (>0.3 at.%) formation of tungsten carbide precipitates is observed. Using a 3-shock 1.6 MJ laser pulse, the targets described in this work produced the first laser driven implosion to break the 1 × 10 16 neutron yield barrier, followed by experiments (described in future publications) with similar targets and slightly more laser energy producing yields as high as 4 × 10 17 .

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Synthesis of BaTiO[subscript 3]-20wt%CoFe[subscript 2]O[subscript 4] Nanocomposites via Spark Plasma Sintering

Barium titanate-20wt% cobalt ferrite (BaTiO{sub 3}-20wt%CoFe{sub 2}O{sub 4}) nanocomposites were sintered from nanocrystalline BaTiO{sub 3} and CoFe{sub 2}O{sub 4} powders using spark plasma sintering (SPS) and pressureless sintering (PS) techniques. Using SPS, dense polycrystalline composites were obtained at a sintering temperature as low as 860 C and a time of 5 min whereas PS required a higher sintering temperature (1150 C) and time (120 min) to obtain similarly dense composites. Microstructural analysis of the composites showed that both the techniques retained nanocrystalline grain sizes after sintering. High resolution X-ray diffraction measurements revealed that the BaTiO{sub 3}-20wt%CoFe{sub 2}O{sub 4} composites sintered by the SPS technique did not exhibit formation of any new phase(s) due to reaction between the BaTiO{sub 3} and CoFe{sub 2}O{sub 4} phases during sintering. However, the PS technique resulted in the formation of additional phases (other than the BaTiO{sub 3} and CoFe{sub 2}O{sub 4} phases) in the composites. While the composites synthesized by SPS were of superior phase-purity, evidence of Fe diffusion from the spinel to the perovskite phase was found from X-ray diffraction and permittivity measurements.

36 MATERIALS SCIENCE↗

Phase Relationship and Ionic Conductivity in Na–SrSiO 3 Ionic Conductor

The Na–SrSiO 3 as a potential high‐conductivity ionic conductor for intermediate temperature solid oxide electrochemical cells (SOECs) has drawn much attention recently. Some of these studies questioned the feasibility of Na doping and therefore the creation of oxygen vacancies, while others suggested an alternative phase responsible for the ionic conduction. In this study, a systematic investigation was carried out to understand the ionic conduction in Na–SrSiO 3 . Through in situ high‐temperature X‐ray diffraction, thermal analysis, microstructural characterization, and electrical conductivity measurement, Na–SrSiO 3 was shown as a two‐phase material, one being slightly Na‐doped SrSiO 3 and another being amorphous Na 2 Si 2 O 5 . The former was an electrical insulator whereas the latter was a good ionic conductor. It was also found that the amorphous Na 2 Si 2 O 5 phase was unstable at the temperature ≥500°C, crystallizing into the insulating polycrystalline Na 2 Si 2 O 5 which causes conductivity to “bend‐over” at higher temperatures. A preliminary Ab Initio Molecular Dynamics ( AIMD ) simulation suggested that the amorphous Na 2 Si 2 O 5 be predominantly a Na + conductor.

Jee, Youngseok↗

Influence of Microstructure and Surface Activation of Dual-Phase Membrane Ce 0.8 Gd 0.2 O 2-δ -FeCo 2 O 4 on Oxygen Permeation

In dual-phase oxygen transport membranes we noticed that there is fast-growing interest in research for oxyfuel combustion process application. One such potential candidate is CGO-FCO (60wt% Ce 0.8 Gd 0.2 O 2-δ -40wt% FeCo 2 O4) identified to provide good oxygen permeation flux with substantial stability in harsh atmosphere. Dense CGO-FCO membranes of 1mm thickness were fabricated by sintering dry pellets pressed from powders synthesized by one-pot method (modified Pechini process) at 1200 degrees C for 10h. Microstructure analysis indicates presence of a third orthorhombic perovskite phase in the sintered composite. We also identified that the spinel phase tends to form an oxygen deficient phase at the grain boundary of spinel and CGO phases. Surface exchange limitation of the membranes was overcome by La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF) porous layer coating over the composite. Moreover, the oxygen permeation flux of the CGO-FCO screen printed with a porous layer of 10mthick LSCF is 0.11mL/cm 2 per minute at 850 degrees C with argon as sweep and air as feed gas at the rates of 50 and 250mL/min.

36 MATERIALS SCIENCE↗

Age and growth of early‐life‐stage Atlantic tarpon ( Megalops atlanticus) from the northcentral Gulf of Mexico

Abstract Age and growth of early‐life‐stage Atlantic tarpon Megalops atlanticus collected from Mississippi coastal waters in the northcentral Gulf of Mexico (GOM) are described using otolith microstructure analysis. Tarpon leptocephali ( n = 95, 16.0—27.8 mm standard length, L S ) collected from June throughOctober 2013—2018, ranged in age from 22 to 43 days (mean = 30.9 ± 0.5 days). Leptocephalus somatic growth rates ranged 0.46—1.24 mm day −1 (mean = 0.76 ± 0.02 mm day −1 ), and leptocephalus otolith growth rates ranged 1.78—3.97 μm day −1 (mean = 2.58 ± 0.04 μm day −1 ). Growth rates were inversely correlated to leptocephalus age, indicating the shrinkage phase associated with leptocephalus metamorphosis. Juvenile tarpon ( n = 358, 50—359 mm fork length, L F ) were collected from August through December 2007—2018. Juveniles exhibited a positive allometric relationship (adjusted R 2 = 0.99, P < 0.001) between length and mass. The age of 100 juveniles (71—277 mm L F ) ranged from 76 to 174 days. Juvenile growth rate was estimated as 1.56 ± 0.11 mm day −1 . Significant ( P < 0.001) linear relationships were found between juvenile age and otolith metrics, including otolith mass ( R 2 = 0.81) and radius ( R 2 = 0.68). Evaluation of the backcalculated hatch dates suggests that specimens in the collection hatched from late May through mid‐September with slight peaks during July and August. A Rao's Spacing Test of Uniformity indicates the presence of significant lunar periodicity in leptocephalus hatch dates ( n = 95, U = 250.1, P < 0.05), with 50% of the leptocephali hatched within 5 days (before or after) of the full moon. This study fills critical gaps in the scientific knowledge of tarpon and provides estimates of early‐life‐history metrics for an iconic game fish at the northernmost extent of its GOM range.

Graham, Patrick M.↗

Investigation of Interfacial Layer for Friction Stir Scribe Welded Aluminum to Steel Joints

Friction stir scribe (FSS) welding as a recent derivative of friction stir welding has successfully fabricated a linear joint between automotive Al and steel sheets. However, there is a lack of understanding on its bonding mechanism. In this paper, the microstructures and phases at the bonding interface of FSS welded Al to ultra-high strength steel joints were studied using scanning electron microscopy and transmission electron microscopy. Based on the microstructural analysis, it is found that both mechanical and chemical bonding occurred simultaneously, and the energy-dispersive X-ray spectroscopy revealed that a thin intermetallic compound (IMC) layer was formed at the interface. Owing to the varied material flow and heat generation, the IMC layer thickness gradually decreased from the advancing side to the retreating side, and two IMCs (i.e. Fe2Al5 and Fe4Al13) were confirmed in different weld regions using diffraction pattern (or 1D fast Fourier transform pattern). Also, a Fe/Al solid solution was noticed in the IMC layer, and several Al fringes were found in the Fe-rich side in the scribe stir zone.

friction stir scribe welding, interfacial layer, i↗

Property-Graded Stainless Steel 316L by Selective Laser Melting: Characterization & Design

Abstract The purpose of this research work is to characterize and inform the design of (mechanical) property-graded bulk structures made from a single metallic alloy via a laser powder bed fusion (LPBF) process, with an end goal of creating repeatable/reproducible functionally-graded additively manufactured (FGAM) parts. This paper specifically investigates the manufacture of stainless steel (SS) 316L structures via a pulsed selective laser melting (SLM) process, and the underlying causes of property variations (within a functionally-acceptable range) through various material characterization techniques. For this, a design of experiments spanning the volumetric energy density (VED) based process parameter design space was utilized to investigate the range of functionally-acceptable physical/mechanical properties achievable in SS 316L. Five sample conditions (made via different process parameter combinations) were down-selected for in-depth microstructure analysis and mechanical/physical property characterization; these were suitably selected to impart a wide and controllable property range (209–318 HV hardness, 90–99.9% relative density, and 154–211 GPa modulus). It was observed that property variations resulted from combinations of porosity types/amounts, martensitic phase fractions, and grain sizes. Based on these findings, property-graded standard test specimens were designed and manufactured for further investigation—tensile specimens having a monotonic hardness change along its gauge length, four-point bending specimens with varying elastic moduli as a function of the distance from the neutral axis, and Moore’s rotating beam fatigue specimens with moduli variations based on the distance from the center. Altogether, this work lays the foundation for understanding and designing the local and global mechanical performance of FGAM bulk structures.

Engineering↗

Neutron Characterization of 3D Printed Gas Turbine Alloy With Internal Cooling Structure

The objective of this research work is to investigate the residual strains induced by the presence of a exit hole and internal hollow geometry present in a 3D printed IN718 similar to that seen in a gas turbine blade. The specimens were manufactured with an internal hollow structure that ended with an exit hole, and fabricated by direct metal laser sintering additive manufacturing technique. Using this technique, metal powder was melted by a laser source and rapidly cooled to form the part layer by layer. Rapid heating and cooling generate large thermal gradients and residual stresses in the 3D printed material. To be aligned with industry standards, specimens were heat-treated to relieve most of the residual stresses as well as to investigate whether IN718 still preserved a nonhomogeneous stress state after the thermal treatment. Roughness and microstructure analysis was performed to understand the heat-treated sample properties. To investigate the volumetric residual strain, the neutron diffraction technique was used with a definite neutron wavelength. Bragg’s law was used to determine lattice spacing. Interplanar lattice spacing and stress-free state lattice spacings were measured to calculate the strains. Residual strains were measured in the x and y direction to understand the impact of the presence of a exit hole and internal hollow geometry. The results of volumetric residual strain in the x and y directions showed no significant variations in the distribution of the strain due to the presence of a hollow structure as well as the exit hole. Overall, no significant stress concentration was observed in the heat treated sample. Sample geometry, instrumentation for neutron diffraction, and material properties are discussed in detail in this paper.

Raju, Nandhini↗

Compatibility of molten plutonium with wrought and additively manufactured metal crucibles

Understanding plutonium’s interaction with metals is crucial for optimizing pyrochemical operations, nuclear fuel containment, and various actinide processing techniques. Traditionally, tantalum crucibles are employed for plutonium processing due to their high durability, excellent temperature stability, and low solubility in plutonium. However, tantalum faces challenges such as plutonium wetting and diffusion, making surface coatings particularly important for crucibles in pyrochemical applications to enhance corrosion resistance against plutonium. Tantalum is also expensive and difficult to machine, prompting the need for advanced manufacturing techniques to address these challenges. Here, in this work, we investigate the interaction of Pu with tantalum and titanium crucibles fabricated using both traditional machining methods and laser powder bed fusion (LPBF) additive manufacturing (AM). LPBF-AM is an advanced technique that allows for the creation of complex geometries from traditionally difficult-to-machine metals by using a high-powered laser to build parts. Previous studies of conventional manufactured tantalum have utilized oxidation and carburization of the surface to mitigate plutonium wetting; however, no studies of surface modified LPBF-AM material have been undertaken. These studies are crucial, given the typical differences in the grain structure between conventional and LPBF-AM materials. All crucibles underwent differential scanning calorimetry to confirm the melting of plutonium. Subsequently, the crucibles were sectioned and mounted in epoxy for microstructural analysis using optical microscopy and scanning electron microscopy. This investigation, comparing the performance of wrought vs AM metal crucibles, provides a basis for future tooling applications in actinide processing techniques and can address the challenges associated with traditional machining, particularly in pyrochemical applications.

Actinides↗

Advanced Synthesis of Na 4 Si 24

The recently discovered orthorhombic allotrope of silicon, Si 24 , is an exciting prospective material for the future of solar energy due to a quasi-direct bandgap near 1.3 eV, coupled with the abundance and environmental stability of silicon. Synthesized via precursor Na 4 Si 24 at high temperature and pressure (~850 °C, 9 GPa), typical synthesis results have yielded polycrystalline samples with crystallites on the order of 20 μm. Several approaches to increase the crystal size have yielded success, including in-situ thermal spikes and refined selection of the starting materials. Microstructural analysis suggests that coherency exists between diamond silicon (d-Si) and Na 4 Si 24 . This hypothesis has led to the successful attempts at single crystal synthesis by selecting large crystals of d-Si along with metallic Na as the precursors rather than powdered and mixed precursor material. The new synthesis approach has yielded single crystals of Na 4 Si 24 greater than 100 μm. These results represent a breakthrough in synthesis that enables further characterization and utility. The promise of Si 24 for the future of solar energy generation and efficient electronics is strengthened through these advances in synthesis.

catalysis (heterogeneous)↗

Fatigue stress concentration and notch sensitivity in nanocrystalline metals

Recent studies have shown the potential for nanocrystalline metals to possess excellent fatigue resistance compared to their coarse-grained counterparts. Although the mechanical properties of nanocrystalline metals are believed to be particularly susceptible to material defects, a systematic study of the effects of geometric discontinuities on their fatigue performance has not yet been performed. In the present work, nanocrystalline Ni–40 wt%Fe containing both intrinsic and extrinsic defects were tested in tension–tension fatigue. The defects were found to dramatically reduce the fatigue resistance, which was attributed to the relatively high notch sensitivity in the nanocrystalline material. Microstructural analysis within the crack-initiation zones underneath the defects revealed cyclically-induced abnormal grain growth (AGG) as a predominant deformation and crack initiation mechanism during high-cycle fatigue. Furthermore, the onset of AGG and the ensuing fracture is likely accelerated by the stress concentrations, resulting in the reduced fatigue resistance compared to the relatively defect-free counterparts.

36 MATERIALS SCIENCE↗

Ceramographic Examinations of Irradiated AGR-1 Fuel Compacts

The AGR 1 experiment involved irradiating 72 cylindrical fuel compacts containing tri-structural isotropic (TRISO)-coated particles to a peak burnup of 19.5% fissions per initial metal atom with no in-pile failures observed out of almost 300,000 particles. Five irradiated AGR 1 fuel compacts were selected for microscopy that span a range of irradiation conditions (temperature, burnup, and fast fluence). These five compacts also included all four TRISO coating variations irradiated in the AGR experiment. The five compacts were cross-sectioned both transversely and longitudinally, mounted, ground, and polished after development of careful techniques for preserving particle structures against preparation damage. Approximately 40 to 80 particles within each cross section were exposed near enough to mid-plane for optical microscopy of kernel, buffer, and coating behavior. The microstructural analysis focused on kernel swelling and porosity, buffer densification and fracture, debonding between the buffer and inner pyrolytic carbon (IPyC) layers, and fractures in the IPyC and SiC layers. Three basic particle morphologies were established according to the extent of bonding between the buffer and IPyC layers: complete debonding along the interface (Type A), no debonding along the interface (Type B), and partial debonding (Type AB). These basic morphologies were subdivided according to whether the buffer stayed intact or fractured. The resulting six characteristic morphologies were used to classify particles within each cross section, but no spatial patterns were clearly observed in any of the cross-sectional morphology maps. Although positions of particle types appeared random within compacts, examining a total of 830 classified particles allowed other relationships among morphological types to be established.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗