Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “electron microscope”

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 757 records · Page 42
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Micro-mechanical investigation of the thermo-mechanical properties of micro-architectured tungsten coatings

The thermo-mechanical response of micro-architectured tungsten coatings is characterized in the temperature range of 293 to 673 K using both in situ micro-compression experiments inside a scanning electron microscope (SEM) as well as image-based crystal plasticity finite element method (CPFEM) simulations. The experiments were conducted on micropillar-like specimens that were focus ion beam milled into the coatings, while the simulations were conducted on columnar-grained micropillar simulation cells constructed based on the statistics of the coating’s microstructure. The experimental results show that the stress–strain response and deformation mode exhibit a strong temperature-dependence. At room temperature, catastrophic failure is observed shortly after yield and is manifested in the form of intergranular fracture and buckling of individual columnar grains. With increasing temperature, this catastrophic failure is gradually suppressed and the material exhibits a steadier strain hardening response at 693 K. The CPFEM simulations are also shown to be in good agreement with the experimental results, and these simulations indicate that the material response is strongly influenced by the local crystallographic anisotropy and microstructure inhomogeneity. Furthermore, the simulations capture the underlying mechanisms that control the temperature-dependent transition in deformation mode. The current results highlight that the micro-architectured microstructure offers a great combination of excellent mechanical strength and structural integrity at elevated temperatures, which is of importance for high temperature applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Effect of Ni content in Cu 1-x Ni x coating on microstructure evolution and mechanical properties of W/Mo joint via low-temperature diffusion bonding

The 93W and Mo1 refractory metals were bonded with different Cu 1- x Ni x coating interlayers of various Ni content using plasma-activated sintering at 700 °C. The effects of the Ni content in the Cu 1- x Ni x coating interlayer on the interfacial microstructure evolution and mechanical properties of the W/Mo joints were studied. The maximum average shear strength of the W/Mo joint was 316.5 MPa when the Ni content of the Cu 1- x Ni x coating interlayer was 25 %. When the Ni content of the Cu 1- x Ni x coating interlayer was below 50 %, the atomic diffusion at the W/Mo joint interface was adequate without the formation of intermetallic compounds, as demonstrated by the High Resolution Transmission Electron Microscope analyses of the joints. The presence of Ni in Cu 1- x Ni x promoted diffusion bonding at the interface, which contributed to the high mechanical properties of the W/Mo joint. With an increase in the Ni content of the Cu 1- x Ni x coating interlayer, the MoNi intermetallic compound (IMC) nucleated and grew at the Cu 1- x Ni x coating/Mo1 interface. When the Ni content of the Cu 1- x Ni x coating interlayer was above 50 %, the generation of a brittle MoNi IMC weakened the shear strength of the W/Mo joint dramatically.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Experimental assessment of antimony (Sb) in pure uranium for immobilizing fission product lanthanides

The use of fuel additives is one of the concepts to mitigate fuel cladding chemical interaction (FCCI) for metallic fuel because fission product lanthanides are expected to be immobilized by the additive. Antimony (Sb) has been discovered to be a good candidate in UZr fuel. The present study focuses on its mechanism for immobilization in pure uranium, U–4Sb alloy was fabricated to understand the Sb behavior, while U–4Sb–4Ce was fabricated to simulate the case when lanthanides are generated. Both of the as-cast and annealed samples were characterized by scanning electron microscope (SEM) and energy dispersive spectrometer (EDS). U–Sb precipitates are formed in U–4Sb alloy, while U–Sb and Ce–Sb were found in U–4Sb–4Ce alloy, thermal exposure does not change the Sb-precipitation morphologies or chemical composition. Furthermore, diffusion couple tests between those alloys and cladding materials (Fe or HT9) under 650 °C for 500 h were performed and analyzed using SEM/EDS. Diffusion couple tests demonstrate the reaction between cladding and uranium, while no reaction between Sb-precipitations and cladding materials was found.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Irradiation effects on Al 0.3 CoCrFeNi and CoCrMnFeNi high-entropy alloys, and 316H stainless steel at 500 °C

To evaluate the potential of high entropy alloys (HEAs) for nuclear applications, two HEAs, Al 0.3 CoCrFeNi and CoCrFeMnNi, and a conventional Type 316H stainless steel (SS) were irradiated with 1 MeV krypton ions at 500 degrees C up to 1 dpa, and examined in-situ with a transmission electron microscope (TEM). After irradiation, a high density of ordered L1 2 nanoparticles was observed in Al 0.3 CoCrFeNi. In contrast, no phase transformation was observed in CoCrFeMnNi and 316H SS. In the thin foil regions of TEM samples, stacking-fault tetrahedra were observed in the HEAs. In the thick foil regions, interstitial dislocation loops were observed for all alloys, and the areal loop density increased linearly with foil thickness. The Al 0.3 CoCrFeNi had the largest loop size (the lowest density), followed by the CoCrFeMnNi and then the 316H SS. The higher loop nucleation rate in the 316H SS was attributed to carbon content. Finally, the degree of irradiation hardening was slightly lower for the HEAs than for the 316H SS, which is a promising sign for the nuclear application of HEAs at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Suppression of Helium Induced Cracking in Laser Repair Welding of Highly Irradiated Stainless Steels

Welding repair of irradiated nuclear reactor materials such as austenitic stainless steels used for the reactor internals has been challenging due to irradiation generated helium in the material matrix over an extended period of time. In this study, improved laser welding techniques, including the novel Auxiliary Beam Stress Improved (ABSI) technique that proactively manages the stresses during laser repair welding is investigated to substantially reduce or avoid the occurrence of intergranular helium-induced cracking (HeIC). Here, laser weld cladding, with and without ABSI technique, was applied to deposit weld metal on irradiated stainless steel (Type 304 L) blocks with various helium concentrations up to approximately 20 atomic parts per million (appm). Welded samples were cross-sectioned and analyzed using optical and electron microscopes. It was found that, with the improved laser welding techniques, no macroscopic (millimeter-sized) cracks were observed in any of the samples. Microscopic (less than 50 μm) cracks were present in the heat affected zone. Statistical analysis on the sample with the highest helium concentration (~20 appm) reveals that the ABSI technique could effectively reduce the size and amounts of microscopic cracks.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Phase stability, mechanical properties, and ion irradiation effects in face-centered cubic CrFeMnNi compositionally complex solid-solution alloys at high temperatures

We report two CrFeMnNi face-centered cubic complex concentrated solid-solution alloys (CSA) have been evaluated for phase stability, mechanical properties, and radiation damage effects from heavy ions. Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe 35 Mn 15 Ni 35 were predicted by thermodynamic calculations to phase separate and maintain a single phase at 700 °C, respectively. Aging experiments at this temperature confirmed varying degrees of precipitation of a body-centered cubic phase in both Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe 35 Mn 15 Ni 35 . The alloys showed promising strength in tensile deformation at room temperature, with yield strengths of 155 MPa and 151 MPa for Cr 18 Fe 27 Mn 27 Ni 28 and Cr 15 Fe3 5 Mn 15 Ni 35 , respectively. At 500 °C, the yield strength of Cr 18 Fe 27 Mn 27 Ni 28 fell to 93 MPa, and to 100 MPa in Cr 15 Fe3 5 Mn 15 Ni 35 . Unlike Cr 18 Fe 27 Mn 27 Ni 28 , Cr 15 Fe 35 Mn 15 Ni 35 gained some ductility at 500 °C compared to room temperature. The two CSAs were irradiated to 75 dpa at 500 °C in the plateau region of the displacement curve using 3.7 MeV Ni 2+ ions, alongside model alloy 709 as a reference. Irradiation results produced similar densities and sizes of dislocations loops in the two CSAs compared to the reference. However, while large voids form in the plateau region of Cr 18 Fe 27 Mn 27 Ni 28 , small voids form just beyond the displacement peak of Cr 15 Fe 35 Mn 15 Ni 35 . Atom probe tomography and energy dispersive X-ray spectroscopy-equipped scanning transmission electron microscopes were used to characterize the alloys for changes in chemical distribution.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

In-situ kinetic study of irradiation induced crystallization in amorphous Al 2 O 3

In the last ten years amorphous alumina coatings, deposited by Pulsed Laser Deposition, emerged as potential key enabling technology in the fields of heavy liquid metal fast reactors (lead and lead-bismuth) and fusion. In the former, as coating of the steel fuel cladding and in the latter as multifunctional coating providing a barrier against tritium permeation, steel corrosion and electrical insulation. Nevertheless, a detailed knowledge of the behavior of this thermodynamically metastable material at high temperatures and under neutron irradiation is still unknown. A knowledge gap that is mandatory to fill up for the deployment of this barrier technology. In the present work, we present a first step towards this goal, by the in-situ dynamic observation of the radiation induced crystallization processes of thin films of amorphous Al 2 O 3 , induced by ion-irradiation over an extensive range of temperatures (400-800 °C). The study was performed at the Intermediate Voltage Electron Microscope (IVEM)-Tandem Facility at Argonne National Laboratory. The experimental findings allow to elucidate the dependence of the grain growth on ion dose and temperature. A kinetic approach has been used to derive the process activation energies and other important parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Synchrotron micro-computed tomography analysis of neutron-irradiated U-Mo fuel

The three-dimensional (3D) microstructure of neutron-irradiated uranium-10 wt.% molybdenum (U-10Mo) fuel with a burn-up of 9.8 × 10 21 fissions/cm 3 was characterized using a novel, multi-modal synchrotron micro-computed tomography approach combining propagation-based phase-contrast enhanced and absorption contrast techniques. The porosity development, porosity interconnectedness, swelling, composition, local thickness of the zirconium (Zr) diffusion barrier, and the influence of the fuel–cladding interaction on the local composition and pore morphology, were uniquely determined in 3D. Two cuboids were produced using a focused ion beam-scanning electron microscope at the Zr diffusion barrier–fuel interface and in the bulk fuel. The bulk fuel sample swelled by 53.3 [+9.7/−3.1]%, while the fuel near the Zr–fuel interface swelled by 63.3 [+14.7/−7.2]%. The average local thickness of the Zr diffusion barrier decreased by 53 %, compared to the expected pre-irradiated thickness. Four pore morphology regions were identified initiating parallel to the fuel–Zr interaction region: (1) an interaction layer of suppressed porosity, (2) a layer of elongated and interconnected porosity, (3) a transition zone of low porosity, and (4) a layer of unoriented porosity representative of the bulk fuel behavior. The increase in porosity near the diffusion barrier corresponded to a higher U concentration compared to that in the bulk fuel. The interconnected porosity in the fuel near the diffusion barrier was extensive and oriented parallel to the diffusion barrier, while the bulk fuel had more compact and isolated pore networks. The interaction layer, despite having suppressed porosity, was nearly 100 wt.% U. Porosity suppression at the diffusion barrier corresponds to the expected reduction in radiation-driven diffusion of Xe at the interface despite the anticipated increase in fission product nucleation originating from a higher U concentration. In conclusion, the novel 3D insights of the porosity, swelling, and compositional variations characterized herein can improve the fidelity of fuel performance codes for proliferation-resistant fuels for research and test reactors.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
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 OSTI2022

Diatom influence on the production characteristics of hydrate-bearing sediments: Examples from Ulleung Basin, offshore South Korea

The Ulleung Basin Gas Hydrate field expeditions in 2007 (UBGH1) and 2010 (UBGH2) sought to assess the Basin's gas hydrate resource potential. Coring operations in both expeditions recovered evidence of gas hydrate, primarily as fracture-filling (or vein type) morphologies in mainly silt-sized, fine-grained sediment, but also as pore-occupying hydrate in the coarser-grained layers of interbedded sand and fine-grained systems. A commonality across many of these occurrences is the presence of diatoms in the fine-grained sediment. Here we tested fine-grained sediment (median grain size <12.5 μm) associated with hydrate occurrences at four UBGH2 sites (UBGH2-2-2, UBGH2-3, UBGH2-6 and UBGH2-11) to investigate potential impacts of diatoms on efforts to extract methane from hydrate, or to tap hydrocarbon reservoirs beneath hydrate-bearing sediment. Two key considerations are: the extent to which diatoms control sediment mechanical properties, and the extent to which pore-water freshening, which occurs as gas hydrate breaks down during resource extraction, alters the diatom control on sediment mechanical properties. We conducted experiments to measure sediment index properties, sedimentation behavior and compressibility to address these considerations. We relied on scanning electron microscope (SEM) imagery and X-ray powder diffraction (XRD) to characterize the sediment mineralogy. Our high-level findings are that at the ~20–45% (by volume) diatom concentrations observed at these UBGH2 sites, sediment compressibility increases with diatom content, but diatoms only appear to increase porosity and permeability at the highest diatom concentration (~45%). Our measurements suggest in situ compression indices of 0.35–0.55 and permeabilities on the order of 0.01milliDarcies (1 × 10 -17 m 2 ) can be anticipated at these sites. Importantly, these properties are not expected to vary significantly upon pore water freshening that accompanies gas hydrate dissociation during production.

58 GEOSCIENCES↗
DOE OSTI2021

A numerical and experimental approach to compare the effect of sample thickness in small in-situ SEM and large ex-situ tensile testing in Alloy 709

ASTM standards for tensile tests define specific sample size requirements regardless of grain size of the material. However, sample size requirements for testing should be considered in conjunction with the number of grains within its reduced cross-sectional area. This is particularly important for in-situ Scanning Electron Microscope (SEM) tensile tests, as they have to be conducted on smaller samples. In this study, a comprehensive experimental and numerical evaluation of the effect of specimen thickness (and the resulting number of grains within the cross-section) were conducted using in-situ SEM tensile test (on submillimeter thick samples) and ex-situ tensile tests (on samples of 0.68–5.9 mm thickness) and the results are compared with FEM simulations outcome. All tests were conducted at room temperature and the results are correlated to the number of grains within the thickness of specimens. The tensile test results indicated that even though the 0.2% proof stress and the tensile strength do not vary for the current range of thicknesses (with number of grains in the cross-section varying from 13 to 118), a difference in necking mechanism exists. Post tensile strength, thinner samples undergo more shear failure and diagonal localized necking whereas thicker samples experience more diffuse necking indicated by decreased area of shear failure at the edges and increased area of dimpled tensile failure at the center of the sample. Further, FEM results complement the experimental findings by showing the formation of conjugated localized shear bands on the upper and lower surface in the 0.68 mm thick sample and shear bands combining to form singular shear bands in thicker samples. These results also confirm the validity of the in-situ SEM tensile tests conducted on thinner samples as long as the required minimum number of grains exist within the cross-section.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Glassy carbon formation from pyrolysis of polymeric coatings on fiber-optic sensors

Deploying fiber-optic sensors in nuclear reactors requires a detailed understanding of radiation effects on the fiber materials and the transmitted signals. Previous work has shown large wavelength shifts in the reflected spectra obtained from polymer-coated fiber-optic temperature sensors exposed to high neutron fluences. The sensor drift resulting from these wavelength shifts cannot be explained by radiation effects on fused silica glass. These shifts are hypothesized to be caused by the conversion of the polymeric fiber coating to a glassy carbon via radiolysis and/or pyrolysis and subsequent radiation-induced compaction. Here, thermal degradation of these polymeric coatings was studied to provide insight into the potential origins of the sensor drift phenomenon. Acrylate- and polyimide-coated fibers were heated under various temperatures (250–1300 °C) and environments (oxidative and inert), and the resulting coating products were characterized via mass-loss data, scanning electron microscope imaging, and Raman spectroscopy. Results suggest that the polymer decomposition product of both coating types, at least under inert conditions, is indeed a glassy carbon. Analytical models that account for radiation-induced glassy carbon coating compaction show significant compressive fiber strains and predicted wavelength shifts that agree well with experimental measurements, providing additional evidence that supports the hypothesized origins of the sensor drift.

36 MATERIALS SCIENCE↗
DOE OSTI2023

An investigation on the structural stability of $\mathrm{ZIF}$-8 in water versus water-derived oxidative species in aqueous environment

We report the zeolitic-imidazolate-framework-8 (ZIF-8) is one of the extensively studied metal-organic frameworks (MOF) materials because of its unique structure. For its potential applicability in numerous fields, it becomes crucial to have detailed studies on the structural stability of ZIF-8, especially in aqueous environments. A number of studies have been conducted to investigate the breakdown process of the ZIF-8 structure in water; which is known as the hydrolysis of ZIF-8. However, those studies reported different opposing experimental observations on the role of water on the structural stability of ZIF-8, which created obscurity in understanding this phenomenon. This study explored the effects of different water-derived species on the structural stability of ZIF-8; specifically, examined the effects of only water and water with different oxidative species that may be generated by water molecules' dissociation under external energy or catalyst presence. To this effort, we experimentally probed the physical and chemical structural changes of ZIF-8 in DI water and three different solutions of hydrogen peroxides (H 2 O 2 ); taking H 2 O 2 as the source of oxidative species. To assess the changes in elemental compositions, chemical bonds, functional groups, crystal structure, and morphology, all the samples were analyzed by X-ray photoelectron spectroscopy (XPS), energy-dispersive x-ray (EDX) spectroscopy, Fourier Transform Infrared (FTIR) spectroscope, X-ray diffractometer (XRD), and scanning electron microscope (SEM). Significant structural changes in ZIF-8 occurred mainly in the presence of oxidative species in water. Notably, oxidative species' concentration exceeding 1 M heightened the deformation of the ZIF-8 structure.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In situ indentation and high cycle tapping deformation responses in a nanolaminate crystalline/amorphous metal composite

The incorporation of nanostructured and amorphous metals into modern applications is reliant on the understanding of deformation and failure modes in constrained conditions. To study this, a 105 nm crystalline Cu/160 nm amorphous Cu 45 Zr 55 (at.%) multilayer structure was fabricated with the two crystalline layers sputter deposited between the top-middle-bottom amorphous layers and prepared to electron transparency. The multilayer was then in situ indented either under a single load to a depth of ~ 100 nm (max load of ~ 100 μN) or held at 20 μN and then repeatedly indented with an additional 5 μN up to 20,000 cycles in a transmission electron microscope to compare the deformation responses in the nanolaminate. For the single indentation test, the multilayer showed serrated load-displacement behavior upon initial indentation inductive of shear banding. Additionally, at an indentation depth of ~ 32 nm, the multilayer exhibited perfect plastic behavior and no strain hardening. Both indented and fatigue-indented films revealed diffraction contrast changes with deformation. Subsequent Automated Crystal Orientation Mapping (ACOM) measurements confirmed and quantified global texture changes in the crystalline layers with specifically identified grains revealing rotation. Using a finite element model, the in-plane displacement vectors under the indent mapped conditions where ACOM determined grain rotation was observed, indicating the stress flow induced grain rotation. Furthermore, the single indented Cu layers also exhibited evidence of deformation induced grain growth, which was not evident in the fatigue-indented Cu based multilayer. Finally, the single indented multilayer retained a significant plastic crater in the upper most amorphous layer that directly contacted the indenter; a negligible crater impression in the same region was observed in the fatigued tested multilayer. These differences are explained by the different loading methods, applied load, and deformation mechanisms experienced in the multilayers.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Two-step deformation-induced martensitic transformation in additively manufactured High-Si stainless steel

Deformation-induced phase transformation in the additively manufactured (AM) Fe–18Cr–8Ni-5.5Si (in wt.%) alloy was analyzed using the in-situ electron backscattered diffraction (EBSD) record during uniaxial tensile testing in a scanning electron microscope (SEM). Analysis of EBSD data was focused to investigate phase transformation behavior during deformation with consideration of mechanical interactions among phases and grains in the ultrafine AM microstructure. The initial EBSD phase map illustrated that the as-built microstructure was a duplex structure consisting of major austenite (γ) and minor ferrite phases, some of which showed non-traditional orientation relationship since the rapid solidification in the AM process has produced non-equilibrium state in phase formation. In the deformed as-built AM alloy, the two-step martensitic transformation (γ→ε→α´) was identified as the main deformation-induced transformation mechanism. Martensitic transformation steps were found to be associated with glides of Shockley partial dislocations on closed packed (111) planes under the influence of atomic disturbance in the γ and ε phases, respectively. Using the closed-packed plane pole figures and unit cell orientations, their evolutions and mechanisms accompanying with the transformation were analyzed. Finally, the results indicate that one variant of ε-martensite forms from their parent γ phase, while two variants of α´ form from their parent ε phase.

36 MATERIALS SCIENCE↗
DOE OSTI2023

ZnO/CuO nanostructures anchored over Ni/Cu tubular films via pulse electrodeposition for photocatalytic and antibacterial applications

In this work, we report the fabrication of Ni and Cu tubular substrates and the synthesis of ZnO/CuO nanocomposite on them through the process of pulse electrodeposition. The systematic variation in CuO incorporation in the ZnO matrix and the processing technique were noticed to affect the structural, optical, photocatalytic, and anti-bacterial properties, which are well in accordance with the Field Emission-Scanning Electron Microscope, X-ray Diffraction, Fourier transform Infrared Spectroscopy and UV-Differential reflectance spectroscopy results. The remediation capabilities of the photocatalytic substrates were assessed through the degradation of methylene blue (MB) dye under solar irradiation. Optimized CuO incorporation within the ZnO nanorods resulted in the degradation of a 20 ppm of MB dye solution within 40 min and a higher concentration of 50 ppm within 95 min. The Ni and Cu electroformed tubes as substrates provided not only a reusable supporting frame but also a large surface-area for the growth of ZnO/CuO nanocomposite. The current study also dealt with the anti-bacterial efficacy of the above-mentioned substrates against E.coli. Hence, the Ni and Cu tubular thin film substrates with nanorods of ZnO/CuO composite were explored for the removal of organic as well as biological contaminants from waste water.

36 MATERIALS SCIENCE↗