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At least 757 records · Page 42

All sources NASA NTRS DOE OSTI

DOE OSTI2014

Coated U(Mo) Fuel: As-Fabricated Microstructures

As part of the development of low-enriched uranium fuels, fuel plates have recently been tested in the BR-2 reactor as part of the SELENIUM experiment. These fuel plates contained fuel particles with either Si or ZrN thin film coating (up to 1 µm thickness) around the U-7Mo fuel particles. In order to best understand irradiation performance, it is important to determine the starting microstructure that can be observed in as-fabricated fuel plates. To this end, detailed microstructural characterization was performed on ZrN and Si-coated U-7Mo powder in samples taken from AA6061-clad fuel plates fabricated at 500°C. Of interest was the condition of the thin film coatings after fabrication at a relatively high temperature. Both scanning electron microscopy and transmission electron microscopy were employed. The ZrN thin film coating was observed to consist of columns comprised of very fine ZrN grains. Relatively large amounts of porosity could be found in some areas of the thin film, along with an enrichment of oxygen around each of the the ZrN columns. In the case of the pure Si thin film coating sample, a (U,Mo,Al,Si) interaction layer was observed around the U-7Mo particles. Apparently, the Si reacted with the U-7Mo and Al matrix during fuel plate fabrication at 500°C to form this layer. The microstructure of the formed layer is very similar to those that form in U-7Mo versus Al-Si alloy diffusion couples annealed at higher temperatures and as-fabricated U-7Mo dispersion fuel plates with Al-Si alloy matrix fabricated at 500°C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2007

High Temperature Protonic Conductors

High Temperature Protonic Conductors (HTPC) with the perovskite structure are envisioned for electrochemical membrane applications such as H2 separation, H2 sensors and fuel cells. Successive membrane commercialization is dependent upon addressing issues with H2 permeation rate and environmental stability with CO2 and H2O. HTPC membranes are conventionally fabricated by solid-state sintering. Grain boundaries and the presence of intergranular second phases reduce the proton mobility by orders of magnitude than the bulk crystalline grain. To enhanced protonic mobility, alternative processing routes were evaluated. A laser melt modulation (LMM) process was utilized to fabricate bulk samples, while pulsed laser deposition (PLD) was utilized to fabricate thin film membranes . Sr3Ca(1+x)Nb(2-x)O9 and SrCe(1-x)Y(x)O3 bulk samples were fabricated by LMM. Thin film BaCe(0.85)Y(0.15)O3 membranes were fabricated by PLD on porous substrates. Electron microscopy with chemical mapping was done to characterize the resultant microstructures. High temperature protonic conduction was measured by impedance spectroscopy in wet air or H2 environments. The results demonstrate the advantage of thin film membranes to thick membranes but also reveal the negative impact of defects or nanoscale domains on protonic conductivity.

Dynys, Fred↗

DOE OSTI2016

Influence of annealing temperature on sensitisation behaviour and corrosion properties of an Al‐6.8 wt% Mg alloy

Influence of annealing temperature on β‐(Al 3 Mg 2 ) phase precipitation and corrosion properties of sensitised Al‐6.8 wt% Mg alloy is investigated. Sensitisation of specimens annealed at 320 °C results in IGC and SCC susceptibility. Microstructural characterization shows fine precipitation of Mg‐rich phase forming nearly continuous film at grain boundaries, despite small precipitated fraction (0.5%), and grain boundary faceting. Sensitised specimens annealed at 265 °C are IGC susceptible, but SCC resistant. Precipitation at grain boundaries is discrete, although the precipitated fraction is greater (3%) than in specimens annealed at 320 °C. Potentiodynamic measurements show that of all measured parameters, charge density is in the strongest correlation with the NAMLT and SSRT results.

Radetić, T.↗

DOE OSTI2019

Effects of Heat Treatment Parameters on the Microstructure and Properties of Bainitic Steel

The results obtained in the present study demonstrate the effects of various types of heat treatment processes on the microstructure and hardness of new trip-assisted carbide-free bainitic steel. The steel was subjected to three variants of heat treatment processing with an isothermal bainitic transformation temperature in a range from 350 to 480 °C. Changes of temperature and time of isothermal holding caused changes in the values of retained austenite (RA) volume fraction and carbon content. Reduction in the isothermal holding temperature resulted in the increased concentration of carbon in austenite. Also, the investigations of the microstructure showed that size and morphology of the austenite evolved during heat treatment. The SEM observations revealed that the steel subjected to heat treatment is composed of the carbide-free bainite with ferrite plates and a high volume fraction of retained austenite in the form of thin layers or islands. With the lower isothermal holding temperature and the higher degree of bainitic transformation, the more the RA morphology changed from island to layer type. The application of the lowest isothermal temperature resulted in a significant refinement of the microstructure components: the bainitic ferrite plates and the RA layers. Also, the mechanical properties obtained from the tensile testing and hardness measurements were correlated to the microstructure of the investigated steel after different isothermal holdings.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Morphology of cementitious material during early hydration

Morphology of hydration products, mainly calcium-silicate-hydrate (C-S-H), has a strong influence on the mechanical and transport properties of hardened cementitious materials. This paper examines the effect of curing conditions and drying methods during specimen preparation on C-S-H morphology. It shows that an appropriate drying method, either supercritical drying (SCD) or isopropanol (IPA) replacement, is able to preserve the delicate microstructure on both macro and micro scales. On the surface of the specimen, the structure is fibrillar for specimens cured in high relative humidity (RH) chamber or reticular for specimens cured in pore solution/limewater. A thin layer with cluster-like structure was found for specimens cured in high RH. By observing the fracture surface, it is found that the interior morphology is complex and varies with depth and curing methods. Consequently, one must take into account the effect of ion transport during the curing and drying when preparing specimens for microstructure analysis. We proposed that the basic units of C-S-H are fine fibers and thin sheets.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Unraveling the mysteries of the thin film composite reverse osmosis membrane

A recent article in Science by Culp, Kumar, Gomez, and colleagues introduces a new approach to characterizing reverse osmosis thin film composite membranes to provide critical insights into understanding how polymer membrane microstructure affects water permeability. Such approaches offer a degree of microstructure characterization that has up until now been unavailable to the membrane science community. Here, combined with modeling of water diffusion coefficient in the polymer membrane itself, this effort has begun to answer decades-old questions about how polyamide reverse osmosis membranes function.

McCutcheon, Jeffrey R.↗

DOE OSTI2014

Low frequency noise in the unstable contact region of Au-to-Au microcontact for microelectromechanical system switches

The noise behavior of Au-to-Au microcontact for microelectromechanical system switches has been experimentally studied in the unstable contact region. The results suggest that the electrical conduction remains nonmetallic at the initial stage during contact formation due to the existence of alien films, and traps in the alien layer located at the contact interface could play an important role in determining the conduction noise. The conduction fluctuation induced by electron trapping-detrapping associated with the hydrocarbon layer is found to be an intrinsic noise source contributing to the low frequency noise in the unstable contact region.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Changes in the Structure and Mechanical Properties of Hard Elastic and Porous Polypropylene Films upon Annealing and Orientation

The effect of the annealing temperature on the characteristics of hard elastic polypropylene samples obtained by annealing of extruded films and having an oriented lamellar structure is studied. It is established using the methods of X-ray scattering and differential scanning calorimetry that the lamellae thickness, the large period, and the degree of orientation of the folded lamellae increase with an increase in the annealing temperature, which is accompanied by an increase in the melting temperature and enthalpy. Porous films are obtained by uniaxial extension of the annealed samples in the orientation direction. It is shown that the porosity and permeability of the porous films increase with an increase in the annealing temperature, owing to an increase in the number and sizes of the through channels. The mechanical characteristics (strength, elastic modulus, and break elongation) of the hard elastic and porous films are measured, and their relationship with changes in the structure and orientation of the samples, depending on the annealing temperature, is established.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Predicted Impacts of Pt and Ionomer Distributions on Low-Pt-Loaded PEMFC Performance

Low-cost, high performance proton exchange membrane fuel cells (PEMFCs) have been difficult to develop due to limited understanding of coupled processes in the cathode catalyst layer (CCL). Low-Pt-loaded PEMFCs suffer losses beyond those predicted solely due to reduced catalyst area. Although consensus links these losses to thin ionomer films in the CCL, a precise mechanistic explanation remains elusive. In this publication, we present a physically based PEMFC model with novel structure-property relationships for thin-film Nafion, validated against PEMFC data with low Pt loading. Results suggest that flooding exacerbates kinetic limitations in low-loaded PEMFCs, shifting the Faradaic current distribution. As current density increases, protons travel further into the CCL, resulting in higher Ohmic overpotentials. We also present a parametric study of CCL design parameters. We find that graded Pt and ionomer loadings reduce Ohmic losses and flooding, but individually do not provide significant improvements. However, a dual-graded CCL (i.e., graded Pt and ionomer) is predicted to significantly improve the maximum power density and limiting current compared to uniformly loaded CCLs. This work highlights the importance of accurate transport parameters for thin-film Nafion and provides a pathway to low-cost PEMFCs via precise control of CCL microstructures.

08 HYDROGEN↗

DOE OSTI2022

Combinatorial Cu-Ni Alloy Thin-Film Catalysts for Layer Number Control in Chemical Vapor-Deposited Graphene

We synthesized a combinatorial library of CuxNi1−x alloy thin films via co-sputtering from Cu and Ni targets to catalyze graphene chemical vapor deposition. The alloy morphology, composition, and microstructure were characterized via scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), and X-ray diffraction (XRD), respectively. Subsequently, the CuxNi1−x alloy thin films were used to grow graphene in a CH4-Ar-H2 ambient at atmospheric pressure. The underlying rationale is to adjust the CuxNi1−x composition to control the graphene. Energy dispersive x-ray spectroscopy (EDS) analysis revealed that a continuous gradient of CuxNi1−x (25 at. % < x < 83 at.%) was initially achieved across the 100 mm diameter substrate (~0.9%/mm composition gradient). The XRD spectra confirmed a solid solution was realized and the face-centered cubic lattice parameter varied from ~3.52 to 3.58 A˙, consistent with the measured composition gradient, assuming Vegard’s law. Optical microscopy and Raman analysis of the graphene layers suggest single layer growth occurs with x > 69 at.%, bilayer growth dominates from 48 at.% < x < 69 at.%, and multilayer (≥3) growth occurs for x < 48 at.%, where x is the Cu concentration. Finally, a large area of bi-layer graphene was grown via a CuxNi1−x catalyst with optimized catalyst composition and growth temperature.

2D materials↗

NASA NTRS1987

High-temperature ordered intermetallic alloys II; Proceedings of the Second Symposium, Boston, MA, Dec. 2-4, 1986

The papers presented in this volume provide on overview of recent theoretical and experimental research in the field of high-temperature ordered intermetallic alloys. The papers are gouped under the following headings: ordering behavior and theory, microstructures, mechanical behavior, alloy design and microstructural control, and metallurgical properties. Specific topics discussed include antiphase domains, disordered films and the ductility of ordered alloys based on Ni3Al; kinetics and mechanics of formation of Al-Ni intermetallics; deformability improvements of L1(2)-type intermetallic compounds; B2 aluminides for high-temperature applications; and rapidly solidified binary TiAl alloys.

Stoloff, N. S.↗

DOE OSTI2014

Intrinsic stress evolution during amorphous oxide film growth on Al surfaces

The intrinsic stress evolution during formation of ultrathin amorphous oxide films on Al(111) and Al(100) surfaces by thermal oxidation at room temperature was investigated in real-time by in-situ substrate curvature measurements and detailed atomic-scale microstructural analyses. During thickening of the oxide a considerable amount of growth stresses is generated in, remarkably even amorphous, ultrathin Al{sub 2}O{sub 3} films. The surface orientation-dependent stress evolutions during O adsorption on the bare Al surfaces and during subsequent oxide-film growth can be interpreted as a result of (i) adsorption-induced surface stress changes and (ii) competing processes of free volume generation and structural relaxation, respectively.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Polyethylene Blends for Improved Oxygen Barrier: Processing-Dependent Microstructure and Gas Permeability

Here this work demonstrates a greater than expected enhancement of oxygen barrier properties in linear low-density polyethylene (LLDPE)-based materials by blending LLDPE with high-density polyethylene (HDPE). The films made by melt pressing the LLDPE/HDPE blends had a greater reduction in oxygen permeability coefficients (PO 2 ) than predicted using common permeability reduction models, i.e., the harmonic average model and zero-permeability nanofiller model. The reduction of PO 2 was attributed to the presence of spherulite crystal structures, as revealed by atomic force microscopy combined with infrared spectroscopy (AFM-IR). The LLDPE matrix exhibited significant spherulite formation even at a relatively low addition of HDPEs, which likely formed tortuous pathways for diffusing oxygen molecules. Transport results from melt-pressed films contrast with the results from films with similar compositions prepared by film blowing, which did not show barrier enhancement beyond expectation. AFM-IR revealed that the blown films lacked spherulite crystals likely due to stretching in the machine direction followed by rapid cooling. These findings demonstrate the role of processing in controlling microstructures and thus the oxygen barrier performance. This work offers the possibility of achieving easily recyclable LLDPE-based packaging materials by simple blending of polyethylenes with different crystalline content.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Elimination of columnar microstructure in N-face InAlN, lattice-matched to GaN, grown by plasma-assisted molecular beam epitaxy in the N-rich regime

The microstructure of N-face InAlN layers, lattice-matched to GaN, was investigated by scanning transmission electron microscopy and atom probe tomography. These layers were grown by plasma-assisted molecular beam epitaxy (PAMBE) in the N-rich regime. Microstructural analysis shows an absence of the lateral composition modulation that was previously observed in InAlN films grown by PAMBE. A room temperature two-dimensional electron gas (2DEG) mobility of 1100 cm{sup 2}/V s and 2DEG sheet charge density of 1.9 × 10{sup 13} cm{sup −2} was measured for N-face GaN/AlN/GaN/InAlN high-electron-mobility transistors with lattice-matched InAlN back barriers.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

A candidate accident tolerant fuel system based on a highly concentrated alloy thin film

The feasibility of depositing a thin film of highly concentrated alloy on zircaloy-4 substrates at low temperatures was investigated. Electron microscopy characterisation at micro and nanoscales showed that the deposited thin film is near-equiatomic, single-phase and with all alloying elements uniformly distributed throughout the microstructure. Heavy-ion irradiations carried out in situ within a transmission electron microscope displayed the generation of both defect clusters and inert gas bubbles at around 1.5 × 10 16 ions·cm –2 (15.4 dpa). Post-irradiation characterisation demonstrated that the thin film preserved its solid solution and that, under the studied conditions, no elemental segregation or phase transformations were observed, indicating a high radiation tolerance.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Reaction kinetics during the thermal activation of the silicon surface passivation with atomic layer deposited Al{sub 2}O{sub 3}

The excellent surface passivation of crystalline silicon provided by Al{sub 2}O{sub 3} requires always an activation by a thermal post-deposition treatment. In this work, we present an indirect study of the reaction kinetics during such thermal activation treatments for Al{sub 2}O{sub 3} synthesized by atomic layer deposition. The study was performed for Al{sub 2}O{sub 3} deposited at varying temperatures, which results in different micro-structures of the films and, in particular, different hydrogen concentrations. The effective carrier lifetime was measured sequentially as a function of the annealing time and temperature. From these data, the reaction rate R{sub act} and the activation energy E{sub A} were extracted. The results revealed a rather constant E{sub A} in the range of 1.4 to 1.5 eV, independent of the deposition temperature. The reaction rate, however, was found to increase with decreasing deposition temperature, which correlates with an increasing amount of hydrogen being incorporated in the Al{sub 2}O{sub 3} films. This is a strong indication for an interface hydrogenation that takes place during the thermal activation, which is limited by the amount of hydrogen provided by the Al{sub 2}O{sub 3} layer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Determination of the density of the defect states in Hf{sub 0.5}Zr{sub 0.5}O{sub 2} high-k film Deposited by using rf-magnetron sputtering technique

A memory structure Pt/Al{sub 2}O{sub 3}/Hf{sub 0.5}Zr{sub 0.5}O{sub 2}/Al{sub 2}O{sub 3}/p-Si was fabricated by using atomic layer deposition and rf-magnetron sputtering techniques, and its microstructure has been investigated by using the high resolution transmission electron microscopy (HRTEM). By measuring the applied gate voltage dependence of the capacitance for the memory structure, the planar density of the trapped charges in Hf{sub 0.5}Zr{sub 0.5}O{sub 2} high-k film was estimated as 6.63 × 10{sup 12} cm{sup −2}, indicating a body defect density of larger than 2.21 × 10{sup 19} cm{sup −3}. It is observed that the post-annealing in N{sub 2} can reduces the defect density in Hf{sub 0.5}Zr{sub 0.5}O{sub 2} film, which was ascribed to the occupancy of oxygen vacancies by nitrogen atoms.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Thin film combinatorial sputtering of TaTiHfZr refractory compositionally complex alloys for rapid materials discovery

Many applications from advanced nuclear reactors to aerospace and automotive industries require materials to operate in extreme environments. In search of new materials that can operate in these extremes, the present work explores this space whereby: (1) guided by atomistic and thermodynamic calculations we utilize thin film combinatorial synthesis to rapidly explore mechanical and thermal properties in a broad range of refractory compositionally complex alloys, and (2) observe transformation induced plasticity via oscillations in the thin film nanoindentation load depth curves that are attributed to, (3) a stress-induced HCP-to-BCC phase transformation in the resulting nanogranular microstructure, which to our knowledge has not been observed before in this alloy system; and finally (4) scale to bulk materials to compare the thin film results.

36 MATERIALS SCIENCE↗