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At least 973 records · Page 54
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Self-Organization and Nitrogen Incorporation in Diamond-Like Carbon Microstructures Synthesized by Nonthermal Plasma

Nonthermal plasma activation of light alkanes is an encouraging decarbonization strategy to produce chemicals or fuels from abundant and/or flared carbon sources. However, prolific carbon growth on both the catalyst and electrode has limited its practicality, requiring additional knowledge of the carbon structure and growth mechanism before breakthroughs are realized. Furthermore, visual evidence is provided for nonuniform diamond-like carbon (DLC) microstructures that materialize in a coaxial dielectric barrier discharge (DBD) reactor flowing ethane and He at 278 K. Through a connection to known behaviors of DBD microdischarge patterns, the microstructure spacing was controlled by altering the applied voltage (ΔV) of the plasma or the burning voltage (U b ). Additionally, carbon valorization through nitrogen incorporation from N 2 was explored as an orthogonal solution to carbon mitigation, with N/C values >0.25 achieved and both sp 2 and sp 3 C–N bonding observed in the microstructures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Investigation of MgO additives on microstructure and properties of thin LLZO electrolytes for all-solid-state batteries

To realize high-energy density lithium lanthanum zirconate (LLZO)-based solid-state batteries (SSB), LLZO electrolytes should be fabricated with low thickness and high mechanical strength. An effective strategy for strengthening ceramic materials is to use additives. Here, we employed MgO nanopowders and fibers as additives for the thin LLZO electrolyte in order to improve the mechanical strength. The microstructure, mechanical properties, and electrochemical properties are characterized to investigate the effects of adding MgO and sintering time. The MgO remains at grain boundaries after sintering, making the microstructure of LLZO fine and uniform. The mechanical strength of the MgO-added LLZO was enhanced by more than 60% while maintaining high ionic conductivity (1 × 10 -4 S cm -1 ) at room temperature. Li symmetric cells using the MgO fiber–LLZO and MgO powder–LLZO exhibit 2 and 3 times higher critical current density (CCD) than those of pure LLZO, and a solid-state full cell exhibits stable cycling performance. Further, these results demonstrate that the use of MgO nanopowder or fiber as an additive for thin LLZO is beneficial for high-current density cycling, by improving mechanical properties and microstructure.

25 ENERGY STORAGE↗
DOE OSTI2010

Electron Backscattered Diffraction Analysis Of Narrow Copper Interconnects In Cross-View To Investigate Scale Effect On Microstructure

In this article, we propose to use Electron Backscattered Diffraction (EBSD) to characterize microstructure of copper interconnects of thin metal level in top view and cross view. These two views give very complementary information about microstructure of copper and thus about recrystallization of copper during annealing. Moreover, for minimum width, as interconnect is two times thicker than wide; It will be easier to analyze smaller interconnect of 45 nm node technology in cross-section. We look for evolution of texture and microstructure of copper with line width in top view and in cross view. We highlight the presence of two recrystallization mechanisms and also the fact that transition from one to the other is progressive with competition of both mechanisms.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Effect of Controlled Hot Rolling Parameters on Microstructure of a Nb-Microalloyed Steel Sheet

The design of controlled rolling process of microalloyed steel sheets is affected by several factors. In this investigation, effect of the reheating, finishing and coiling temperatures of rolling, which are considered as the most effective parameters on microstructure of hot rolled products has been studied. For this purpose, seven different reheating temperatures between 1000 to 1300 deg. C with 50 deg. C increments, three different finishing temperatures of 950, 900 and 850 deg. C below the non-recrystallization temperature and one temperature of 800 deg. C in the inter critical range and four different coiling temperatures of 550, 600, 650 and 700 deg. C were chosen. By soaking the specimens in furnace, the grain coarsening temperature (T{sub gc}) is obtained about 1250 deg. C. Hence, for these kinds of steels, the reheating temperature 1200 to 1250 deg. C is recommended. Moreover, it is observed that decreasing the coiling and finishing temperatures causes more grain refinement of microstructure and the morphology is changed from polygonal ferrite to acicular one. Findings of this research provide a good connection among reheating, finishing and coiling temperatures and microstructural features of Nb-microalloyed steel sheets.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Influence of high power impulse magnetron sputtering plasma ionization on the microstructure of TiN thin films

HIPIMS (High Power Impulse Magnetron Sputtering) discharge is a new PVD technology for the deposition of high-quality thin films. The deposition flux contains a high degree of metal ionization and nitrogen dissociation. The microstructure of HIPIMS-deposited nitride films is denser compared to conventional sputter technologies. However, the mechanisms acting on the microstructure, texture and properties have not been discussed in detail so far. In this study, the growth of TiN by HIPIMS of Ti in mixed Ar and N{sub 2} atmosphere has been investigated. Varying degrees of metal ionization and nitrogen dissociation were produced by increasing the peak discharge current (I{sub d}) from 5 to 30 A. The average power was maintained constant by adjusting the frequency. Mass spectrometry measurements of the deposition flux revealed a high content of ionized film-forming species, such as Ti{sup 1+}, Ti{sup 2+} and atomic nitrogen N{sup 1+}. Ti{sup 1+} ions with energies up to 50 eV were detected during the pulse with reducing energy in the pulse-off times. Langmuir probe measurements showed that the peak plasma density during the pulse was 3 x 10{sup 16} m{sup -3}. Plasma density, and ion flux ratios of N{sup 1+}: N{sub 2}{sup 1+} and Ti{sup 1+}: Ti{sup 0} increased linearly with peak current. The ratios exceeded 1 at 30 A. TiN films deposited by HIPIMS were analyzed by X-ray diffraction, and transmission electron microscopy. At high I{sub d}, N{sup 1+}: N{sub 2}{sup 1+} > 1 and Ti{sup 1+}: Ti{sup 0} > 1 were produced; a strong 002 texture was present and column boundaries in the films were atomically tight. As I{sub d} reduced and N{sup 1+}: N{sub 2}{sup 1+} and Ti{sup 1+}: Ti{sup 0} dropped below 1, the film texture switched to strong 111 with a dense structure. At very low I{sub d}, porosity between columns developed. The effects of the significant activation of the deposition flux observed in the HIPIMS discharge on the film texture, microstructure, morphology and properties are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Texture and microstructure evolution in single-phase Ti{sub x}Ta{sub 1-x}N alloys of rocksalt structure

The mechanisms controlling the structural and morphological features (texture and microstructure) of ternary transition metal nitride thin films of the Ti{sub x}Ta{sub 1-x}N system, grown by various physical vapor deposition techniques, are reported. Films deposited by pulsed laser deposition, dual cathode magnetron sputtering, and dual ion beam sputtering have been investigated by means of x-ray diffraction in various geometries and scanning electron microscopy. We studied the effects of composition, energetic, and kinetics in the evolution of the microstructure and texture of the films. We obtain films with single and mixed texture as well as films with columnar ''zone-T'' and globular type morphology. The results have shown that the texture evolution of ternary transition metal nitrides as well as the microstructural features of such films can be well understood in the framework of the kinetic mechanisms proposed for their binary counterparts, thus giving these mechanisms a global application.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Low temperature magnetic behaviour of glass-covered magnetic microwires with gradient nanocrystalline microstructure

Slow nanocrystallization driving dynamics can be affected by the combination of two factors: sample residual stresses and sample geometry. This effect is evidenced at the initial stages of nanocrystallization of amorphous CoFeSiBCuNb magnetic microwires. Transmission electron microscopy observations indicate how crystallization at temperatures between 730 and 780 K results in a graded microstructure where the crystallization at the surface skin of the microwire, which remains almost amorphous, differs from that of the middle, where elongated grains are observed, and inner regions. However, samples annealed at higher temperatures present a homogeneous microstructure. The effect of gradient microstructure on magnetic properties has been also analyzed and a loss of bistable magnetic behaviour at low temperatures, from that obtained in the amorphous and fully nanocrystallized sample, has been observed and ascribed to changes in sign of magnetostriction for measuring temperatures below 100 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Fire performance, microstructure and thermal degradation of an epoxy based nano intumescent fire retardant coating for structural applications

Intumescent fire retardant coating (IFRC) is a passive fire protection system which swells upon heating to form expanded multi-cellular char layer that protects the substrate from fire. In this research work, IFRC’s were developed using different flame retardants such as ammonium polyphosphate, expandable graphite, melamine and boric acid. These flame retardants were bound together with the help of epoxy binder and cured together using curing agent. IFRC was then reinforced with nano magnesium oxide and nano alumina as inorganic fillers to study their effect towards fire performance, microstructure and thermal degradation. Small scale fire test was conducted to investigate the thermal insulation of coating whereas fire performance was calculated using thermal margin value. Field emission scanning electron microscopy was used to examine the microstructure of char obtained after fire test. Thermogravimetric analysis was conducted to investigate the residual weight of coating. Results showed that the performance of the coating was enhanced by reinforcement with nano size fillers as compared to non-filler based coating. Comparing both nano size magnesium oxide and nano size alumina; nano size alumina gave better fire performance with improved microstructure of char and high residual weight.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The influence of sintering temperature on microstructure and mechanical properties of Ni-Al intermetallics fabricated by SPS

In the present study PN85Yu15 was used as elemental powder to produce a sintered compound with Ni3Al as main phase. The Spark Plasma Sintering (SPS) technique is used to compact the powders. The powder was sintered in a temperature range between 1000°C and 1150°C to observe the influence of the sintering temperature on the microstructure and the mechanical properties. The microstructure was observed with optical microscope (OM), the phase composition was characterized by X-ray diffraction (XRD) technique. Density and microhardness were observed and compared the values with the results of other researchers. The compressive-, density- and microhardness tests show as clear result that with increasing the sintering temperature nearly all properties become better and also the microstructure studies show that porous places become less.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Nanoscale microstructure effects on hydrogen behavior in rapidly solidified aluminum alloys

The present work summarizes recent progress in the investigation of nanoscale microstructure effects on hydrogen behavior in rapidly solidified aluminum alloys foils produced at exceptionally high cooling rates. We focus here on the potential of modification of hydrogen desorption kinetics in respect to weak and strong trapping sites that could serve as hydrogen sinks in Al materials. It is shown that it is important to elucidate the surface microstructure of the Al alloy foils at the submicrometer scale because rapidly solidified microstructural features affect hydrogen trapping at nanostructured defects. We discuss the profound influence of solute atoms on hydrogen−lattice defect interactions in the alloys. with emphasis on role of vacancies in hydrogen evolution; both rapidly solidified pure Al and conventionally processed aluminum samples are considered.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Synthesize and microstructure characterization of Ni{sub 43}Mn{sub 41}Co{sub 5}Sn{sub 11} Heusler alloy

The ferromagnetic heusler alloys are promising materials in many technical applications due to their multifunctional properties such as shape memory effect, magnetocaloric effect, giant magnetoresistance, etc. In this work, synthesize and characterization of polycrystalline Ni{sub 43}Mn{sub 41}Co{sub 5}Sn{sub 11} (NMCS) alloy are reported. Alloy preparation was conducted by melting the constitute elements under an innert Argon (Ar) atmosphere in a vacuum mini arc-melting furnace. Homogenization of the microstructure of the as-cast ingot was obtained after annealing process at 750°C for 48 hours. It is shown that the dendrites structure has changed to equaixed grains morphology after homogenization. Microstructure characteristics of material by x-ray diffraction revealed that the alloy has a L{sub 21}-type cubic crystal structure as the main phase at room temperature. In order to induce the shape anisotropy, a forging treatment was applied to show the shape orientation of material. Various enhancements of magnetic properties in a longitudinal direction were observed at various degree of anisotropy. The microstructure changes of as-cast NMCS and effects of homogenization treatments as studied by scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS) are discussed in details.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure and composition analysis of low-Z/low-Z multilayers by combining hard and resonant soft X-ray reflectivity

Microstructure and composition analysis of periodic multilayer structure consisting of a low electron density contrast (EDC) material combination by grazing incidence hard X-ray reflectivity (GIXR), resonant soft X-ray reflectivity (RSXR), and transmission electron microscopy (TEM) are presented. Measurements of reflectivity at different energies allow combining the sensitivity of GIXR data to microstructural parameters like layer thicknesses and interfacing roughness, with the layer composition sensitivity of RSXR. These aspects are shown with an example of 10-period C/B{sub 4}C multilayer. TEM observation reveals that interfaces C on B{sub 4}C and B{sub 4}C on C are symmetric. Although GIXR provides limited structural information when EDC between layers is low, measurements using a scattering technique like GIXR with a microscopic technique like TEM improve the microstructural information of low EDC combination. The optical constants of buried layers have been derived by RSXR. The derived optical constants from the measured RSXR data suggested the presence of excess carbon into the boron carbide layer.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2019

A data-driven approach to construct a quantitative relationship between microstructural features of fatigue cracks and contact acoustic nonlinearity

This study demonstrates the feasibility of a data-driven approach to construct a quantitative relationship between nonlinear acoustic parameters and microstructural features of contact interfaces. The near-surface nonlinearity is measured using dynamic acousto-elastic testing (DAET) with a surface wave probe, while the microstructural features are extracted from scanning electron microscopy (SEM) images of fatigue cracks. Four aluminum alloy samples, each having a fatigue crack are prepared. Six local nonlinearity parameters are measured at different locations along the crack propagation direction. A total of 40 local measurements are acquired. A principal component analysis (PCA) reveals that all six nonlinearity parameters are correlated and hence can be replaced by one principal component (PC). Fifteen crack micro-geometrical features at each measurement point were extracted from the SEM images. Regression analysis is used to relate the PC of the nonlinearity parameters to the microstructural features at the crack interface. We compare three regression models that take variable selection into account: stepwise multiple linear regression (MLR), stepwise principal component regression (PCR), and least absolute shrinkage and selection operator (LASSO). Despite having different principles, the three predictive models identify two features as the most significant in predicting the interface nonlinearity: the crack aperture (opening) distribution and the distance to the crack tip. The differences between the three models and the physical interpretation of the data-driven predictions are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Pre-Irradiation Comparison of W-Based Alloys for the PHENIX Campaign: Microstructure, Composition, and Mechanical Properties

Tungsten is the material of choice as the plasma-facing material in future plasma-burning fusion reactors. During operation, plasma-facing materials will be simultaneously exposed to 14-MeV neutrons, low-energy D/He particles, and high heat loads. Neutron irradiation of tungsten results in bulk material damage, including knock-on damage causing loops and voids, and transmutation reactions leading to the transmutation of tungsten to rhenium and osmium. Under irradiation to high dose, Re and Os atoms can amalgamate into precipitates that drastically alter the material properties, noticeably increasing the hardness. However, the early-stage development of Re and Os precipitates under a fast neutron spectrum has not been investigated.In this work, the microstructure and hardening behavior of W-Re alloys containing 0 to 2.2 wt% Re, TiC-doped W, and powder-injection-molded W are investigated prior to neutron irradiation at 500ºC and 800ºC to ~0.1 displacement per atom in the High Flux Isotope Reactor (HFIR) to establish a baseline understanding of the starting microstructures.Transmission electron microscopy analysis indicates a dislocation-heavy microstructure, and scanning transmission electron microscopy–energy dispersive spectroscopy shows no spatial segregation of Re and W. Similarly, surface compositional studies performed with electron backscatter diffraction and X-ray photoelectron spectroscopy showed no presence of Re, indicating the Re did not segregate or form new phases during fabrication. Here, the alloys in their as-fabricated state showed no Re segregation or second-phase development, with no significant differences between their microstructures and Vickers hardness values.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructure-dependent rate theory model of defect segregation and phase stability in irradiated polycrystalline LiAlO 2

We report gamma lithium aluminate (LiAlO 2 ) is a breeder material for tritium and is one of key components in a tritium-producing burnable absorber rod (TPBAR). Dissolution and precipitation of second phases such as LiAl 5 O 8 and voids are observed in irradiated LiAlO 2 . Such microstructure changes cause the degradation of thermomechanical properties of LiAlO 2 and affect tritium retention and release kinetics, and hence, the TPBAR performance. In this work, a microstructure-dependent model of radiation-induced segregation (RIS) has been developed for investigating the accumulation of species and phase stability in polycrystalline LiAlO 2 structures under irradiation. Three sublattices (i.e. [Li, Al, V] I [O, V o ] II [Li i , Al i , O i , V i ] III ), and concentrations of six diffusive species (i.e. Li; vacancy of Li or Al at [Li, Al, V] I sublattice, O vacancy at [O, V o ] II sublattice, and Li, Al and O interstitials at [Li i , Al i , O i , V i ] III interstitial sublattices; are used to describe spatial and temporal distributions of defects and chemistry. Microstructure-dependent thermodynamic and kinetic properties including the generation, reaction, and chemical potentials of defects and defect mobility are taken into account in the model. The parametric studies demonstrated the capability of the developed RIS model to assess the effect of thermodynamic and kinetic properties of defects on the segregation and depletion of species in polycrystalline structures and to explain the phase stability observed in irradiated LiAlO 2 samples. The developed RIS model will be extended to study the precipitation of LiAl 5 O 8 and voids and tritium retention by integrating the phase-field method.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Reducing leakage current and enhancing polarization in multiferroic 3D super-nanocomposites by microstructure engineering

Abstract Multiferroic materials have generated great interest due to their potential as functional device materials. Nanocomposites have been increasingly used to design and generate new functionalities by pairing dissimilar ferroic materials, though the combination often introduces new complexity and challenges unforeseeable in single-phase counterparts. The recently developed approaches to fabricate 3D super-nanocomposites (3D‐sNC) open new avenues to control and enhance functional properties. In this work, we develop a new 3D‐sNC with CoFe 2 O 4 (CFO) short nanopillar arrays embedded in BaTiO 3 (BTO) film matrix via microstructure engineering by alternatively depositing BTO:CFO vertically-aligned nanocomposite layers and single-phase BTO layers. This microstructure engineering method allows encapsulating the relative conducting CFO phase by the insulating BTO phase, which suppress the leakage current and enhance the polarization. Our results demonstrate that microstructure engineering in 3D‐sNC offers a new bottom–up method of fabricating advanced nanostructures with a wide range of possible configurations for applications where the functional properties need to be systematically modified.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Synergetic effects of dual-beam implantation on the microstructural development in silicon

We report a synergy effect on the microstructural development of silicon specimens as a result of dual-beam high temperature irradiation/implantation. In situ transmission electron microscopy experiments using two different experimental setups have been used, where the primary 50 keV Co{sup +} ion implantation beam was supplemented with either a 300 keV electron beam or a 500 keV Si{sup +} ion beam. In both cases, the secondary beam intensity was such that both beams created comparable overall primary damage. Completely different microstructural response has been found in these two cases. An intensive electron irradiation was found to sharply accelerate the evolution of dislocation structure, only weakly affecting the disilicide kinetics. On the contrary, the Si ion beam weakly affected the kinetics of either dislocation loops or coherent CoSi{sub 2} precipitates, but drastically increased the number density of thermodynamically unstable semicoherent precipitates. Possible microstructural reasons for the observed effects and the implications for both dislocation loop and cobalt disilicide nucleation mechanisms in high-temperature implanted TEM samples are discussed and supported by detailed molecular dynamics calculations of annealing of cascade remnants produced by the energetic silicon recoils.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Enhanced Terahertz Emission of GaAs Microstructures

We observed the enhancement of terahertz radiation emitted from GaAs microstructures under wavelength tuned optical excitation. GaAs microstructure thin films were prepared by molecular beam epitaxy method. The peak amplitude of terahertz radiation from GaAs microstructure is more than eight times that from semi-insulating GaAs.

36 MATERIALS SCIENCE↗