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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.

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At least 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Exploring dynamic surface processes during silicate mineral (wollastonite) dissolution with liquid cell

Most liquid cell transmission electron microscopy (LC TEM) studies focus on nanoparticles or nanowires, in large part because the preparation and study of materials in this size range is straightforward. By contrast, this is not true for samples in the micrometre size range, in large part because of the difficulties associated with sample preparation starting from a ‘bulk’ material. There are also many advantages inherent to the study of micrometre-sized samples compared to their nanometre-sized counterparts. Here, we present a liquid cell transmission electron study that employed an innovative sample preparation technique using focused ion beam (FIB) milling to fabricate micrometre-sized electron transparent lamellae that were then welded to the liquid cell substrate. This technique, for which we have described in detail all of the fabrication steps, allows for samples having dimensions of several square micrometres to be observed by TEM in situ in a liquid. We applied this technique to test whether we could observe and measure in situ dissolution of a crystalline material called wollastonite, a calcium silicate mineral. More specifically, this study was used to observe and record surface dynamics associated with step and terrace edge movement, which are ultimately linked to the overall rate of dissolution. The wollastonite lamella underwent chemical reactions in pure deionized water at ambient temperature in a liquid cell with a 5-math formulam-spacer thickness. The movement of surface steps and terraces was measured periodically over a period of almost 5 h. Quite unexpectedly, the one-dimensional rates of retreat of these surface features were not constant, but changed over time. In addition, there were noticeable quantitative differences in retreat rates as a function crystallographic orientation, indicating that surface retreat is anisotropic. Several bulk rates of dissolution were also determined (1.6–4.2 • 10 -7 mol m -2 s -1 ) using the rates of retreat of representative terraces and steps, and were found to be within one order of magnitude of dissolution rates in the literature based on aqueous chemistry data.

36 MATERIALS SCIENCE↗
DOE OSTI2024

High efficiency active environmental sampling of chemical traces

A method of sample collection includes collecting an analyte from a sampling surface using a rapidly curable liquid gel comprising one or more metal particles; co-aggregating the one or more metal particles from the rapidly curable liquid gel and the analyte from the sampling surface; and rapidly curing the rapidly curable liquid gel. The composition and sample preparation conditions may facilitate improved collection efficiency of analytes during environmental and forensic evidence sampling. In addition, the composition and sample preparation conditions may facilitate enhanced detection and identification of the analyte using e.g., Surface Enhanced Raman Spectrometry (SERS).

Junghans, Ann↗
DOE OSTI2020

The sensitive surface chemistry of Co-free, Ni-rich layered oxides: identifying experimental conditions that influence characterization results

Recent studies have suggested that Co-free, Ni-rich layered cathodes (e.g., doped LiNiO2) can provide promising battery performance for practical applications. However, these layered cathodes suffer from significant surface instability during various stages of the sample history, which generates inherent challenges for achieving stable battery performance and obtaining statistically representative characterization results. To reliably report the surface chemistry of these materials, delicate controls of stepwise sample preparation are required. In this study, we aim to reveal how the surface chemistry of LiNiO2 based materials changes with various environments, including human exhalation, sample storage, sample preparation, electrochemistry cycling, and surface doping. Our results demonstrate that the surface of these materials is highly reactive and prone to alter at various stages of sample handling and characterization. The sensitive surface could impact the interpretation of the surface chemical and structural information, including surface carbonate formation, transition metal reduction and dissolution, and surface reconstruction. Importantly, the heterogeneity of the surface degradation calls for a consolidation of nanoscale, high-resolution characterization, and ensemble-averaged methods in order to improve statistical representation. Furthermore, the doping chemistry can effectively mitigate the surface degradation and improve overall battery performance due to the enhanced surface oxygen retention. Our study highlights the necessity of strict measurements through complementary characterizations at multiple length scales to eliminate unintentional biased conclusions.

surface chemistry, Co-free Ni-rich cathodes, Istab↗
DOE OSTI2018

Laser Powder Deposition Parametric Optimization and Property Development for Ti-6Al-4V Alloy

In this study, Ti6Al4V alloy was produced via laser powder deposition (LPD). To obtain Ti6Al4V alloy with maximum density, LPD parameters for preparing Ti6Al4V samples were optimized using the Taguchi method. Results were analyzed on the basis of the signal-to-noise (S/N) ratios and analyses of variance. A high energy density should be used to achieve higher levels of densification. The optimal combination of parameters for density was a scanning speed of 550 mm/min, laser power of 160 W, powder feeding rate of 0.99 g/min, and shield gas flow of 8 L/min. An almost fully dense Ti6Al4V sample was prepared using the optimized LPD process, and the relative density was greater than 99%. In addition, the microstructure and properties of Ti6Al4V samples prepared by optimized LPD process were investigated. The microstructure investigation revealed that the LPD-prepared Ti6Al4V sample was predominantly composed of fine acicular α phase and lath-type α phase. Tensile and microhardness tests indicated that the LPD sample had higher mechanical properties than the traditional cast Ti6Al4V alloy because of the acicular martensitic phase and smaller grain size.

36 MATERIALS SCIENCE↗
NASA NTRS2013

Stardust Interstellar Preliminary Examination II: Curating the Interstellar Dust Collector, Picokeystones, and Sources of Impact Tracks

We discuss the inherent difficulties that arise during "ground truth" characterization of the Stardust interstellar dust collector. The challenge of identifying contemporary interstellar dust impact tracks in aerogel is described within the context of background spacecraft secondaries and possible interplanetary dust particles and beta-meteoroids. In addition, the extraction of microscopic dust embedded in aerogel is technically challenging. Specifically, we provide a detailed description of the sample preparation techniques developed to address the unique goals and restrictions of the Interstellar Preliminary Exam. These sample preparation requirements and the scarcity of candidate interstellar impact tracks exacerbate the difficulties. We also illustrate the role of initial optical imaging with critically important examples, and summarize the overall processing of the collection to date.

Dust↗
DOE OSTI2016

Revealing the nanostructure of calcium phosphate coatings using HRTEM/FIB techniques

Herein, we report on the micro- and nanostructure of the calcium phosphate coating produced by pulsed laser deposition (PLD), using focused ion beam (FIB) lamella sample preparation and transmission electron microscopy (TEM) as the characterization technique. The initial selected area electron diffraction (SAED) data demonstrated the presence of hydroxyapatite (HA) over any other possible calcium phosphate crystalline structure and the polycrystalline nature of the coating. Moreover, the SAED analyses showed clear textured ring patterns coherent with the presence of a preferred orientation in the HA nano-crystal growth. The SAED data also indicated that the coating appears to be textured in the 〈002〉 crystalline direction. Dark-field images obtained using 002 as the working reflection showed a clear oriented crystal growth in columns, from bottom to top. These columns have a peculiar arrangement of nano-crystals since, in some cases, the preferred orientation appears to start at a certain distance from the substrate. Direct d-spacing measurements on high-resolution TEM images provided further proof of the presence of an HA nano-crystal structure. The reported data may be of interest in the future to adjust the microstructure of the HA coatings. - Highlights: •The FIB lift-out technique allows a very site-specific sample preparation method for HRTEM analysis. •It also permits a fast assessment of the HA coating thickness and elemental composition (EDS). •The coatings exhibit a nano-crystalline nature, with a texturing effect along the 002 planes. •PLD is suitable for the production of crystalline c-axis oriented hydroxyapatite coatings. •The crystalline HA phase in the PLD coating is very similar to the present in bone.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Large grain CBMM Nb ingot slices: An ideal test bed for exploring the microstructure-electromagnetic property relationships relevant to SRF

High purity (RRR > 200), large grain (> 5-10 cm) niobium ingot slices have been successfully used to fabricate radio frequency (RF) cavities for particle accelerators. They offer significantly reduced fabrication cost by eliminating processing steps and furthermore they provide the opportunity to study the influence of individual grain boundaries in SRF Nb. Here we summarize our measurements of grain boundary (GB) effects on the superconducting properties of large grain high purity niobium sheet manufactured by CBMM. We show by magneto-optical (MO) imaging that GBs allow premature flux penetration, but only when they are oriented close to the direction of the magnetic field. However, even low angle GBs produced by minor deformations commensurate with half-cell forming produce localized flux penetration. The transport properties of grain boundaries were investigated by direct transport across them and evidence for preferential vortex flow along the GBs of SRF Nb was observed for the first time. Using transmission electron microscopy (TEM) and micro crystallographic analysis with electron backscattered diffraction (EBSD), we were able to quantitatively characterize surface substructures that can lead to localized thermal breakdown of superconductivity. Important to these studies was the development of sample preparation techniques that made the cutout single, bi-crystal and tri-crystal Nb coupons as representative as possible of the surface properties of cavities manufactured by standard techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Solvent-controlled preparation and photocatalytic properties of nanostructured TiO{sub 2} thin films with different morphologies

Graphical abstract: Low-temperature growth of nanostructured TiO{sub 2} thin films was presented by a solvent-controlled method. Nanoparticle structured films in anatase phase have been successfully fabricated with some adjustment. The effects of the solvent were investigated and the formation mechanism was proposed. - Highlights: • Nanostructured TiO{sub 2} thin films with different morphologies were obtained at low temperature. • The effects of the solvent on the morphologies of the products were investigated. • The effects of the solvent on the phtocatalytic activity were investigated. - Abstract: A low-temperature growth method of nanostructured TiO{sub 2} thin films with different morphologies was reported. Rod-like, grass-like and nanosheet structured films have been successfully fabricated just by adjusting the ratio of different solvents. The effects of the solvent on the morphologies of the TiO{sub 2} nanostructures were investigated. The formation mechanism of different morphologies was proposed based on the experiment results. The as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM). The photocatalytic activity of as-prepared samples for the degradation of methylene blue (MB) in water was evaluated under UV illumination. Results showed that the solvents exhibited important effect on the morphologies and photocatalytic activity of as-prepared nanostructured titania films.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Mechanisms of material removal and mass transport in focused ion beam nanopore formation

Despite the widespread use of focused ion beam (FIB) processing as a material removal method for applications ranging from electron microscope sample preparation to nanopore processing for DNA sequencing, the basic material removal mechanisms of FIB processing are not well understood. We present the first complete atomistic simulation of high-flux FIB using large-scale parallel molecular dynamics (MD) simulations of nanopore fabrication in freestanding thin films. We focus on the root mechanisms of material removal and rearrangement and describe the role of explosive boiling in forming nanopores. FIB nanopore fabrication is typically understood to occur via sputter erosion. This can be shown to be the case in low flux systems, where individual ion impacts are sufficiently separated in time that they may be considered as independent events. But our detailed MD simulations show that in high flux FIB processing, above a threshold level at which thermal effects become significant, the primary mechanism of material removal changes to a significantly accelerated, thermally dominated process. Under these conditions, the target is heated by the ion beam faster than heat is conducted away by the material, leading quickly to melting, and then continued heating to nearly the material critical temperature. This leads to explosive boiling of the target material with spontaneous bubble formation and coalescence. Mass is rapidly rearranged at the atomistic scale, and material removal occurs orders of magnitude faster than would occur by simple sputtering. While the phenomenology is demonstrated computationally in silicon, it can be expected to occur at lower beam fluxes in other cases where thermal conduction is suppressed due to material properties, geometry, or ambient thermal conditions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

A versatile and low-cost chip-to-world interface: enabling ICP-MS characterization of isotachophoretically separated lanthanides on a microfluidic device

Microfluidics offer novel and state-of-the-art pathways to process materials. Microfluidic systems drastically reduce timeframes and costs associated with traditional lab-scale efforts in the area of analytical sample preparations. The challenge arises in effectively connecting microfluidics to off-chip analysis tools to accurately characterize samples after treatment on-chip. Here, a fused silica microfluidic device (MFD) is connected to a fused-silica capillary in order to create a world-to-chip connection between the MFD and an inductively coupled plasma mass spectrometer (ICP-MS). Specifically, this is demonstrated by utilizing isotachophoresis (ITP) on a microfluidic chip to separate samples containing up to 14 lanthanides into elementally pure bands. The separated sample is successfully transferred across a 7 nL dead space at the microchip-capillary junction, such that separation resolution is maintained and even increased through the interface and into the ICP-MS, where the elemental composition of the separated sample is analysed. Lanthanide samples of varying composition are detected using ICP-MS, demonstrating this versatile and cost-effective approach that does not degrade the separation quality achieved on the MFD. This simple and inexpensive connection enables fast, low-cost sample preparation immediately prior to injection into an ICP-MS or other analytical instruments.

Lackey, Hope E.↗
DOE OSTI2015

Thermal-history dependent magnetoelastic transition in (Mn,Fe){sub 2}(P,Si)

The thermal-history dependence of the magnetoelastic transition in (Mn,Fe){sub 2}(P,Si) compounds has been investigated using high-resolution neutron diffraction. As-prepared samples display a large difference in paramagnetic-ferromagnetic (PM-FM) transition temperature compared to cycled samples. The initial metastable state transforms into a lower-energy stable state when the as-prepared sample crosses the PM-FM transition for the first time. This additional transformation is irreversible around the transition temperature and increases the energy barrier which needs to be overcome through the PM-FM transition. Consequently, the transition temperature on first cooling is found to be lower than on subsequent cycles characterizing the so-called “virgin effect.” High-temperature annealing can restore the cycled sample to the high-temperature metastable state, which leads to the recovery of the virgin effect. A model is proposed to interpret the formation and recovery of the virgin effect.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2019

Electron backscatter diffraction of Nb 3 Sn coated niobium: Revealing structure as a function of depth

Over the last two decades, advances in Electron Backscatter Diffraction (EBSD) have moved the technique from a research tool to an essential characterization technique in many fields of material research. EBSD is the best suited technique for determining structure as a function of depth. This characterization is critically important, but has been previously absent from Nb 3 Sn efforts. While EBSD is the technique of choice, obtaining quality data can be difficult. Sample preparation in particular is non-trivial. Here we summarize the general principles of EBSD, discuss specific sample preparation techniques for Nb 3 Sn coated SRF cavity material, and give examples of how EBSD is being used to understand fundamental growth mechanisms for Nb 3 Sn coatings.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Facile Template-Free Fabrication of the hollow sea cucumber-like TbF{sub 3} and luminescent properties

Graphical abstract: Hollow sea cucumber-like TbF{sub 3} has been prepared via a facile hydrothermal route. The possible growth mechanism and the luminescent properties of the as-prepared sample have been discussed. - Highlights: • TbF3 particles were prepared by a facile hydrothermal route. • TbF3 product show strong green emission. • This method may be more widely applicable in the design of other rare-earth compounds. - Abstract: Hollow sea cucumber-like TbF{sub 3} was successfully fabricated by a self-assembled hydrothermal method. The crystal structure, morphology and photoluminescence properties of the as-prepared TbF{sub 3} crystals were investigated. The results revealed that the as-prepared TbF{sub 3} sample has orthorhombic structure and composed of monodispersed 3D hollow sea cucumber-like particles. The possible formation mechanism for sea cucumber-like TbF{sub 3} is presented in detail. Additionally, the as-prepared sample possesses property of down-conversion photoluminescence. The excitation spectrum of TbF{sub 3} sample was obtained by monitoring the emission of Tb{sup 3+} at 545 nm was composed of the characteristics f–f transition lines within the Tb{sup 3+} 4f{sup 8} configuration. Under the UV light irradiation, the emission spectrum exhibited four obvious lines centered at 491, 545, 588, and 620 nm, which was corresponding to the {sup 5}D{sub 4} → {sup 7}F{sub J} (J = 6, 5, 4, 3) transitions of the Tb{sup 3+} ions in the TbF{sub 3} nanoparticles.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Electrical, Structural, and Thermal Properties of Ferrite/Superconductor (Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}){sub x}/YBa{sub 2}Cu{sub 3}O{sub 7-δ}) Nanocomposite Materials

The superconductor YBa{sub 2}Cu{sub 3}O{sub 7-δ} (Y123) is prepared by the solid-state route, while the nanosized Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} (Ni-Zn ferrite) is synthesized via citric acid sol-gel technique. The composite material of the type (Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}){sub x}/YBa{sub 2}Cu{sub 3}O{sub 7-δ}, where x = 0.00, 0.03, 0.10, and 0.50 wt%, is prepared by a modified solid-state method to study the effect of doping Ni-Zn nanosized ferrite on the superconducting, structure, and thermal properties of Y123. The prepared samples show Meissner effect which confirmed the presence of superconducting phase at liquid nitrogen temperature (77 K). The prepared samples have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion of X-ray (EDX), infra-red (IR) spectroscopy, thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), DC resistance by four-probe, and critical current density measurements. It was found that by increasing Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} nanoparticles in the Y123 compound, the unit cell volume of the orthorhombic phase decreases, but the transition temperature T{sub c} and critical current density J{sub c} decrease for low doping (x = 0.03 wt%) then increase (x = 0.10 and 0.50 wt%) for Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} doped in Y123. The transport properties of the (Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}){sub x}/YBa{sub 2}Cu{sub 3}O{sub 7}-{sub δ} composite as electrical resistance R, T{sub c}, and J{sub c} are interpreted according to Bean’s critical state model and charge-vortex interaction combined with vortex pinning in Y123 high-T{sub c} mixed-state type-II superconductor. Highlights: The critical current density J{sub c} decreased for low doping of nanosized Ni-Zn ferrite into Y123 with ratio of 0.03 wt% and increased by increasing doping ratio to 0.50 wt%. The physical properties are improved by the coexistence of the superconductor Y123 and nanosized Ni-Zn ferrites in nanocomposite material.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2023

Rapid in situ nutrient element distribution in plants and soils using laser-induced breakdown spectroscopy ($\mathrm{LIBS}$)

The aim of this study is to develop and test the applicability of a rapid in situ plant chemistry profiling technique to determine elemental composition of small-volume plant and soil samples obtained from a woody bioenergy crop species, Populus trichocarpa. Expanding the research tools available to characterize the nutrient element correlations among plant tissue types and soil depths is a critical need in the path of understanding productivity and adaptation of plants to variations in external abiotic and biotic factors and developing sustainable perennial bioenergy crops that are co-optimized for biomass valorization aboveground and carbon sequestration belowground. Several plant root, stem, and soil samples were tested using laser-induced breakdown spectroscopy (LIBS) to evaluate the presence and distribution of nutrient elements. Samples were tested as collected and after being dried and cross sectioned to evaluate the effectiveness of using LIBS for in situ analysis on plant samples. The collected LIBS spectra show the elemental peaks were the same in both the as collected and prepared samples for roots and stems. Qualitative amounts of elements such as H, C, N, O, Li, Na, Mg, K, Ca, Fe, Al, and Si were able to be identified rapidly in raw samples. Here in this report we demonstrate suitability of LIBS in obtaining rapid, in situ, elemental distribution in plant and soil samples, utilizing only small sample volumes and minimal sample preparation. This demonstration opens up a new rapid phenotyping avenue necessary to fill the asymmetrical knowledge gaps in belowground performance of plant systems.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Strategies for preparing and analyzing thin passive films with atom probe tomography

Atom probe tomography provides a unique, three-dimensional map of elemental and isotopic distributions over a wide range of materials with near-atomic scale resolution and is particularly strong at analyzing buried interfaces within materials. However, it is much more difficult to apply atom probe to the analysis of nanoscale surface films, such as those formed during alloy passivation, where unique challenges persist for sample preparation and data collection. Here, we present sample preparation strategies involving the deposition of a < 100 nm capping layer that enables reliable characterization of thin passive films approximately 2–5 nm thick formed on binary and multi-principal element alloys via atom probe tomography. Several capping layer materials (Pt, Ti, Ni/Cr bi-layer) and deposition methods are contrasted. Our results indicate a sputtered Ni/Cr bi-layer enables the characterization of the entire passive film and concentration profiles that can easily be interpreted to clearly distinguish base alloy/passive film/capping layer interfaces. Lastly, we highlight ongoing challenges and opportunities for this experimental approach.

Kautz, Elizabeth J. [University of Florida]↗
DOE OSTI2018

Comparison of the Physicochemical and Electrochemical Properties of Vanadium Oxide-Based Nanomaterials Prepared by Cryochemical Synthesis and Supercritical Drying Technique

Vanadium oxide-based nanomaterials have been prepared by cryochemical synthesis (CCS) and supercritical drying (SCD) in n-hexane and acetone. We have performed the first comparative analysis which demonstrates differences in the physicochemical and electrochemical properties of the products, related to the key features of the effect of the CCS and SCD approaches. The nanomaterials prepared from the same precursor using CCS and SCD (in acetone and n-hexane) have been shown to differ in phase composition and morphology. The oxidizing annealing of the resultant aerogels and cryogel at 500°C in air leads to the formation of only one phase: α-V{sub 2}O{sub 5}. In all cases except the aerogel prepared using SCD in n-hexane, the crystalline α-V{sub 2}O{sub 5} has a higher discharge capacity in comparison with the unannealed aerogels and cryogel. The highest discharge capacity among the annealed aerogels is offered by the sample prepared using SCD in acetone (255 mAh/g), and the highest discharge capacity among the unannealed materials is offered by the sample prepared using SCD in n-hexane (280 mAh/g). The samples range in energy density from 110 to 640 Wh/kg. The highest energy density is also offered by the aerogel prepared using SCD in n-hexane.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study of magneto-optical characteristics of cerium incorporated yttrium iron garnet films

Highlights: • Ce:YIG films deposited by sol–gel method. • XRD results shows crystallite size of films decreases by Ce concentrations. • Morphological studies indicate of smooth and connected surface for all films. • Ce ions increased Faraday rotation of YIG films. - Abstract: In the current study, yttrium iron garnet films incorporated with cerium with the general formula of Ce{sub x}Y{sub 3-x}Fe{sub 5}O{sub 12} and values of (x = 0, 0.1, 0.3, 0.5, 0.7) were prepared through sol–gel method using spin coating technique and heating treatment on quartz substrates. Prepared samples were studied to check physical characteristics. X-ray diffraction analysis (XRD), scanning electron microscope (SEM), atomic force microscope (AFM) and vibrating sample magnetometer (VSM) were applied to study the impact of Ce impurities on the structural characteristic, surface morphology of films and magnetic properties, respectively. Faraday rotation values of samples were measured at the wavelength of 632 nm. The image of the atomic force microscope (AFM) of the prepared samples shows that the films have a continuous and smooth surface.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗