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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 937 records · Page 52
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Structure of thermoelectric films of higher manganese silicide on silicon according to electron microscopy data

The structural features of higher manganese-silicide films obtained by the diffusion doping of single-crystal silicon substrates with manganese vapor in a sealed cell and a flow-through quartz reactor with continuous pumping are comparatively analyzed. Scanning electron microscopy and high-resolution transmission electron microscopy show that a single-phase textured film of higher manganese silicide is formed in the evacuated cell. A change in the growth conditions from steady (cell) to quasi-steady-state (reactor) leads to the formation of polycrystalline islands of higher manganese silicide with nanoscale inclusions of the manganese- monosilicide phase.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Surface chemistry of a Cu(I) beta-diketonate precursor and the atomic layer deposition of Cu{sub 2}O on SiO{sub 2} studied by x-ray photoelectron spectroscopy

The surface chemistry of the bis(tri-n-butylphosphane) copper(I) acetylacetonate, [({sup n}Bu{sub 3}P){sub 2}Cu(acac)] and the thermal atomic layer deposition (ALD) of Cu{sub 2}O using this Cu precursor as reactant and wet oxygen as coreactant on SiO{sub 2} substrates are studied by in-situ x-ray photoelectron spectroscopy (XPS). The Cu precursor was evaporated and exposed to the substrates kept at temperatures between 22 °C and 300 °C. The measured phosphorus and carbon concentration on the substrates indicated that most of the [{sup n}Bu{sub 3}P] ligands were released either in the gas phase or during adsorption. No disproportionation was observed for the Cu precursor in the temperature range between 22 °C and 145 °C. However, disproportionation of the Cu precursor was observed at 200 °C, since C/Cu concentration ratio decreased and substantial amounts of metallic Cu were present on the substrate. The amount of metallic Cu increased, when the substrate was kept at 300 °C, indicating stronger disproportionation of the Cu precursor. Hence, the upper limit for the ALD of Cu{sub 2}O from this precursor lies in the temperature range between 145 °C and 200 °C, as the precursor must not alter its chemical and physical state after chemisorption on the substrate. Five hundred ALD cycles with the probed Cu precursor and wet O{sub 2} as coreactant were carried out on SiO{sub 2} at 145 °C. After ALD, in-situ XPS analysis confirmed the presence of Cu{sub 2}O on the substrate. Ex-situ spectroscopic ellipsometry indicated an average film thickness of 2.5 nm of Cu{sub 2}O deposited with a growth per cycle of 0.05 Å/cycle. Scanning electron microscopy and atomic force microscopy (AFM) investigations depicted a homogeneous, fine, and granular morphology of the Cu{sub 2}O ALD film on SiO{sub 2}. AFM investigations suggest that the deposited Cu{sub 2}O film is continuous on the SiO{sub 2} substrate.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Martensitic Transformation and Magnetic Properties of the CuAl, CuAlMn, and CuAlMnZn Alloys

In the present work, the effect of alloying elements on the phase transformation which are formed by cooling effect in CuAl, CuAlMn, and CuAlMnZn (wt%) alloys are investigated using scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM) characterization techniques. From SEM observations, the martensite formation with different morphologies is observed in these alloys. But the results of the scanning electron microscope investigations presented in this work have not formed the precipitates in the CuAl alloy with Mn or Zn additions. We found that magnetic saturation and coercivity values decreased with the addition of Mn and Zn elements to the CuAl alloy. The findings confirmed the variation in magnetic properties, which occurred in the result of adding different alloying elements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Properties of Cu(In,Ga,Al)Se{sub 2} thin films fabricated by magnetron sputtering

Cu(In,Ga,Al)Se{sub 2} (CIGAS) thin films were studied as an alternative absorber layer material to Cu(In{sub x}Ga{sub 1−x})Se{sub 2}. CIGAS thin films with varying Al content were prepared by magnetron sputtering on Si(100) and soda-lime glass substrates at 350 °C, followed by postdeposition annealing at 520 °C for 5 h in vacuum. The film composition was measured by an electron probe microanalyzer while the elemental depth profiles were determined by secondary ion mass spectrometry. X-ray diffraction studies indicated that CIGAS films are single phase with chalcopyrite structure and that the (112) peak clearly shifts to higher 2θ values with increasing Al content. Scanning electron microscopy images revealed dense and well-defined grains, as well as sharp CIGAS/Si(100) interfaces for all films. Atomic force microscopy analysis indicated that the roughness of CIGAS films decreases with increasing Al content. The bandgap of CIGAS films was determined from the optical transmittance and reflectance spectra and was found to increase as Al content increased.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Experimental and Numerical Investigations of Cyclic Plastic Deformation of Al-Mg Alloy

In this work, low-cycle fatigue (LCF) tests are performed on as-received and solution-treated Al-Mg alloy (AA 5754). Solution heat treatment of the as-received alloy is performed at 530 °C for 2 h and then quenched in water at room temperature. The low-cycle fatigue response of the as-received and solution-treated alloy is evaluated at five different strain amplitudes from 0.2 to 0.6%. The strain rate of 0.5 × 10{sup −3} s{sup −1} is kept constant in all the LCF tests. The LCF behavior of AA 5754 is modeled by finite element method (FEM) using Chaboche kinematic hardening cyclic plasticity model. Hardening behavior or fatigue life of as-received and solution-treated alloy is successfully simulated using this model. The results obtained by FEM simulations are compared with those obtained by LCF experiments. Microstructural studies are also performed for as-received and solution-treated alloy. The fracture surfaces obtained from LCF tests are analyzed by scanning electron microscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Mechanical and morphological properties of kenaf powder filled natural rubber latex foam

This research is carried out by incorporate kenaf powder with natural rubber latex (NRL) compound and is foamed to make natural rubber latex foam (NRLF) by using a well known technique called Dunlop method. Different loading of kenaf powder was added to NRL compound and was foamed to make NRLF. The tensile properties, and morphology of kenaf filled NRLF was studied. Increase in kenaf loading reduced the tensile strength and elongation at break and of a compound. Modulus at 100% elongation of the compound increased with increased in filler loading. The morphological and micro structural characterization has been performed by using scanning electron microscopy (SEM)

36 MATERIALS SCIENCE↗
DOE OSTI2015

Investigations on Ni-Co-Mn-Sn thin films: Effect of substrate temperature and Ar gas pressure on the martensitic transformations and exchange bias properties

We report the effect of substrate temperature (T{sub S}) and Ar gas pressure (P{sub D}) on the martensitic transformations, magnetic and exchange bias (EB) properties in Heusler type Ni-Co-Mn-Sn epitaxial thin films. Martensitic transformation temperatures and EB fields at 5 K were found to increase with increasing T{sub S}. The observed maximum EB value of 320 Oe after field cooling in the film deposited at 650 {sup ∘}C is high among the values reported for Ni-Mn-Sn thin films which is attributed to the coexistence of ferromagnetic (FM) and antiferromagnetic (AF) phases in the martensitic state. In the case of P{sub D} variation, with increase in P{sub D}, martensitic transformation temperatures were increased and a sharp transformation was observed in the film deposited at 0.06 mbar. Magnetization values at 5 K were higher for increasing P{sub D}. These observations are attributed to the compositional shift. EB effect is also present in these films. Microstructural features observed using atomic force microscopy (AFM) shows a fine twinning and reduced precipitation with increase in P{sub D}, which is also confirmed from the scanning electron microscopy (SEM) images. EB effects in both series were confirmed from the training effect. Target ageing effect has been observed in the films deposited before and after ninety days of time interval. This has been confirmed both on substrate temperature and Ar gas pressure variations.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Ferromagnetic-to-Paramagnetic Phase Transition of MnAs Studied by Calorimetry and Magnetic Measurements

Manganese monoarsenide samples have been prepared by the sealed-ampule technique and characterized by X-ray diffraction, differential thermal analysis, and scanning electron microscopy. The hexagonal- to-orthorhombic phase transition of MnAs has been studied using differential scanning calorimetry (DSC) and magnetic measurements. The enthalpy and temperature range of the transition have been determined to be ΔH =–5.6 J/g and 312.5–319 K, respectively. The enthalpy and temperature range of the transition are influenced by the quality of the samples. The samples containing inclusions of the metastable, orthorhombic phase have a lower enthalpy and broader temperature range of the magnetostructural transformation of manganese monoarsenide. It has been demonstrated that DSC is an effective tool for assessing the quality of MnAs samples. Temperature dependences of specific magnetization and magnetic permeability for MnAs lend support to the DSC results. From these data, the Curie temperature of MnAs has been determined to be 40°C, in good agreement with previously reported data.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of surface pattern on the biological properties of Ti grade 2

Highlights: • Laser modification causes changes in chemical composition of the surface. • Laser treatment creates roughness in a range from nano- to micrometers. • The surface modification presented results in a multimodal topography. • A hierarchical topography promotes protein adsorption. - Abstract: This paper presents a detailed characterization of Ti surface geometries as produced by non-contact laser functionalization and its impact on the process of protein adsorption. The proposed surface modification is designed for the local treatment of implantable devices with original roughness. In this work, titanium plates were initially modified by the two most common mechano-chemical treatments, shot peening and acid etching. The material under study was next functionalized DLIL (Direct Laser Interference Lithography) in order to obtained two different surface patterns: grooves and islands. The modified surfaces were characterized in terms of their shape, roughness, wettability, surface energy and chemical composition. For this purpose, the following methods were used: scanning electron microscopy, optical profilometry, atomic force microscopy, contact angle measurements, and X-ray photoelectron spectroscopy. Protein adsorption tests were conducted to consider the potential of the proposed methodology in biomedical applications and to compare the influence of the two different surface patterns on the initial state of ossointegration. To this end, XPS and FTIR studies were conducted. The systematic analysis presented will be useful when selecting an appropriate surface geometry for the local surface functionalization of implantable devices.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effect of aluminum substitution on structural and electromagnetic properties of nanocrystalline MgCuMn ferrites

The effect of substitution of nonmagnetic Al{sup 3+} ions on the structural and electromagnetic properties were studied in nanocrystalline ferrite series of Mg{sub 0.8}Cu{sub 0.2}Al{sub x}Fe{sub 1.95-x}Mn{sub 0.05}O{sub 4} where x varies 0-0.4 in steps of 0.1. This series was synthesized by using microwave hydrothermal method. The nanocrystalline ferrite phase was observed at temperature 150°C/40 min. Synthesized powders were characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The synthesized powders were densified using microwave sintering method at 950°C/40 min. The sintered samples were characterized using XRD. Surface morphology was observed by using field effective scanning electron microscopy (FESEM). The electrical and magnetic properties were measured at room temperature. These results led us to interfere that the values of d.c resistivity increases and dielectric constant, initial permeability, saturation magnetization and Curie temperature were observed to be decreased with the substitution of Al{sup 3+} ions with those of Fe{sup 3+}. The low dielectric and magnetic losses and low magnetization exhibited by aluminum substituted MgCuMn ferrites makes them find applications in microwave devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Probing the thermal decomposition of plutonium (III) oxalate with IR and Raman spectroscopy, X-ray diffraction, and electron microscopy

The thermal decomposition of Pu(III) oxalate was analyzed by Raman microspectroscopy, infrared spectroscopy, scanning electron microscopy, and powder X-ray diffraction. These data show that crystalline Pu 2 (C 2 O 4 ) 3 •9H 2 O progressively loses water and oxalate ligands as it is heated, which leads to a decrease in long-range lattice ordering, though minimal changes are observed in gross crystalline morphology. The onset of PuO 2 formation was observed between 200 - 250 °C. Thermal decomposition of oxalate ligands leads to the formation of CO 2 and plutonium oxalate-carbonate moieties, which had not been observed in previously published thermogravimetric measurements of Pu(III) oxalate. Formation of plutonium oxalate-carbonate moieties is believed to be associated with a change in the plutonium oxidation state from 3+ to 4+, which occurs prior to PuO 2 formation. The data provided herein demonstrate the rich spectroscopic nature of a rather underexplored, and technologically relevant, plutonium system. Ideally these results will further future investigations into the Pu(III) oxalate system both experimentally and computationally.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural tuning of nanogaps using electromigration induced by field emission current with bipolar biasing

We report a new method for fabrication of Ni nanogaps based on electromigration induced by a field emission current. This method is called “activation” and is demonstrated here using a current source with alternately reversing polarities. The activation procedure with alternating current bias, in which the current source polarity alternates between positive and negative bias conditions, is performed with planar Ni nanogaps defined on SiO{sub 2}/Si substrates at room temperature. During negative biasing, a Fowler-Nordheim field emission current flows from the source (cathode) to the drain (anode) electrode. The Ni atoms at the tip of the drain electrode are thus activated and then migrate across the gap from the drain to the source electrode. In contrast, in the positive bias case, the field emission current moves the activated atoms from the source to the drain electrode. These two procedures are repeated until the tunnel resistance of the nanogaps is successively reduced from 100 TΩ to 48 kΩ. Scanning electron microscopy and atomic force microscopy studies showed that the gap separation narrowed from approximately 95 nm to less than 10 nm because of the Ni atoms that accumulated at the tips of both the source and drain electrodes. These results show that the alternately biased activation process, which is a newly proposed atom transfer technique, can successfully control the tunnel resistance of the Ni nanogaps and is a suitable method for formation of ultrasmall nanogap structures.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Novel nanocomposites based on polythiophene and zirconium dioxide

Highlights: • Crystallinity of polythiophene decreased with doping process. • Zirconium dioxide changed the surface morphology of PT significantly. • Doping process increased the glass transition temperature of polythiophene. • Charge transport mechanism of all samples is consistent with CBH model. - Abstract: This paper reports charge transport mechanism of polythiophene (PT) and its nanocomposites having various weight of zirconium dioxide (ZrO{sub 2}). Fourier transform infrared (FT-IR) spectral studies showed that the Zr ions mostly affected the C−S bond of the polythiophene. X-ray diffraction (XRD) patterns indicated that ZrO{sub 2} powder was a mixture of monoclinic (64.62%) and tetragonal (35.38%) phase. XRD measurements revealed that crystallinity of PT decreased with increasing doping level. Significant morphological differences were observed in scanning electron microscopy (SEM) images of PT depending on the doping process. Thermal analysis carried out by differential scanning calorimetry (DSC) indicated that the doping processes increased glass transition temperature of PT. The alternating current (ac) conductivity mechanism analysis by universal power law indicated that charge transport mechanism of both PT and PT/ZrO{sub 2} nanocomposites was consistent with correlated barrier hopping (CBH) model. The doping process and frequency affected the hopping distance between the sites.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Fabrication of single phase p-CuInSe{sub 2} nanowire arrays by electrodeposited into anodic alumina templates

Single-phase CuInSe{sub 2} nanowire (NW) arrays were prepared at various pH values in a heated electrolyte by using pulse electrodeposition techniques and an anodized aluminum oxide template. X-ray diffraction showed that the CuInSe{sub 2} NW nucleation mechanism received H{sup +} constraints when the NWs were deposited at pH 1.7 with a (112) orientation and annealed at 550 °C. The CuInSe{sub 2} NW band gap was determined to be approximately 1 eV through optical measurements. Transmission electron microscopy showed that at the pH value of 1.7, small particles of the single-phase CuInSe{sub 2} NWs aligned along the crystallographic direction are nucleated to form large particles. Scanning electron microscopy revealed that the NW diameter and the length were 80 nm and 2.3 μm, respectively. From Mott–Schottky and Ohmic contact plots, the CuInSe{sub 2} NWs were found to be p-type semiconductors, and their work function was estimated to be approximately 4.69 eV.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Influence of concentration and volume of precursor on the electrochemical properties of vanadium oxide thin films prepared by spray pyrolysis

Vanadium oxide (V{sub 2}O{sub 5}) thin films have been prepared by spray pyrolysis using different concentrations and volumes of precursor solution via aqueous route at 673K deposition temperature. The influences of concentration and volume on the structural, morphological and electrochemical properties of the deposited samples are studied well. X - ray diffraction study shows orthorhombic crystal structure with V{sub 2}O{sub 5} phase, confirmed by FTIR spectroscopy. Scanning electron microscopy shows granular, homogeneous and dense surface morphology. Cyclic voltammetery of all samples carried at all scan rates. Samples prepared using 0.05M, 40 ml of precursor solution shows highest specific capacitance 428.25 F/gm at 5 mV/s, Charge discharge behavior exhibits specific energy 18.73 Wh/kg, specific power 36.00 kW/kg, columbic efficiency 87.50 %. Impedance spectroscopy study was carried in the frequency range 1mHz – 1MHz, reveals pseudocapacitive behavior of the electrode exhibiting internal resistance 1.34 ohm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Metalorganic chemical vapor deposition of ZnGeN 2 films on GaN: effects of cation stoichiometry on surface morphology and crystallinity

Novel optoelectronic device designs based on the heterostructures of III-N and II-IV-N 2 are promising to advance device performance significantly. For example, by utilizing InGaN-ZnGeN 2 quantum well (QW) structures instead of pure InGaN, the band structure engineering in the QW active region can lead to improved electron-hole wavefunction overlap, and thus enhance the radiative efficiency for photon generation. These novel heterostructures have great potential to address the current challenge of low quantum efficiency in InGaN QW based light emitting diodes emitting in green and beyond. The materials development of ZnGeN 2 is still at an early stage as compared to the much matured GaN material system. In an ideal octet rule preserving ordered structure of ZnGeN 2 , every N atom is coordinated by exactly two Zn and two Ge atoms. However, local violation of octet rule can be caused by non-ideal coordination of N by the cations. The disordered structure is thermodynamically less favorable but can still be achieved, for example, in kinetics-limited growth regime. The ordered ZnGeN 2 has a bandgap very close to that of GaN (~3.4 eV) and a lattice mismatch of <0.1% with GaN. Interestingly, the valence band of ZnGeN 2 has been predicted to be ~1 eV above that of GaN, which has inspired novel designs for high efficiency light emitters. In this work, we investigated the metalorganic chemical vapor deposition (MOCVD) of ZnGeN 2 films on GaN/c-sapphire templates. Diethylzinc (DEZn), germane (GeH4) and ammonia were used as the precursors for Zn, Ge and N, respectively. A systematic study was conducted to investigate the cation stoichiometry as a function of growth temperature (TG), total reactor pressure (P) and DEZn/GeH 4 molar flow rate ratio (RII/IV). Under the investigated growth window, the Zn/(Zn+Ge) composition in the films, determined from energy dispersive X-ray spectroscopy, decreased monotonically with increase in TG but increased with increase in P and RII/IV. Atom probe tomography data did not indicate the presence of any secondary phases such as Zn 3 N 2 or Ge 3 N 4 . The surface morphology and crystallinity of the grown films had strong correlation with the Zn/(Zn+Ge) composition. The scanning electron microscopy images showed that the near-stoichiometric films have planar surfaces whereas Zn-rich films had crystallites on their surface and the Zn-poor films had faceted surface. Scanning transmission electron microscopy (STEM) imaging revealed that the Zn-rich and Zn-poor films have columnar and filament-like morphology, respectively, whereas the near-stoichiometric films have continuous film-like cross-sectional morphology. TEM nano-diffraction patterns as well as X-ray diffraction 2θ-ω scan profiles indicate that the near stoichiometric films are single crystalline. Nano-diffraction pattern of the stoichiometric films resembled that of a disordered ZnGeN 2 structure. Room temperature Raman spectra of near-stoichiometric films showed only the phonon density of states like features of a cation disordered ZnGeN 2 . Cathodoluminescence and photoluminescence spectra measured at different temperatures had similar features with peak emission wavelength at ~ 2 eV. In conclusion, the stoichiometry of ZnGeN 2 films can be widely tuned by tuning the MOCVD growth parameters. The surface morphology and the crystallinity of the films were found to have strong correlation with the Zn/(Zn+Ge) composition. The stoichiometric ZnGeN 2 films grown on GaN were demonstrated with uniform surface morphology and high crystalline quality. The results from this work will provide pathway to implement ZnGeN 2 in device structures.

Karim, Md Rezaul↗
DOE OSTI2021

The influence of electrochemical cycling protocols on capacity loss in nickel-rich lithium-ion batteries

The transition towards electric vehicles and more sustainable transportation is dependent on lithium-ion battery (LIB) performance. Ni-rich layered transition metal oxides, such as NMC811 (LiNi 0.8 Mn 0.1 Co 0.1 O 2 ), are promising cathode candidates for LIBs due to their higher specific capacity and lower cost compared with lower Ni content materials. However, complex degradation mechanisms inhibit their use. In this work, tailored aging protocols are employed to decouple the effect of electrochemical stimuli on the degradation mechanisms in graphite/NMC811 full cells. Using these protocols, impedance measurements, and differential voltage analysis, the primary drivers for capacity fade and impedance rise are shown to be large state of charge changes combined with high upper cut-off voltage. Focused ion beam-scanning electron microscopy highlights that extensive microscale NMC particle cracking, caused by electrode manufacturing and calendering, is present prior to aging and not immediately detrimental to the gravimetric capacity and impedance. Scanning transmission electron microscopy electron energy loss spectroscopy reveals a correlation between impedance rise and the level of transition metal reduction at the surfaces of aged NMC811. The present study provides insight into the leading causes for LIB performance fading, and highlights the defining role played by the evolving properties of the cathode particle surface layer.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

A microfluidic electrochemical cell for studying the corrosion of uranium dioxide (UO 2 )

We have developed a specialized microfluidic electrochemical cell that enables in situ investigation of the electrochemical corrosion of microgram quantities of redox active solids. The advantage of downscaling is the reduction of hazards, waste, expense, and greatly expanding data collection for hazardous materials, including radioactive samples. Cyclic voltammetry was used to monitor the oxidation–reduction cycle of minute quantities of micron-size uraninite (UO 2 ) particles, from the formation of hexavalent uranium (U(VI)), U 3 O 7 and reduction to UO 2+x . Reaction progress was also studied in situ with scanning electron microscopy. The electrochemical measurements matched those obtained at the bulk-scale and were consistent with ex situ characterization of the run products by X-ray photoelectron spectroscopy, scanning transmission electron microscopy, and atomic force microscopy; thus, demonstrating the utility of the microfluidic approach for studying radioactive materials.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗