Search NASA⌕ Search

SEARCH · Search NASA

Results for “scanning electron diffraction”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,153 records · Page 64

Synthesis and characterization of DC magnetron sputtered nano structured molybdenum thin films

Molybdenum (Mo) thin films were deposited on corning glass (#7059) substrates using DC magnetron sputtering system. The effect of substrate temperature on the structural, morphology and topological properties have been investigated. Films were characterized by variety of techniques such as low angle x-ray diffraction (low angle XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM). The low angle XRD analysis revealed that the synthesized Mo films are nanocrystalline having cubic crystal structure with (110) preferential orientation. The microstructure of the deposited Mo thin films observed with FE-SEM images indicated that films are homogeneous and uniform with randomly oriented leaf shape morphology. The AFM analysis shows that with increase in substrate temperature the rms roughness of Mo films increases. The obtained results suggest that the synthesized nanostructured Mo thin films have potential application as a back contact material for high efficiency solar cells like CdTe, CIGS, CZTS etc.

36 MATERIALS SCIENCE↗

Optimization of BaZrO{sub 3} concentration as secondary phase in superconducting YBa{sub 2}Cu{sub 3}O{sub 7} for high current applications

We report the superconducting state properties of YBa{sub 2}Cu{sub 3}O{sub 7} (YBCO) on introduction of BaZrO{sub 3} (BZO) as a secondary phase. YBCO+xBZO (x= 0, 2, 4, 6, and 10 wt%) composite samples were prepared by solid state reaction method and characterized for structural, morphological and superconducting properties. X-ray diffraction confirms the increased crystallinity and images of scanning electron microscopy measurement show an increase in both grain size and grain connectivity on addition of BZO in YBCO. These effects are well pronounced in an applied magnetic field. Critical current density, J{sub C}, as well as the pinning force peaks at 4% of BZO concentration showed significant difference. A three-fold enhancement in J{sub C} and a six-fold enhancement in pinning force were observed at this optimum BZO concentration. This has been attributed to the pinning of flux lines in YBCO due to introduction of BZO as a secondary phase. These results show that this composite has potential application in high current applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Oxide Growth and Validation for Aluminum Research Reactor Fuel - 19422

Aluminum fuel cladding will undergo general corrosion with resulting formation of adherent oxide films during in-reactor and post-discharge exposures under various water conditions and temperatures. These oxides include chemically-bound water that can pose challenges for extended dry storage. This paper describes laboratory experiments performed to produce hydroxide (oxide) films on aluminum 1100, 6061 and 5052 series alloy substrates immersed in water at controlled temperatures. The results are compared to the oxide film present on a spent fuel assembly irradiated in research reactor. This work is part of a broad investigation to address knowledge gaps and technical data needs for dry storage of aluminum-clad spent nuclear fuel (SNF). To adequately assess the risks posed by chemically-bound water on SNF in dry storage and strategies for removing chemically bound water, it is necessary to understand the expected composition and loading of oxide films on SNF of different service histories and to investigate the response of such oxides to irradiation and potential drying methods. These efforts require both the growth of films under controlled conditions and the production of non-radioactive surrogates for testing. The current work comprises experimental investigation of oxide growth via (1) laboratory experiments to produce hydroxide films on aluminum alloy substrates immersed in water at controlled temperatures and (2) characterization and comparison of laboratory-grown oxides to oxides on service-exposed aluminum alloys. The important factors affecting oxide growth and characteristics typical of oxide films formed by aqueous corrosion under conditions similar to in-reactor are reviewed. Aluminum oxide films were grown under a variety of controlled temperature conditions and durations to serve as surrogates for oxides found on aluminum-clad spent nuclear fuel due to aqueous corrosion. The chemically-bound water found in oxides formed by aqueous corrosion poses challenges for extended dry storage, requiring investigation of how the oxide loading and characteristics vary with exposure history and to provide the initial condition for investigation of drying methods. Characteristics including chemical composition, oxide morphology, and film thickness were measured to assess whether the surrogate films were representative of in-service-produced oxides on SNF. Tests were conducted in liquid water at atmospheric pressure in the temperature range 50-100 deg. C, with and without heat flux through the corroding surface, to replicate in-service conditions, and at 185 deg. C inside pressure vessels to replicate pre-filming procedures. Three different alloys commonly used in aluminum clad research reactor fuel were considered: Al-1100, Al-6061, and Al-5052. Specimens were characterized by weighing before and after exposure to measure oxide mass loading, X-ray diffraction to identify oxide composition, and scanning electron microscopy to examine the oxide morphology and film thickness. The oxide type and the morphological characteristics of the film on a fuel element from the Uruguay RU1 research reactor were determined and compared to the laboratory surrogates. The results show some differences compared to the 50 deg. C laboratory specimen that are rationalized with the service storage history of the element. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Solid-state transformation of Fe-rich intermetallic phases in Al–5.0Cu–0.6Mn squeeze cast alloy with variable Fe contents during solution heat treatment

The Al–5.0 wt.% Cu–0.6 wt.% Mn alloys with a variable Fe content were prepared by squeeze casting. Optical microscopy (OM), Deep etching technique, scanning electron microscopy(SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to examine the solid-state transformation of Fe-rich intermetallics during the solution heat treatment. The results showed that the Chinese script-like α-Fe, Al{sub 6}(FeMn) and needle-like Al{sub 3}(FeMn) phases transform to a new Cu-rich β-Fe (Al{sub 7}Cu{sub 2}(FeMn)) phase during solution heat treatment. The possible reaction and overall transformation kinetics of the solid-state phase transformation for the Fe-rich intermetallics were investigated. - Graphical abstract: Display Omitted - Highlights: • The α-Fe, Al{sub 6}(FeMn) and Al{sub 3}(FeMn) phases change to the β-Fe phases. • Possible reactions of Fe phases during solution heat treatment are discussed. • The overall fractional transformation rate follows an Avrami curve.

36 MATERIALS SCIENCE↗

Effect of low-dimensional alumina structures on viability of L 929 cells

In the study, we estimated the cytotoxicity of alumina nanoparticles differing in shape (nanofibers, nanoplates, nanosheets, agglomerates of nanosheets) and close in physicochemical properties (particle size, specific surface area, phase composition, and zeta potential). The alumina structures were characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD) data, low-temperature nitrogen adsorption, and dynamic light scattering (DLS). The cytotoxicity was estimated on fibroblast cells of the L929 line. It was found that a more adverse effect on the cells was exerted by alumina nanofibers and nanosheets. The action of nanosheets on the cells was inhibitory and was of about the same level, irrespective of the observation period. The effect of alumina nanosheet agglomerates and nanoplates on the cell proliferation was weak even at an exposure time of 72 h.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Embedded Ge nanocrystals in SiO{sub 2} synthesized by ion implantation

200 nm thick SiO{sub 2} layers grown on Si substrates were implanted with 150 keV Ge ions at three different fluences. As-implanted samples were characterized with time-of-flight secondary ion mass spectrometry and Rutherford backscattering spectrometry to obtain depth profiles and concentration of Ge ions. As-implanted samples were annealed at 950 °C for 30 min. Crystalline quality of pristine, as-implanted, and annealed samples was investigated using Raman scattering measurements and the results were compared. Crystalline structure of as-implanted and annealed samples of embedded Ge into SiO{sub 2} matrix was studied using x-ray diffraction. No secondary phase or alloy formation of Ge was detected with x-ray diffraction or Raman measurements. Scanning transmission electron microscope measurements were done to get the nanocrystal size and localized information. The results confirmed that fluence dependent Ge nanocrystals of different sizes are formed in the annealed samples. It is also observed that Ge is slowly diffusing deeper into the substrate with annealing.

36 MATERIALS SCIENCE↗

Verification of high efficient broad beam cold cathode ion source

An improved form of cold cathode ion source has been designed and constructed. It consists of stainless steel hollow cylinder anode and stainless steel cathode disc, which are separated by a Teflon flange. The electrical discharge and output characteristics have been measured at different pressures using argon, nitrogen, and oxygen gases. The ion exit aperture shape and optimum distance between ion collector plate and cathode disc are studied. The stable discharge current and maximum output ion beam current have been obtained using grid exit aperture. It was found that the optimum distance between ion collector plate and ion exit aperture is equal to 6.25 cm. The cold cathode ion source is used to deposit aluminum coating layer on AZ31 magnesium alloy using argon ion beam current which equals 600 μA. Scanning electron microscope and X-ray diffraction techniques used for characterizing samples before and after aluminum deposition.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Preparation of Cationic/Anionic Chitin Nanofiber Composite Materials

In this study, we investigated the preparation of cationic/anionic chitin nanofiber (CNF) composite materials by electrostatic interaction. An aqueous dispersion of amidinium CNF was prepared by a top-down approach, and a maleylated CNF film was obtained by a bottom-up approach from a chitin ion gel in an ionic liquid with subsequent maleylation on the CNFs. The resulting film was dispersed in ammonia (aq), which was then mixed with the aqueous cationic CNF dispersion to give the composite film. The composition of the two CNFs was evaluated by scanning electron microscopy and X-ray diffraction measurements. Tensile testing results indicated that the mechanical properties of the composites were enhanced with increasing degrees of substitution of the cationic and anionic groups on CNFs, and also when the molar ratio of these groups approached 1:1. The dissociation of the two kinds of CNFs by alkaline treatment of the composite film was achieved, suggesting the presence of an electrostatic interaction among the interactions between them.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effects of Sn microalloying on cold rolling and recrystallization textures and microstructure of a ferritic stainless steel

Highlights: • Sn microalloying contributes to the enhancement in cold rolling texture intensity and the acceleration in cold rolling texture transformation. • Sn microalloying promotes the recrystallization process, and recrystallization occurs preferentially in steel with Sn compared with Sn-free steel. • Sn microalloying inhibits the growth of recrystallized grains, and the finer grains are obtained in steel with Sn. - Abstract: We investigated the effects of Sn microalloying on cold rolling and recrystallization textures and microstructure of a ferritic stainless steel. The as-received hot rolled sheets were cold rolled at 10%–90% reductions; the sheets cold rolled up to an 80% reduction were annealed at 740–880 °C for 5 min. For comparison, the cold rolling and recrystallization textures of the steel sheets with and without Sn were determined with the conventional X-ray diffraction method. The cold rolling and recrystallization metallographic microstructures were measured by scanning electron microscope and optical microscope, and the crystal orientation maps of the cold rolled and annealed samples were observed by electron backscattered diffraction. The micro-hardness was determined using a digital micro-hardness tester. Our results show that Sn microalloying in a medium chromium ferritic stainless steel plays multiple roles in the cold rolling and recrystallization processes. Sn micrcoalloying contributes to the enhancement in cold rolling texture intensity and the acceleration in cold rolling texture transformation. Sn microalloying is beneficial in promoting the recrystallization process. Recrystallization occurs preferentially in the ferritic stainless steel with Sn. Sn microalloying plays an important role in inhibiting the growth of recrystallized grains. The finer grains are obtained in ferritic stainless steel with Sn when annealing at high temperatures.

36 MATERIALS SCIENCE↗

Adsorption of Ammonium by Graphene Oxide-Based Composites Prepared by UV Irradiation and Using as Slow-Release Fertilizer

A novel sodium alginate-grafted poly(acrylic acid)/graphene oxide (NaAlg-g-PAA/GO) composite hydrogel was prepared via ultraviolet irradiation, and characterized by infrared spectroscopy spectrometer. X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy. It was employed to adsorb NH{sub 4}{sup +} from aqueous solution and used as slow-release nitrogen fertilizers (SNFs). Result indicated that the adsorption process for NH{sub 4}{sup +} reached equilibrium within 50 min, with the adsorption capacity of 6.6 mmol g{sup −1} even if 30 wt% GO was incorporated. The results of adsorption kinetic and isotherm were well described by the pseudo-second-order and Freundlich model. The thermodynamics analysis showed the adsorption process was spontaneous. The study indicated excellent water-holding ratio of soil with 2 wt% SNFs was 81.2%, and nitrogen release was up to 55.1% within 40 days in soil. Overall, NaAlg-g-PAA/GO could be considered as an efficient adsorbent for the recovery of nitrogen with the agronomic reuse as a fertilizer.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Formation of conductive copper lines by femtosecond laser irradiation of copper nitride film on plastic substrates

In this paper, we report a simple method to form conductive copper lines by scanning a single-beam femtosecond pulse laser on a plastic substrate covered with copper nitride (Cu{sub 3}N) film. The Cu{sub 3}N films were prepared by DC magnetron sputtering in the presence of an Ar + N{sub 2} atmosphere at 100 °C. The influence of the laser power and scanning speed on the formed copper line width, surface features, and morphology was analyzed by means of optical microscopy, X-ray diffraction, non-contact 3D profilometer, and scanning electron microscopy. The experimental results demonstrate that low laser power and low scanning speed favor the formation of uniform and flat Cu lines. After process optimization, copper lines with a width less than 5 μm were obtained, which provides an attractive application prospect in the field of flexible electronic devices.

36 MATERIALS SCIENCE↗

Synthesis of gadolinium carbonate-conjugated-poly(ethylene)glycol (Gd{sub 2}(CO{sub 3}){sub 3}@PEG) particles via a modified solvothermal method

PEGylated gadolinium carbonate ((Gd{sub 2}(CO{sub 3}){sub 3})@PEG) powder was successfully synthesized by a modified solvothermal method. The synthesized products were characterized by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Spectroscopy (EDS). A systematic change in the chemical surface composition, crystallinity and size properties of the Gd{sub 2}(CO{sub 3}){sub 3}@PEG particles was observed by increasing the reaction time at 5 hours, 7 hours, and 8 hours. The corresponding XRD patterns showed that the Gd{sub 2}(CO{sub 3}){sub 3} particles had hexagonal symmetry (JCPDS No. 37-0559) with a crystallite size of 3.5, 2.9, and 4.6 nm. FTIR spectra showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles were formed with the PEG as carbonyl and hydroxyl group attached to the surface. SEM analysis showed that the Gd{sub 2}(CO{sub 3}){sub 3})@PEG particles had a flake-like morphology of homogeneous sized particles and agglomerates. EDS analysis confirmed the presence of constituent Gd{sub 2}(CO{sub 3}){sub 3} elements.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Preparation and characterization of RF magnetron sputtered CuO/CaTi{sub 4}O{sub 9} thin films with enhanced third-order nonlinear optical properties

The titanate, is a material of interest for various energy applications, including photovoltaics, catalysts, and high-rate energy storage devices. Herein, its related materials, CuO/CaTi{sub 4}O{sub 9} [CCTO] thin films, were successfully fabricated on SrTiO{sub 3} (100) substrates by RF magnetron sputtering assisted with subsequent oxygen annealing. This obtained CCTO thin films were then systemically studied by X-ray powder diffraction (XRD), atomic force microscopy (AFM), scan electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and high-resolution transmission electron microscopy (HRTEM). It was found that CuO and CaTi{sub 4}O{sub 9} (001) particles were closely accumulated together on the surface of the substrate in the annealing process after comparing with that of the as-prepared thin film, which was verified by SEM and AFM results. Furthermore, we investigated the third-order nonlinear optical (NLO) properties of the as-prepared and annealed CCTO thin film by means of the Z-scan technique using 650 nm femtosecond laser pulse. Post-deposition oxygen annealing was found to modify the morphological characteristics of the films, resulting in enhancing their NLO properties. The observation of NLO performance of annealed CCTO thin film indicates that RF magnetron sputtering is a feasible method for the fabrication of optical thin films, which can be expanded to fabricate other NLO materials from the corresponding dispersions. Naturally, we concluded that the CCTO thin film occupy a better NLO property, and thus enlarge its application in nonlinear optics. - Highlights: • The CCTO thin film was prepared using the RF magnetron sputtering and oxygen annealing. • The film was prepared on the SrTiO{sub 3}(100) substrates with a Ca{sub 2}CuO{sub 3} target. • The oxygen annealing was found can effectively enhance the film quality and NLO property. • The film was characterized using XPS, SEM, AFM, TEM, XRD and Z-scan techniques.

36 MATERIALS SCIENCE↗

Morphological and electrical properties of epoxy-based composites reinforced with exfoliated graphite

An experimental study has been carried out to prepare and characterize epoxy/amine-based composites filled with different percentages of partially exfoliated graphite (i.e. pEG) particles having an exfoliation degree of 56% in order to analyze the effect of the filler amounts on the electrical properties of the resulting nanocomposites. Moreover, in order to fully investigate the direct relationship between the physical properties of the employed filler and the results of the electrical characterization, a structural and morphological characterization of the pEG samples is carried out by means of various type of analysis such as X-ray diffraction patterns, micro-Raman and Scanning Electron Microscopy (SEM) images. The DC electrical characterization reveals a percolation thresholds (EPT) that falls in the range [2–3] wt% and an electrical conductivity of about 0.66 S/m at the highest filler loading (6.5 wt%). From the analysis of the percolative curve it is possible to derive the percolation law parameters and in particular the critical exponent t, whose value (i.e. 1.2) reflects an effective 2D organization of the percolating structure consistent with the type of filler used (2-dimensional). Finally, an extensive analysis concerning the electrical properties in the frequency domain has been carried out in order to evaluate the effectiveness of pEG-loaded composites in terms of electromagnetic interference compatibility (EMC) and their applicability as radar absorbers materials (RAMs).

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effects of Inorganic Antiseptic on the Properties of Zein-Based Active Films

Zein, one of corn processing byproducts, has excellent film-forming ability. However, zein does not have intrinsic antibacterial or antioxidant activity which limits its direct applicability as active food packaging material. In the present study, the rod-shaped micro-sized ZnO crystals were incorporated into zein films to construct zein-based active films as active packaging material with antibacterial property. The morphologies, structural analysis and sizes of ZnO crystals were analyzed by field emission scanning electron microscope and X-ray diffraction. Prepared zein films were evaluated for ZnO loading and distribution. Furthermore, antibacterial activities on Gram-negative bacteria and Gram-positive bacteria were tested by using the disc diffusion method. Lastly, the stability of zein-based active films under the different storage temperature and humidity was investigated. The results showed that zein based-active films had well mechanical properties, stability and antibacterial activities, which were related to the sizes of ZnO crystals in films.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Modification of the structural, textural, and mechanical properties of an Al{sub 2}O{sub 3}/Al composite on the addition of an Al-SBA-15-type mesoporous phase

The formation of the pore structure of metal–ceramic materials based on Al{sub 2}O{sub 3}/Al composites has been studied in detail by modifying them via the incorporation of SBA-15-type mesoporous materials. The composition, pore structure, pore size, and morphology of the composite particles have been studied using nitrogen adsorption/desorption isotherms, scanning electron microscopy, and X-ray diffraction. We have produced Al-SBA-15/Al{sub 2}O{sub 3}/Al monoliths that combine properties of both adsorbents and permeable materials, but the incorporation of Al-SBA-15 into an Al{sub 2}O{sub 3}/Al matrix reduces the permeability and mechanical strength of the composites.

36 MATERIALS SCIENCE↗

Understanding the structural and morphological effects of synthesis route on NpO 2

The availability of actinide standard materials for use in nuclear safeguard applications is critical, as is thorough characterization thereof. Although accurate trace element compositions and isotopic considerations are paramount for deployment of reference standards, structural characterization is also essential towards accurately describing the chemical form and potential matrix effects in candidate materials. Here, to this end, samples of NpO 2 were synthesized via a direct denitration (DD) method and probed with powder X-ray diffraction (PXRD), Raman spectroscopy, and scanning electron microscopy (SEM) for structural and morphological characterization and comparison with NpO 2 materials produced via modified direct denitration (MDD). PXRD confirmed the bulk identity of NpO 2 , and no additional phases were identified using this method. Analysis of Raman data collected using a 532 nm excitation wavelength indicates that samples are mostly phase pure; however, some variability in spectral features is observed. Analysis of additional spectroscopic data collected with a 785 nm excitation wavelength revealed variability in the relative intensity of spectral features. Raman spectroscopy indicates that the sample is primarily NpO 2 ; however, additional signals indicate possible structural disorder, oxidized species, or potential contributions from other Np phases. To further investigate the possibility of additional phase contributions within the sample of NpO 2 , Raman spectroscopic mapping was employed to examine the homogeneity of the sample produced via DD. From this analysis, we determined that despite variability in the intensity of Raman-active vibrational modes, consistent spectra are obtained throughout the area of the sample investigated. SEM images show aggregates with variable sizes and shapes, with rounded, primary particles possessing an average diameter of approximately 100 nm. Comparison of the results of these multimodal analyses to the literature indicates that the crystal chemical, spectroscopic, and microstructural properties of NpO 2 vary based on synthesis method, even if X-ray diffraction data indicate that the bulk phase is NpO 2 .

Direct denitration↗

Direct conversion of h-BN into c-BN and formation of epitaxial c-BN/diamond heterostructures

We have created a new state of BN (named Q-BN) through rapid melting and super undercooling and quenching by using nanosecond laser pulses. Phase pure c-BN is formed either by direct quenching of super undercooled liquid or by nucleation and growth from Q-BN. Thus, a direct conversion of hexagonal boron nitride (h-BN) into phase-pure cubic boron nitride (c-BN) is achieved by nanosecond pulsed laser melting at ambient temperatures and atmospheric pressure in air. According to the P-T phase diagram, the transformation from h-BN into c-BN under equilibrium processing can occur only at high temperatures and pressures, as the hBN-cBN-Liquid triple point is at 3500 K/9.5 GPa or 3700 K/7.0 GPa with a recent theoretical refinement. Using nonequilibrium nanosecond laser melting, we have created super undercooled state and shifted this triple point to as low as 2800 K and atmospheric pressure. The rapid quenching from super undercooled state leads to the formation of a new phase, named as Q-BN. We present detailed characterization of Q-BN and c-BN layers by using Raman spectroscopy, high-resolution scanning electron microscopy, electron-back-scatter diffraction, high-resolution TEM, and electron energy loss spectroscopy, and discuss the mechanism of formation of nanodots, nanoneedles, microneedles, and single-crystal c-BN on sapphire substrate. We have also deposited diamond by pulsed laser deposition of carbon on c-BN and created c-BN/diamond heterostructures, where c-BN acts as a template for epitaxial diamond growth. We discuss the mechanism of epitaxial c-BN and diamond growth on lattice matching c-BN template under pulsed laser evaporation of amorphous carbon, and the impact of this discovery on a variety of applications.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗