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At least 451 records · Page 25

Vapor annealing synthesis of non-epitaxial MgB 2 films on glassy carbon

Here, we describe the fabrication and characterization of 25–800 nm thick MgB 2 films on glassy carbon substrates by Mg vapor annealing of sputter-deposited amorphous B films. Results demonstrate a critical role of both the initial B film thickness and the temperature–time profile on the microstructure, elemental composition, and superconducting properties of the resultant MgB 2 films. Films with thicknesses of 55 nm and below exhibit a smooth surface, with a roughness of 1.1 nm, while thicker films have surface morphology consisting of elongated nano-crystallites. The suppression of the superconducting transition temperature for thin films scales linearly with the oxygen impurity concentration and also correlates with the amount of lattice disorder probed by Raman scattering. The best results are obtained by a rapid (12 min) anneal at 850°C with large temperature ramp and cooling rates of ~540°C min -1 . Such fast processing suppresses the deleterious oxygen uptake.

36 MATERIALS SCIENCE↗

Synthesis of nickel selenide thin films for high performance all-solid-state asymmetric supercapacitors

As a significant semiconductor, nickel selenide shows enormous potential and extensive application prospects in the field of sensor, photocatalysis and supercapacitor. In this paper, nickel selenide (Ni 3 Se 2 , NiSe) thin films were successfully fabricated on stainless-steel sheet using a facile, effective electrodeposition technique. The morphologies, microstructures and chemical compositions of the thin films are characterized systematically. Electrochemical tests exhibit that the Ni3Se2 and NiSe possess high specific capacitance of 581.1 F/g and 1644.7 F/g, respectively. A flexible, all-solid-state asymmetric supercapacitor is assembled by utilizing NiSe film as positive electrode and activated carbon as negative electrode. The solid device delivers a high areal capacitance of 27.0 mF/cm 2 at the current density of 0.7 mA/cm 2 . Furthermore, the maximum volumetric energy density and power density of the NiSe//AC asymmetric SCs can achieve 0.26 mWh/cm 3 and 33.35 mW/cm 3 , respectively. The device shows robust cycling stability with 84.6% capacitance retention after 10000 cycles, outstanding flexibility and satisfactory mechanical stability. Moreover, two devices in series can light up a red light-emitting diode, which displayed great potential applications for energy storage.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enhanced field emission from lanthanum hexaboride coated multiwalled carbon nanotubes: Correlation with physical properties

Detailed results from field emission studies of lanthanum hexaboride (LaB{sub 6}) coated multiwalled carbon nanotube (MWCNT) films, pristine LaB{sub 6} films, and pristine MWCNT films are reported. The films have been synthesized by a combination of chemical and physical deposition processes. An impressive increase in field enhancement factor and temporal stability as well as a reduction in turn-on field and threshold field are observed in LaB{sub 6}-coated MWCNTs compared to pristine MWCNT and pristine LaB{sub 6} films. Surface morphology of the films has been examined by scanning electron microscopy. Introduction of LaB{sub 6} nanoparticles on the outer walls of CNTs LaB{sub 6}-coated MWCNTs films is confirmed by transmission electron microscopy. The presence of LaB{sub 6} was confirmed by X-ray photoelectron spectroscopy results and further validated by the Raman spectra. Raman spectroscopy also shows 67% increase in defect concentration in MWCNTs upon coating with LaB{sub 6} and an upshift in the 2D band that could be attributed to p-type doping. Ultraviolet photoelectron spectroscopy studies reveal a reduction in the work function of LaB{sub 6}-coated MWCNT with respect to its pristine counterpart. The enhanced field emission properties in LaB{sub 6}-coated MWCNT films are correlated with a change in microstructure and work function.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Microstructure and electrical properties of Na{sub 0.5}Bi{sub 0.5}(Ti{sub 0.98}Zr{sub 0.02})O{sub 3} thin film deposited on indium tin oxide/glass substrate

Highlights: • NBTZr deposited on ITO/glass under O{sub 2} exhibits a phase-pure perovskite structure. • NBTZr shows a well-defined P–E with a remanent polarization of 11.5 μC/cm{sup 2}. • At 100 kHz and 14 V, the dielectric tunability is 44.97% and FOM is 3.58. • At 100 kHz, the ϵ{sub r} and tanδ are 205 and 0.092, respectively. - Abstract: Na{sub 0.5}Bi{sub 0.5}(Ti{sub 0.98}Zr{sub 0.02})O{sub 3} (NBTZr) thin film has been prepared by chemical solution deposition onto indium tin oxide (ITO)/glass under O{sub 2} atmosphere. The microstructure and related electrical performance are investigated. The film exhibits a phase-pure polycrystalline perovskite structure, with evenly distributed grain size and full compactness. A well-defined polarization-electric field (P–E) loop can be observed with a remanent polarization (P{sub r}) of 11.5 μC/cm{sup 2} and small gap. At 14 V and 100 kHz, the dielectric tunability as high as 44.97% can be achieved and the dielectric constant of 205, dissipation factor of 0.092 as well as figure of merit of 3.58 are obtained.

36 MATERIALS SCIENCE↗

Atomic resolution strain analysis in highly textured FePt thin films

In this work, we present a detailed investigation of FePt-substrate interfaces and their influence towards the microstructural and magnetic configurations of the resulting metallic films. Discontinuous FePt films of roughly 15 nm thickness are deposited at 750 °C on MgO, MgAl{sub 2}O{sub 4}, SrTiO{sub 3}, and (La,Sr)(Al,Ta)O{sub 3} single-crystalline substrates. All of these films mainly show out-of-plane textured FePt islands; however, fractions of L1{sub 2} and in-plane oriented crystals are observed for the films on substrates with reduced lattice mismatch. Reduced easy axis coercivities and enhanced hard axis remanence values affirm this observation. Moreover, quantitative high-resolution transmission electron microscope analysis reveals that the reduced lattice mismatch results in a decreased density of dislocations, especially misfit dislocations, at the FePt-substrate interface. To further extend the research, carbon-doped FePt+32%C films are deposited on single-crystalline and sputtered MgO at 750 °C and 650 °C, respectively, to characterize the influence of a segregating media and reduced grain size. A comparison to the pure FePt sample reveals that the presence of seed layer grain boundaries leads to an increased fraction of in-plane oriented material, while the density of misfit dislocations solely depends on the degree of lattice mismatch.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Room-Temperature Ferroelectric LiNb 6 Ba 5 Ti 4 O 30 Spinel Phase in a Nanocomposite Thin Film Form for Nonlinear Photonics

Tetragonal tungsten bronze (TTB) materials are one of the most promising classes of materials for ferroelectric and nonlinear optical devices, owing to their very unique noncentrosymmetric crystal structure. In this work, a new TTB phase of LiNb 6 Ba 5 Ti 4 O 30 (LNBTO) has been discovered and studied. A small amount of a secondary phase, LiTiO 2 (LTO), has been incorporated as nanopillars that are vertically embedded in the LNBTO matrix. The new multifunctional nanocomposite thin film presents exotic highly anisotropic microstructure and properties, e.g., strong ferroelectricity, high optical transparency, anisotropic dielectric function, and strong optical nonlinearity evidenced by the second harmonic generation results. An optical waveguide structure based on the stacks of α-Si on SiO 2 /LNBTO–LTO has been fabricated, exhibiting low optical dispersion with an optimized evanescent field staying in the LNBTO–LTO active layer. Lastly, this work highlights the combination of new TTB material designs and vertically aligned nanocomposite structures for further enhanced anisotropic and nonlinear properties.

36 MATERIALS SCIENCE↗

Intermediate-phase engineering via dimethylammonium cation additive for stable perovskite solar cells

Achieving the long-term stability of perovskite solar cells is arguably the most important challenge required to enable widespread commercialization. Understanding the perovskite crystallization process and its direct impact on device stability is critical to achieving this goal. The commonly employed dimethyl-formamide/dimethyl-sulfoxide solvent preparation method results in a poor crystal quality and microstructure of the polycrystalline perovskite films. In this work, we introduce a high-temperature dimethyl-sulfoxide-free processing method that utilizes dimethylammonium chloride as an additive to control the perovskite intermediate precursor phases. By controlling the crystallization sequence, we tune the grain size, texturing, orientation (corner-up versus face-up) and crystallinity of the formamidinium (FA)/caesium (FA) y Cs 1-y Pb(I x Br 1-x )3 perovskite system. A population of encapsulated devices showed improved operational stability, with a median T80 lifetime (the time over which the device power conversion efficiency decreases to 80% of its initial value) for the steady-state power conversion efficiency of 1,190 hours, and a champion device showed a T80 of 1,410 hours, under simulated sunlight at 65 degrees C in air, under open-circuit conditions. In conclusion, this work highlights the importance of material quality in achieving the long-term operational stability of perovskite optoelectronic devices.

14 SOLAR ENERGY↗

Structure and transport in high pressure oxygen sputter-deposited BaSnO{sub 3−δ}

BaSnO{sub 3} has recently been identified as a high mobility wide gap semiconductor with significant potential for room temperature oxide electronics. Here, a detailed study of the high pressure oxygen sputter-deposition, microstructure, morphology, and stoichiometry of epitaxial BaSnO{sub 3} on SrTiO{sub 3}(001) and MgO(001) is reported, optimized conditions resulting in single-phase, relaxed, close to stoichiometric films. Most significantly, vacuum annealing is established as a facile route to n-doped BaSnO{sub 3−δ}, leading to electron densities above 10{sup 19} cm{sup −3}, 5 mΩ cm resistivities, and room temperature mobility of 20 cm{sup 2} V{sup −1} s{sup −1} in 300-Å-thick films on MgO(001). Mobility limiting factors, and the substantial scope for their improvement, are discussed.

36 MATERIALS SCIENCE↗

Impact of laser anneal on NiPt silicide texture and chemical composition

We have combined synchrotron X-ray pole figure measurements and transmission electron microscopy (TEM) nano-beam diffraction to study the impact of millisecond laser anneal on the texture and microstructure of NiPt silicide thin films. The powerful use of nano-beam diffraction in plan-view geometry allows here for both a mapping of grain orientation and intra-grain measurements even if these crystalline grains become very small. With this unique combination of local and large-scale probes, we find that silicide formation on n and p doped substrates using laser annealing results in smaller grains compared with the films processed using standard rapid thermal annealing. The laser annealed samples also result in grains that are more epitaxially oriented with respect to the Si substrate. For n-type substrate, the film is dominated by (020) and (013) oriented fibers with significant levels of intra-grain bending (transrotation) observed in both types of grains. For p-type substrates, mostly epitaxially aligned grains are detected. TEM coupled with energy-dispersive X-ray analysis was also used to study the elemental distribution in the silicide samples. Furthermore, we confirm that laser anneal leads to a larger accumulation of platinum at the silicide-substrate interface and modifies the distribution of dopants throughout the film.

36 MATERIALS SCIENCE↗

Time resolved surface photovoltage measurements using a big data capture approach to KPFM

Optoelectronic behavior in materials such as organic/inorganic hybrid perovskites depend on a complex interplay between fast (electronic) and slower (ionic) processes. These processes are thought to be influenced by structural inhomogeneities (e.g. interfaces and grain boundaries) bringing forward the necessity for development of techniques capable of correlating nanostructure and photo-transport behavior. While Kelvin probe force microscopy (KPFM) is ideally suited to map surface potentials on relevant length scales, it lacks sufficient temporal resolution to extract the meaningful system dynamics. Here, we develop a time resolved surface photovoltage (SPV) measurement based on full information capture of the photodetector stream during open loop KPFM operation. G-Mode, or G-KPFM allows quantification of SPV with microsecond temporal and nanoscale spatial resolution. Using this technique, we observe concurrent spatial and fast temporal variations in the SPV generated across a methylammonium lead bromide (MAPbBr3) thin film, a possible indicator relating microstructure with heterogenous photo-transport behavior. Here, we further demonstrate the advantage of adopting big data analytics including unsupervised clustering methods to quickly discern spatial variability in the information rich SPV dataset. Beyond G-KPFM, such clustering methods will be useful for interpretation of the multidimensional datasets arising from the growing number of time resolved KPFM approaches now available.

36 MATERIALS SCIENCE↗

Microstructure Characteristics of High Lift Factor MOCVD REBCO Coated Conductors With High Zr Content

We report the microstructural characteristics of high levels of Zr-added REBa2Cu3O7-x (RE = Gd, Y rare earth) coated conductors fabricated by Metal Organic Chemical Vapor Deposition (MOCVD). The enhancements of the lift factor defined as a ratio of the in-field (3 T, B parallel to c-axis) critical current density (J(c)) at 30 K and self-field J(c) at 77 K have been achieved for Zr addition levels of 20 and 25 mol% via optimization of deposition parameters. The presence of strong flux pinning is attributed to the aligned nanocolumns of BaZrO3 and nanoprecipitates embedded in REBa2Cu3O7-x matrix with good crystal quality. A high density of BZO nanorods with a typical size 6-8 nm and spacing of 20 nm has been observed. Moreover, the high Zr content was found to induce a high density of intrinsic defects, including stacking faults and dislocations. The correlation between in-field performance along the c-axis and microstructure of (Gd, Y) BCO film with a high level of Zr addition is discussed.

Galstyan, E↗

The role of gamma radiation on zircaloy-4 corrosion - 2016-0029

A key microstructural feature of irradiated oxide films that form on Zircaloy-4 is the development of significant amounts of interconnected porosity or microcracking, particularly along oxide grain boundaries. This development disrupts the protective nature of the barrier layer, effectively resulting in an increase in the observed post-transition corrosion rates. This observation suggests that some aspect of oxide dissolution may be occurring. It is noteworthy that when exposed to photons with energies greater than that of the oxide band gap, n-type semiconducting oxides are prone to dissolution. Because zirconia (ZrO{sub 2}) is an n-type semiconductor, it is plausible that high-energy photons may play an important role in corrosion. In an operating nuclear reactor, neutron and gamma flux levels are closely interrelated because they arise, for the most part, from the same originating process (i.e., the fissioning of nuclear fuel). Thus, it is difficult to isolate the independent effects of neutron and gamma radiation on corrosion. It is, however, theoretically conceivable to assess the role that gamma radiation may have on corrosion by comparing instances where variations in radiation environment exists; specifically by comparing where variations in gamma flux levels relative to neutron flux levels within different regions of a reactor or from reactor to reactor exist. Comparisons of the corrosion rates obtained between two different reactors (the Halden test reactor and the advanced test reactor [ATR]) that have differing gamma-to-neutron ratios were performed. In addition, an examination of corrosion rate data from the ATR, in which a variation in gamma-to-neutron flux ratio exists, was also conducted. Results are presented, from both assessments, which indicate that gamma radiation plays a role in the irradiated corrosion behavior of Zircaloy-4. In addition to a discussion of experimental data, potential mechanisms associated with photon-induced oxide dissolution of n-type semiconducting oxides, such as zirconia, is also provided. (authors)

36 MATERIALS SCIENCE↗

TEM investigation of beta-SiC grown epitaxially on Si substrate by CVD

A transmission electron microscopy study is being conducted on the microstructure of beta-SiC films grown epitaxially on 001-plane silicon by chemical vapor deposition. Observations have been made in plain view and in cross-section. A high density of stacking faults has been found in the bulk of the epilayer which are bounded by partials of the Shockley type with Burgers vectors 1/6 211-line. Cross-sectional high resolution electron microscopy of the interface has shown it to be semicoherent with misfit dislocations to accommodate the lattice parameter difference between the substrate and the epilayer. In addition to misfit dislocations, a high density of twins and some stacking faults are present in the SiC near the interface. Mechanisms for the nucleation and growth of these defects are discussed.

Chorey, C. M.↗

Analysis of the performance of the space ultravacuum research facility in attached and free-flyer mode

The old concept of using the wake of a spacecraft to obtain an ultrahigh vacuum is revisited with a somewhat different emphasis. Since it is possible to configure a wake shield so that a surface of interest does not subtend any walls that could become contaminated, it appears that it should be possible to achieve a contamination-free, ultrahigh vacuum capability with infinite pumping speed even in the presence of high heat loads and moderate gas loads. With the new interest in developing thin films with precision controlled synthetic microstructures such as superlattices, mixed metal oxide high temperature superconductors, rare-earth magneto-optical devices, and nano-crystalline alloys, the ability to work with a variety of different materials without cross contamination should be of significance. This paper analyzes the performance of the conceptual design for a Space Ultravacuum Research Facility (SURF), both in a Shuttle-attached mode and as a free-flyer. It is shown that even in the Shuttle-attached mode, it should be possible to obtain vacuum levels equivalent to 10 to the -10 Torr with O and N2 as the primary constituents. This should be sufficient to demonstrate the feasibility of the concept, particularly the infinite pumping speed and virtual elimination of contamination aspects. As a free-flyer the SURF will be limited primarily by the gas load associated with the process being performed. For chemical beam epitaxy (CBE) it is shown that equivalent vacuum levels of 10 to the -14 Torr should be possible at 300 km.

Naumann, Robert J.↗

Adhesion scratch testing - A round-robin experiment

Six sets of samples, TiN coated by chemical or physical vapor deposition methods (CVD or PVD) onto cemented carbide or high-speed steel (HSS), and TiC coated by CVD onto cemented carbide have been scratch tested using three types of commercially available scratch adhesion tester. With exception of one cemented carbide set, the reproducibility of the critical loads for any given set with a given stylus is excellent, about + or - 5 percent, and is about + or - 20 percent for different styli. Any differences in critical loads recorded for any given sample set can be attributed to the condition of the stylus (clean, new, etc.), the instrument used, the stylus itself (friction coefficient, etc.), and the sample set itself. One CVD set showed remarkably large differences in critical loads for different styli, which is thought to be related to a mechanical interaction between stylus and coating which is enhanced by a plastic deformability in the film related to the coating microstructure. The critical load for TiN on HSS increases with coating thickness, and differences in frictional conditions led to a systematic variation in the critical loads depending on the stylus used.

Perry, A. J.↗

Ionizing Organic Compound Based Nanocomposites for Efficient Gamma-Ray Sensor

Thin film and nanocrystalline materials of oxides have been very attractive choice as low cost option for gamma-ray detection and have shown great promise. Our studies on pure oxide films indicated that thickness and microstructure have pronounced effect on sensitivity. Since the interaction of gamma-ray with composites involves all three interaction processes; photoelectric effect, Compton scattering, and pair production, composites containing ionic organics have better chance for enhancing sensitivity. In the composites of ionizing organics oxidation effect of unusual oxides changes much faster and hence increases the sensitivity of radiation. In this study, we have used nickel oxide and titanium oxide in ionic organics to develop composite materials for low energy gamma-ray sensing. We prepared composites containing ethylene carbonate and evaluated the effect of commercial Cs-137 radiation source by studying current-voltage relationship at several frequencies. Radiated samples showed higher resistivity compared to as prepared composites.

Singh, N. B.↗

Impact of solvents and supercritical CO{sub 2} drying on the morphology and structure of polymer-based biofilms

In the present work, two-dimensional systems based on biodegradable polymers such as poly(ε-caprolactone) (PCL), poly(ethylene oxide) (PEO) and polylactic acid (PLA) are fabricated by means of a sustainable approach which consists in inducing phase separation in solutions of such polymers and “green” solvents, namely ethyl lactate (EL) and ethyl acetate (EA). The extraction of the solvent is promoted by a controlled drying process, which is performed in either air or supercritical CO{sub 2}. The latter can indeed act as both an antisolvent, which favors the deposition of the polymer by forming a mixture with EL and EA, and a plasticizing agent, whose solvation and transport properties may considerably affect the microstructure and crystallinity of the polymer films. The morphological, topographical and crystalline properties of the films are tailored through a judicial selection of the materials and the processing conditions and assessed by means of thermal analyses, polarized optical microscopy, scanning electron microscopy and confocal interferometric microscopy. The results show that the morphological and crystalline properties of the films are strongly dependent on the choice of both the polymer/solvent system and the operating conditions during the drying step. In particular, the morphological, topographical and thermal properties of films prepared starting from highly crystalline polymers, namely PCL and PEO, are greatly affected by the crystallization of the material. Conversely, the less crystalline PLA forms almost completely amorphous films.

36 MATERIALS SCIENCE↗