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At least 415 records · Page 23

Characterization of MoS 2 films via simultaneous grazing incidence X-ray diffraction and grazing incidence X-ray fluorescence (GIXRD/GIXRF)

Physical vapor deposited (PVD) molybdenum disulfide (nominal composition MoS 2 ) is employed as a thin film solid lubricant for extreme environments where liquid lubricants are not viable. The tribological properties of MoS 2 are highly dependent on morphological attributes such as film thickness, orientation, crystallinity, film density, and stoichiometry. These structural characteristics are controlled by tuning the PVD process parameters, yet undesirable alterations in the structure often occur due to process variations between deposition runs. Nondestructive film diagnostics can enable improved yield and serve as a means of tuning a deposition process, thus enabling quality control and materials exploration. Grazing incidence X-ray diffraction (GIXRD) for MoS 2 film characterization provides valuable information about film density and grain orientation (texture). However, the determination of film stoichiometry can only be indirectly inferred via GIXRD. The combination of density and microstructure via GIXRD with chemical composition via grazing incidence X-ray fluorescence (GIXRF) enables the isolation and decoupling of film density, composition, and microstructure and their ultimate impact on film layer thickness, thereby improving coating thickness predictions via X-ray fluorescence. We have augmented an existing GIXRD instrument with an additional X-ray detector for the simultaneous measurement of energy-dispersive X-ray fluorescence spectra during the GIXRD analysis. This combined GIXRD/GIXRF analysis has proven synergetic for correlating chemical composition to the structural aspects of MoS 2 films provided by GIXRD. We present the usefulness of the combined diagnostic technique via exemplar MoS 2 film samples and provide a discussion regarding data extraction techniques of grazing angle series measurements.

MoS2↗

Gas sensing properties of magnesium doped SnO{sub 2} thin films in relation to AC conduction

Conducting magnesium doped (0 to 1.5 wt %) tin oxide thin films prepared by Spray Pyrolysis technique achieved detection of 1000 ppm of LPG. The films deposited at 304 °C exhibit an enhanced response at an operating temperature of 350 °C. The microstructural properties are studied by means of X-ray diffraction. AC conductivity measurements are carried out using precision LCR meter to analyze the parameters that affect the variation in sensing. The results are correlated with compositional parameters and the subsequent modification in the charge transport mechanism facilitating an enhanced LPG sensing action.

36 MATERIALS SCIENCE↗

Tin oxide thick film by doping rare earth for detecting traces of CO{sub 2}: Operating in oxygen-free atmosphere

Highlights: • La, Gd, and Lu doped SnO{sub 2} with their sensing properties toward CO{sub 2} were compared. • The microstructures of SnO{sub 2}-based nanoparticles were elaborately characterized. • La-SnO{sub 2} thick film shows superior response toward trace ppm CO{sub 2}. • Our sensing material can be recommended to employ in oxygen-free environment. - Abstract: SnO{sub 2} thick films doped with atomic ratios ranging from 0 up to 8 at.% La, 8 at.% Gd, 8 at.% Lu were fabricated, respectively, via hydrothermal and impregnation methods. The crystal phase, morphology, and chemical composition of the SnO{sub 2}-based nanoparticles were characterized by XRD, FE-SEM, EDX, HRTEM and XPS. Sensing properties of La-SnO{sub 2}, Gd-SnO{sub 2}, Lu-SnO{sub 2} films, as well as the pure SnO{sub 2} film, were analyzed toward CO{sub 2} in the absence of O{sub 2}. It was found that the optimal doping element was La and the best doping ratio was 4 at.%. The maximum response appeared at an operating temperature of 250 °C, on which condition the 4 at.% La-SnO{sub 2} exhibited a remarkable improvement of response from 5.12 to 29.8 when increasing CO{sub 2} concentration from 50 to 500 ppm. Furthermore, the working mechanism underlying such enhancement in CO{sub 2}-sensing functions by La additive in the absence of O{sub 2} was proposed and discussed.

36 MATERIALS SCIENCE↗

Influence of implantation temperature and He implantation-induced defects on morphological evolution of co-deposited Cu-Mo nanocomposites

Here, we investigate the effect of high-temperature helium (He) implantation on microstructural evolution in physical-vapor-co-deposited nanocomposite thin films of copper (Cu) and molybdenum (Mo). The microstructure morphologies of He-implanted and He-free domains are characterized using transmission electron microscopy and statistical analysis. High implantation temperatures (500°C and 750°C) lead to coarsening of Cu and Mo domains and their eventual reorientation. The microstructure evolution in He-implanted and He-free domains is comparable, indicating that implantation-induced defects do not accelerate the coarsening of the nanocomposite as compared to annealing alone. This observation contrasts with previously reported effects of implantation-induced defects on single-phase nanocrystalline metals, which include enhancement of grain growth by increasing self-diffusivity or its inhibition by pinning of grain boundaries.

36 MATERIALS SCIENCE↗

Enhanced tunable magnetoresistance properties over a wide temperature range in epitaxial (La{sub 0.7}Sr{sub 0.3}MnO{sub 3}){sub 1−x}:(CeO{sub 2}){sub x} nanocomposites

Vertically aligned nanocomposite (VAN) (La{sub 0.7}Sr{sub 0.3}MnO{sub 3}){sub 1−x}:(CeO{sub 2}){sub x} (LSMO:CeO{sub 2}) thin films have been grown on SrTiO{sub 3} (001) substrates by pulsed laser deposition. Tunable magnetoresistance properties as well as microstructures are demonstrated in these VAN films by modulating the film composition (x = 0, 0.3, 0.4, 0.45, 0.5, and 0.55). The sample of x = 0.3 shows a large low-field magnetoresistance (LFMR) in a high temperature range, i.e., over 10% at the range of 280 K to 320 K under 1 T and with a peak value of ∼13.5% at 310 K. In addition, a vast enhancement of LFMR in a low temperature range of 20–150 K with peak of ≈34.3% at 45 K for 1 T could be achieved with x = 0.5. The enhanced LFMR properties can be attributed to both the phase boundary induced spin fluctuation and the magnetic tunneling effect through vertical ferromagnetic/insulator/ferromagnetic structures. The observed enhanced LFMR performance, especially at high temperatures, as well as its simple growth method, offers a great potential for LSMO:CeO{sub 2}nanocomposites to be used in spintronic devices in a large temperature range.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Permeation Properties of Disordered Metal-Organic Framework Membranes Made by Vapor Phase Ligand Treatment

Zeolitic imidazolate frameworks (ZIFs) are nanoporous molecular sieves offering exciting opportunities for membrane- and adsorption-based gas separations. The Tsapatsis group developed an all-vapor-phase ligand induced permselectivation (LIPS) method for the fabrication of ZIF nanocomposite membranes. The LIPS method consists of a combination of atomic layer deposition of a dense oxide inside the mesopores of a porous support followed by transformation of the dense oxide deposit to nanoporous ZIF by exposure to sublimated vapors of an imidazolate ligand. It enables the formation of thin nanocomposite films consisting of ZIF deposited inside pores with diameters smaller than 10 nm. Vapor-phase conversion of the impermeable ZnO to ZIF increases flux of certain gases more than others. Vapor phase linker/ligand treatment (VPLT) can further modify the properties of LIPS and other membranes. The combination of LIPS with VPLT provides an all-vapor methodology for making and modifying ZIF membranes with the ability to control the ZIF deposit composition and the level of confinement in a variety of mesoporous supports. The propylene/propane separation performance of LIPS/VPLT ZIF membranes confined (entirely or partially) inside mesopores is remarkably superior to that of most conventional ZIF membranes consisting of unconfined (deposited on the external surface of porous supports) polycrystalline films. The accomplishments of this award are: (i) understanding of the LIPS process using mathematical models of atomic layer deposition (ALD), (ii) development of surface modification methods (vapor, e-beam, plasma, and X-ray treatments) to tune permeation properties, (iii) microstructural control of ZIF-8 films using ALD (support modification, direct ALD, and by use of in situ permeability monitoring), (iv) molecular simulations, and (v) thin film characterization and adsorption measurements using spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Suppression of magnetostructural transition on GdSiGe thin film after thermal cyclings

The influence of thermal cycling on the microstructure, magnetic phase transition and magnetic entropy change of a Gd 5 Si 1.3 Ge 2.7 thin film up to 1000 cycles is investigated. The authors found that after 1000 cycles a strong reduction of the crystallographic phase responsible for the magnetostructural transition (Orthorhombic II phase) occurs. We attribute this to the chemical disorder, caused by the large number of expansion/compression cycles that the Orthorhombic II phase undergoes across the magnetostructural transition. The suppression of the magnetostructural transition corresponds to a drastic decrease of the thin film magnetic entropy change. Our results reveal the importance of studying the thermal/magnetic cycles influence on magnetostructural transitions as they can damage a real-life device.

36 MATERIALS SCIENCE↗

Enhanced ferroelectric photoelectrochemical properties of polycrystalline BiFeO{sub 3} film by decorating with Ag nanoparticles

Polycrystalline BiFeO{sub 3} (BFO) films are fabricated on Pt/Ti/SiO{sub 2}/Si(100) substrate as photoelectrode using sol-gel method. The microstructure, optical, and photoelectrochemical (PEC) properties of the films are characterized and optimized by controlling the film thickness. Moreover, the PEC properties of the BFO films are dependent on ferroelectric polarization, which is mainly ascribed to the modulation of band structure at the BFO/electrolyte interface by the polarization. Further enhancement of PEC properties is obtained by decorating the samples with appropriate amounts of Ag nanoparticles, which is attributed to the reduced electron-hole recombination, and localized surface plasmon resonance effect of Ag nanoparticles.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Structural studies of zirconium doped Ba{sub 0.70}Sr{sub 0.30}TiO{sub 3} lead free ferroelectric thin films

Ba{sub 0.7}Sr{sub 0.3}(Zr{sub x}Ti{sub 1-x})O{sub 3}(BSZT, x=0,0.05,0.10,0.15,0.20) thin films were prepared by using sol gel method. Structural and microstructural properties were studied by using XRD, Raman Spectroscopy and atomic force microscopy (AFM) respectively. XRD and Raman Spectroscopy show the presence of tetragonal phase in multilayer BSZT thin film. The experimental results demonstrate that structural and microstructural properties of BSZT thin film were significantly dependent on variation of Zr content.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Nano-Ceramic Coated Plastics

Plastic products, due to their durability, safety, and low manufacturing cost, are now rapidly replacing cookware items traditionally made of glass and ceramics. Despite this trend, some still prefer relatively expensive and more fragile ceramic/glassware because plastics can deteriorate over time after exposure to foods, which can generate odors, bad appearance, and/or color change. Nano-ceramic coatings can eliminate these drawbacks while still retaining the advantages of the plastic, since the coating only alters the surface of the plastic. The surface coating adds functionality to the plastics such as self-cleaning and disinfectant capabilities that result from a photocatalytic effect of certain ceramic systems. These ceramic coatings can also provide non-stick surfaces and higher temperature capabilities for the base plastics without resorting to ceramic or glass materials. Titanium dioxide (TiO2) and zinc oxide (ZnO) are the candidates for a nano-ceramic coating to deposit on the plastics or plastic films used in cookware and kitchenware. Both are wide-bandgap semiconductors (3.0 to 3.2 eV for TiO2 and 3.2 to 3.3 eV for ZnO), so they exhibit a photocatalytic property under ultraviolet (UV) light. This will lead to decomposition of organic compounds. Decomposed products can be easily washed off by water, so the use of detergents will be minimal. High-crystalline film with large surface area for the reaction is essential to guarantee good photocatalytic performance of these oxides. Low-temperature processing (<100 C) is also a key to generating these ceramic coatings on the plastics. One possible way of processing nanoceramic coatings at low temperatures (< 90 C) is to take advantage of in-situ precipitated nanoparticles and nanostructures grown from aqueous solution. These nanostructures can be tailored to ceramic film formation and the subsequent microstructure development. In addition, the process provides environment- friendly processing because of the aqueous solution. Low-temperature processing has also shown versatility to generate various nanostructures. The growth of low-dimensional nanostructures (0-D, 1-D) provides a means of enhancing the crystallinity of the solution-prepared films that is of importance for photocatalytic performance. This technology can generate durable, fully functional nano-ceramic coatings (TiO2, ZnO) on plastic materials (silicone, Teflon, PET, etc.) that can possess both photocatalytic oxide properties and flexible plastic properties. Processing cost is low and it does not require any expensive equipment investment. Processing can be scalable to current manufacturing infrastructure.

Cho, Junghyun↗

Understanding the Impact of Fuel on Surfactant Microstructure of Firefighting Foam

Abstract Aqueous film-forming foam is being phased out due to the environmental impacts of fluorinated surfactants contained in the firefighting foams. To develop an environmentally friendly firefighting foam, it is important to understand the factors controlling the firefighting performance of surfactants. Fuel transport through foam has been considered as a dominant mechanism for foam collapse. Therefore, the impact of fuels (heptane, octane and trimethylbenzene (TMB)) on surfactant microstructure was studied for three different types of surfactants (Capstone, Glucopon, and siloxane) that have applications in firefighting foam. Multiple techniques were used to identify the microstructure and interfacial properties of surfactants with and without exposure to liquid fuel. The ignition time of fuel vapor through foam and solubility of fuel through liquid surfactant solution were measured as well. This work shows fuel solubility has an impact on the surfactant microstructure and interfacial properties. In addition, fuel solubility and vapor pressure affect the ignition time of fuel vapors.

Engineering↗

Magnetic and microwave properties of U-type hexaferrite films with high remanence and low ferromagnetic resonance linewidth

U-type barium hexaferrite films (Ba{sub 4}Ni{sub 1.4}Co{sub 0.6}Fe{sub 36}O{sub 60}) were deposited on (0001) sapphire substrates by pulsed laser deposition. Microstructure and magnetic properties of the films were characterized by X-ray diffraction, scanning electron microscopy and vibrating sample magnetometry. Ferromagnetic resonance (FMR) measurements were performed at X-band. The results indicate an anisotropy field of ∼8 kOe, and the saturation magnetization (4πM{sub s}) of ∼3.6 kG. An optimal post-deposition annealing of films results in a strong (0 0 n) crystallographic texture and a high hysteresis loop squareness (M{sub r}/M{sub s} = 92%) leading to self biased properties. Furthermore, the highly self-biased ferrite films exhibited an FMR linewidth of ∼200 Oe. The U-type hexaferrite films having low microwave loss, low magnetic anisotropy field, and high squareness are a suitable alternative to Sc or In doped BaM ferrites that have been the choice material for self-biased microwave devices at X-band frequencies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Correlation between thickness dependent nanoscale structural chemistry and superconducting properties of ultrathin epitaxial NbN films

NbN-based superconductors have attracted interest for superconducting circuits, quantum computation and high frequency devices. The superconducting properties of NbN films are predominately reliant on the microstructure, therefore, an atomic-level understanding of the structure-chemistry is required to achieve high quality epitaxial NbN films. Here, in this study, the thickness-dependent superconducting properties of NbN films (5, 10, and 50 nm) within NbN/AlN/Al 2 O 3 heterostructures are investigated. NbN and AlN were epitaxially grown by an industrial scale physical vapor deposition technique. The role of nanoscale chemistry on the ultrathin NbN superconducting film is investigated at the atomic level for the first time via atom probe tomography, providing three-dimensional atomic distribution, chemical homogeneity, effect of impurities, specially, in secondary phase formations and interfacial abruptness. The NbN film with 5 nm of thickness demonstrates a superconducting transition temperature of 11.2 K as compared to 50 nm NbN films with a transition temperature of 15.3 K. These thickness dependent variation of superconducting properties are associated with the chemical inhomogeneity in terms of in-plane N:Nb distribution, secondary phase formations and NbN/AlN interfacial abruptness as a function of the NbN films thicknesses. The analysis depicts the interplay between the surface/interface and the superconducting properties of ultrathin NbN films. These results provide insights on material design and growth that will enable the development of optimized superconducting NbN films for quantum devices.

36 MATERIALS SCIENCE↗

Dislocation-induced stop-and-go kinetics of interfacial transformations

Most engineering materials are based on multiphase microstructures produced either through the control of phase equilibria or by the fabrication of different materials as in thin-film processing. In both processes, the microstructure relaxes towards equilibrium by mismatch dislocations (or geometric misfit dislocations) across the heterophase interfaces (1-5) . Despite their ubiquitous presence, directly probing the dynamic action of mismatch dislocations has been unachievable owing to their buried nature. In this work, using the interfacial transformation of copper oxide to copper as an example, we demonstrate the role of mismatch dislocations in modulating oxide-to-metal interfacial transformations in an intermittent manner, by which the lateral flow of interfacial ledges is pinned at the core of mismatch dislocations until the dislocation climbs to the new oxide/metal interface location. Together with atomistic calculations, we identify that the pinning effect is associated with the non-local transport of metal atoms to fill vacancies at the dislocation core. These results provide mechanistic insight into solid-solid interfacial transformations and have substantial implications for utilizing structural defects at buried interfaces to modulate mass transport and transformation kinetics.

25 ENERGY STORAGE↗

Structural properties of pure and Fe-doped Yb films prepared by vapor condensation

Ytterbium and iron-doped ytterbium films were prepared by vapor quenching on Kapton substrates at room temperature. Structural characterization was performed by X-ray diffraction and transmission electron microscopy. The aim was to study the microstructure of pure and iron-doped films and thereby to understand the effects induced by iron incorporation. A coexistence of face centered cubic and hexagonal close packed-like structures was observed, the cubic-type structure being the dominant contribution. There is an apparent thickness dependence of the cubic/hexagonal relative ratios in the case of pure ytterbium. Iron-clusters induce a crystalline texture effect, but do not influence the cubic/hexagonal volume fraction. A schematic model is proposed for the microstructure of un-doped and iron-doped films including the cubic- and hexagonal-like structures, as well as the iron distribution in the ytterbium matrix. - Highlights: • Pure and Fe-doped Yb films have been prepared by vapor condensation. • Coexistence of fcc- and hcp-type structures was observed. • No oxide phases have been detected. • Fe-clustering does not affect the fcc/hcp ratio, but favors a crystalline texture. • A schematic model is proposed to describe microscopically the microstructure.

36 MATERIALS SCIENCE↗