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At least 919 records · Page 51

Structural and magnetic properties of NiZn-ferrite thin films prepared by radio frequency magnetron sputtering

Polycrystalline NiZn-ferrite thin films were deposited on Si(100) substrate by rf magnetron sputtering, using targets with a nominal composition of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4}. The effects of substrate condition, sputtering pressure, and postannealing on the structure and magnetic properties of thin films have been investigated. Our results show that the preferred orientation of the NiZn spinel film changed from (311) to (400) with increasing the Ar pressure from 0.8 to 1.6 Pa, meanwhile, the grain size also increased. Atomic force microscopy analysis indicates that perfect surface morphology of the film can be obtained at a relatively lower sputtering pressure of 1.0 Pa. The relative percentage of residual oxygen increases significantly on a condition of lower sputtering pressure, and plays an important role in film structure due to the strong molecular adsorption tendency of oxygen on the film surface during the deposition process. A thin film with a typical thickness of 1 {mu}m, a saturation magnetization of 150 emu/cm{sup 3}, and a coercivity of 8.8 kA/m has been obtained after annealing at 800 deg. C, which has the potential application in magnetic integrated circuits.

36 MATERIALS SCIENCE↗

Enhanced Magneto-optical and Photocatalytic Properties of Ferromagnetic Mg{sub 1−y}Ni{sub y}Fe{sub 2}O{sub 4} (0.0 ≤ y ≤ 1.0) Spinel Nano-ferrites

Spinel Mg{sub 1−y}Ni{sub y}Fe{sub 2}O{sub 4} (0.0 ≤ y ≤ 1.0) ferrite magnetic nanoparticles (MNPs) were synthesized by a sol-gel combustion method using urea as the reducing agent/fuel. Powder X-ray diffraction (XRD) analysis revealed the formation of cubic spinel Mg{sub 1−y}Ni{sub y}Fe{sub 2}O{sub 4} powders and confirmed pure crystalline phase and the average crystalline size of 21.25 to 17.04 nm. Functional group bonds between metal and oxygen (M–O) were confirmed by Fourier transform infrared (FT-IR) spectra. The microstructure of the powders was recorded by high-resolution scanning electron microscope (HR-SEM) and confirmed the particle-like surface morphology with smaller agglomeration, due to the magnetic interaction of the particles. Energy-dispersive X-ray (EDX) results showed the composition of the expected elements and confirmed the phase purity of the products. Vibrating sample magnetometer (VSM) technique recorded at room temperature was used to analyse the magnetic properties of the samples and the hysteresis loops showed the ferromagnetic behaviour. Moreover, the samples Mg{sub 1−y}Ni{sub y}Fe{sub 2}O{sub 4} NPs were tested for the photocatalytic degradation (PCD) of methylene blue (MB) dye and the sample y = 0.6 showed maximum degradation efficiency (96.83 %), due to the smaller particle size with higher surface area than other compositions. Furthermore, spinel Mg{sub 1−y}Ni{sub y}Fe{sub 2}O{sub 4} nano-photocatalysts can be reused several times without change of its catalytic activity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Large-angle illumination STEM: Toward three-dimensional atom-by-atom imaging

To completely understand and control materials and their properties, it is of critical importance to determine their atomic structures in all three dimensions. Recent revolutionary advances in electron optics – the inventions of geometric and chromatic aberration correctors as well as electron source monochromators – have provided fertile ground for performing optical depth sectioning at atomic-scale dimensions. In this study we theoretically demonstrate the imaging of top/sub-surface atomic structures and identify the depth of single dopants, single vacancies and the other point defects within materials by large-angle illumination scanning transmission electron microscopy (LAI-STEM). The proposed method also allows us to measure specimen properties such as thickness or three-dimensional surface morphology using observations from a single crystallographic orientation.

36 MATERIALS SCIENCE↗

Pb 2+ –Calcite Interactions under Far-from-Equilibrium Conditions: Formation of Micropyramids and Pseudomorphic Growth of Cerussite

The presence of impurity ions is known to significantly influence mineral surface morphology during crystal growth from aqueous solution, but knowledge on impurity ion-mineral interactions during dissolution under far-from equilibrium conditions remains limited. Here we show that calcite (CaCO 3 ) exhibits a rich array of dissolution features in the presence of Pb. During the initial stage, calcite exhibits non-classical surface features characterized as micro pyramids developed spontaneously in acidic Pb-bearing solutions. Subsequent pseudomorphic growth of cerussite (PbCO 3 ) was observed, where nucleation occurred entirely within a pore space created by dissolution at the calcite/substrate interface. Uneven growth rates yielded a cerussite shell made of lath- or dendritic-shaped crystals. The cerussite phase was separated from the calcite by pores of less than 200 nm under transmission X-ray microscopy, consistent with the interface-coupled dissolution-precipitation mechanism. These results show that impurity metal ions exert significant control over the microscale dissolution features found on mineral surfaces and provide new insights into interpreting and designing micro structures observed in naturally-occurring and synthetic carbonate minerals by dissolution. In addition, heterogeneous micro-environments created in transport limited reactions under pore spaces may lead to unusual growth forms during crystal nucleation and precipitation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Annealing effects on structural, electrical and optical properties of antimony-tinoxide thin films deposited by sol gel dip coating technique

Antimony-doped tin dioxide possess interesting physical and chemical properties. These properties have a wide range of applications such as catalysis and optoelectronic devices. In the present study, antimony-doped tin oxide (SnO2:Sb) thin films were deposited on the quartz substrates by sol-gel dip coating technique. The films were annealed at temperatures 350°C, 550°C and 850°C in air for 2 hours. The structure and surface morphologies were observed by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). XRD patterns shows tetragonal structure for the SnO2:Sb films annealed at different temperatures. Crystallite size increased from 6 to 14 nm as annealing temperature increased from 350°C to 850°C. SEM studies reveals crack free and smooth surface for all the films. The grains are found to be homogenously distributed for films annealed at higher temperature. The electrical conductivity of the films annealed at 350°C and 550°C decreased and increased for the films annealed at 850°C. The optical properties of the films were investigated in the UV-visible-NIR region (200-900 nm) using UV spectra. The transmittance of the films decreased for films annealed at higher temperature. The optical energy band gap values (4.13 eV-4.83 eV) increased with the increase in annealing temperature.

36 MATERIALS SCIENCE↗

Effect of laser beam parameters on magnetic properties of Nd-Fe-B thick-film magnets fabricated by pulsed laser deposition

The effects of varying the laser power and the spot diameter of a laser beam on the magnetic properties, morphology, and deposition rate of Nd-Fe-B thick-film magnets fabricated by pulsed laser deposition (PLD) were investigated. Reducing the laser fluence on the target reduces the remanence and increases the Nd content and consequently the coercivity of the prepared films. The spot size of the laser beam was found to affect the film surface morphology, the deposition rate, and the reproducibility of the magnetic properties of the prepared films. Reducing the spot size reduces the number of droplets and the reproducibility of the magnetic properties and increases the droplet size. Controlling the spot size of the laser beam enabled us to maximize the deposition rate. Consequently, a coercivity of 1210 kA/m and a remanence of 0.51 T were obtained at a deposition rate of 11.8 {mu}m/(h{center_dot}W). This deposition rate is 30% greater than the highest previously reported deposition rate by PLD.

36 MATERIALS SCIENCE↗

Physical and Electrochemical Characterization of Aluminum Electrodes during Electrocoagulation

Electrocoagulation (EC) of synthetic groundwater was conducted using a sacrificial aluminum electrode in a flow-through EC reactor with short retention times (<1 min) under varying hydrodynamic and electrochemical conditions. The treated water was allowed to settle for 24 h and achieved silicate removal of up to 50 ± 4%, and hardness removal of 11 ± 1%. Physical, chemical, and electrochemical characterization was performed to explore changes in electrode surface morphology and composition. Electrochemical impedance spectroscopy (EIS) showed that chemical reactions at the electrode/water interface are sensitive to changes in the immediate chemical environment. We demonstrate that the most energy-intensive step in EC is aluminum dissolution at the anode, which remained fairly constant due to the continuous renewal of the anode’s surface, a result of aluminum dissolution. At the cathode, a structural change in the oxide layer, from γ-Al 2 O 3 to gibbsite, was detected by grazing-incidence X-ray diffraction, which decreased the resistance to charge transfer at the cathode surface, resulting in decreased electrode resistance. The high flow rate in the system minimized the accumulation of aluminum hydroxide solids and aluminum ions at the electrode/water interface, which minimized the formation of thick scalants and amorphous Al(OH) 3 on the cathode and anode, respectively. In conclusion, it was further demonstrated by EIS that under these conditions the resistance to charge transfer was constant throughout the duration of the experiment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Molecular-Beam Epitaxy of Two-Dimensional GaSe Layers on GaAs(001) and GaAs(112) Substrates: Structural and Optical Properties

The results of studies of the structural and optical properties of two-dimensional GaSe layers grown by molecular-beam epitaxy on GaAs(001) and GaAs(112) substrates using a valve cracking cell for the Se source are reported. The influence of the MBE growth parameters (the substrate temperature, Ga flux intensity, Se/Ga incident flux ratio) on the surface morphology of the layers is studied. By means of transmission electron microscopy, electron diffraction technique, and Raman spectroscopy, it is shown that the structure of the GaSe layers corresponds to the γ-GaSe polytype. From X-ray diffraction analysis, it is established that there exist α-Ga{sub 2}Se{sub 3} inclusions in the GaSe layers grown under conditions of high enrichment of the growth surface with Se.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Observation of crystallization and characterizations on thiourea cadmium iodide: A semi-organic optical material

Graphical abstract: - Highlights: • Thiourea cadmium iodide (TCI) was grown by slow evaporation solution technique. • Morphology and growth rate of the grown compound are determined with the help of inverted microscope. • Optical band gap has been determined. • Microstructure analysis has been reported. • Electrical study has been reported and discussed. - Abstract: In this work, the single crystals of thiourea cadmium iodide were grown by slow evaporation solution technique in two different ratios 2:1 and 1:1. During the formation of their single crystals the morphological features and its live growth process were recorded with the help of inverted microscope. Structural studies of the grown crystals have been carried out by powder X-ray diffraction to confirm the crystal system and vibrational modes by Raman spectroscopy. The optical energy band gaps were investigated through UV–vis spectroscopy study. The surface morphology of the grown single crystals was analyzed by using Scanning Electron Microscope and thermal analysis was carried out by using thermogravimetric analysis. The electrical properties were also studied as a function of frequency and the obtained results are discussed.

36 MATERIALS SCIENCE↗

Thermal Degradation of Single Crystal Zinc Oxide and the Growth of Nanostructures

Heat treatment of (0001) single crystal zinc oxide (ZnO) seems to degrade the surface morphology at high temperature. The degradation, however, does not suppress the growth of ZnO nanostructures on selective regions of the single crystal ZnO that have been sputtered with metallic zinc (Zn) and annealed at 800 degree sign C. On the uncoated regions, no growth occurs but the presence of pits suggests material loss from the surface. The formation of ZnO nanostructures on the selective regions could be aided by the preferential loss of oxygen as well as zinc suboxides from the uncoated regions. Indirect evidence of the role of oxygen and zinc suboxides can be inferred from the formation of nickel zinc oxide Ni{sub 0.9}Zn{sub 0.1}O and nickel oxide NiO{sub 2} when Zn is replaced by Ni and annealed under similar conditions.

36 MATERIALS SCIENCE↗

Effect of nitrogen doping on wetting and photoactive properties of laser processed zinc oxide-graphene oxide nanocomposite layers

Zinc oxide-graphene oxide nanocomposite layers were submitted to laser irradiation in air or controlled nitrogen atmosphere using a frequency quadrupled Nd:YAG (λ = 266 nm, τ{sub FWHM} ≅ 3 ns, ν = 10 Hz) laser source. The experiments were performed in air at atmospheric pressure or in nitrogen at a pressure of 2 × 10{sup 4} Pa. The effect of the irradiation conditions, incident laser fluence value, and number of subsequent laser pulses on the surface morphology of the composite material was systematically investigated. The obtained results reveal that nitrogen incorporation improves significantly the wetting and photoactive properties of the laser processed layers. The kinetics of water contact angle variation when the samples are submitted to laser irradiation in nitrogen are faster than that of the samples irradiated in air, the surfaces becoming super-hydrophilic under UV light irradiation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Quantification of waste morphology in Martian fretted terrain

Qualitative and quantitative analyses are performed on the northern fretted terrain of the Martian Isnenius Lacus quadrangle to determine the formation processes. The fretted terrain lies between 35-50 deg N latitude and 305-350 deg W longitude and was mapped with Viking orbiter instrumentation. The dominant landforms are a sequence of heavily cratered terrain, scattered flat-floored, fretted valleys, linear waste-covered valleys between flat-topped mesas, circum-mesa debris areas, a transition from mesas to knobby terrain, fewer upland forms, and low-relief, mantled, polar plains. The features spread out from a cratered terrain boundary in a succession of shapes. A principal components analysis characterizes definable spatial variations in the surface morphology and suggests that the features are youngest in the southwest direction. Relationships are also found between neighboring features. The principal components analysis technique is concluded to be a valuable tool for explaining the geomorphic evolution of the Martian surface.

Kochel, R. C.↗

Electrolytic Synthesis of Ni-W-MWCNT Composite Coating for Alkaline Hydrogen Evolution Reaction

Nickel–tungsten multi-walled carbon nanotube (Ni-W-MWCNT) composite films were fabricated by an electrodeposition technique, and their electrocatalytic activity toward hydrogen evolution reaction (HER) was studied. Ni-W-MWCNT composite films with a homogeneous dispersion of MWCNTs were deposited from an optimal Ni-W plating bath containing functionalized MWCNTs, under galvanostatic condition. The presence of functionalized MWCNT was found to enhance the induced codeposition of the reluctant metal W and resulted in a W-rich composite coating with improved properties. The electrocatalytic behaviors of Ni-W-MWCNT composite coating toward HER were studied by cyclic voltammetry (CV) and chronopotentiometry techniques in 1.0 M KOH medium. Further, Tafel polarization and electrochemical impedance spectroscopy (EIS) studies were carried out to establish the kinetics of HER on the alloy and composite electrodes. The experimental results revealed that the addition of MWCNTs (having a diameter of around 10-15 nm) into the alloy plating bath has a significant effect on the electrocatalytic behavior of Ni-W alloy deposit. The Ni-W-MWCNT composite coating was found to show better HER activity than the conventional Ni-W alloy coating. The enhanced electrocatalytic activity of Ni-W-MWCNT composite coating is attributed to the MWCNT intersticed in the deposit matrix, evidenced by surface morphology, composition and phase structure of the coating through SEM, EDS and XRD analyses, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Scalable Gas Diffusion Electrode Fabrication for Electrochemical CO 2 Reduction Using Physical Vapor Deposition Methods

Electrochemical CO 2 reduction (ECR) promises the replacement of fossil fuels as the source of feedstock chemicals and seasonal storage of renewable energy. While much progress has been made in catalyst development and electrochemical reactor design, few studies have addressed the effect of catalyst integration on device performance. Using a microfluidic gas diffusion electrolyzer, we systematically studied the effect of thickness and the morphology of electron beam (EB) and magnetron-sputtered (MS) Cu catalyst coatings on ECR performance. We observed that EB-Cu outperforms MS-Cu in current density, selectivity, and energy efficiency, with 400 nm thick catalyst coatings performing the best. Additionally, the superior performance of EB-Cu catalysts is assigned to their faceted surface morphology and sharper Cu/gas diffusion layer interface, which increases their hydrophobicity. Tests in a large-scale zero-gap electrolyzer yielded similar product selectivity distributions with an ethylene Faradaic efficiency of 39% at 200 mA/cm 2 , demonstrating the scalability for industrial ECR applications.

36 MATERIALS SCIENCE↗

Simultaneous in situ Optical Monitoring Techniques during Crystal Growth of ZnSe by Physical Vapor Transport

ZnSe crystals grown in sealed ampoules by the physical vapor transport method were monitored in situ using three techniques, simultaneously. A Michelson interferometer was set-up to observe the growth rate and surface morphological evolution. An interference pattern (interferogram) is formed by the interaction between the reflection of a HeNe laser (632.8 nm wavelength) off the crystal-vapor interface and a reference beam from the same laser. Preliminary results indicate that the rate of growth/thermal-etching can be calculated using analog data acquisition and simple fringe counting techniques. Gross surface features may also be observed using a digital frame grabber and fringe analysis software. The second in situ technique uses optical absorption to determine the partial pressures of the vapor species. The Se2 and Zn vapor species present in the sealed ampoule absorb light at characteristic wavelengths. The optical absorption is determined by monitoring the light intensity difference between the sample and reference beams. The Se2 Partial pressure profile along the length of the ampoule was estimated from the vibronic absorption peaks at 340.5, 350.8, 361.3 and 379.2 nm using the Beer's law constants established in the calibration runs of pure Se. Finally, because the high temperature crystal growth furnace contains windows, in situ visual observation of the growing crystal is also possible. The use of these techniques not only permits in situ investigation of high temperature vapor growth of semiconductors, but also offers the potential for real time feed back on the growing crystal and allows the possibility of actively controlling the growth process.

Su, C.- H.↗

In Vitro Fabrication and Biocompatibility Assay of a Biomimetic Osteoblastic Niche

A novel HAp-CS/Gel biomimetic osteoblastic niche was fabricated by freeze-drying, and its mechanical strength and biocompatibility were characterized. HAp-CS/Gel scaffolds in various ratios of 100:5, 100:10, and 100:20 (CS/Gel to HAp) were prepared by freeze-drying prior to chemical cross-linking followed by infrared spectrum analysis, EDS, FITR, SEM, fluorescence microscopy, MTT, and ALP experiments. Results from the infrared spectrum analysis showed that HAp doping remained the surface morphology and the architecture of scaffold with interconnected pores in the size range of 135 to 150 μm. The HAp doping ratio of 100:20 was found to be optimal based on its high porosity of 90%, better water uptake folds of 19.1. In addition, EDS and FITR analyses demonstrated that HAps were uniformly distributed on the surface of a scaffold with aggregates and particles, which has sufficient roughness for cell attachment and proliferation of osteoblasts. Under SEM and fluorescent microscopy, osteoblasts seeded onto the scaffold showed evenly distributed viable cells, which is believed to form a biomimetic niche. In the present study, we further demonstrate that osteoblasts can maintain their function and grow well on the scaffold through MTT and ALP tests. Thus, the scaffold has favorable physical properties and biocompatibility to support the proliferation and differentiation of osteoblasts and further to support the constructs of biomimetic osteoblastic niche.

60 APPLIED LIFE SCIENCES↗

Unraveling the Formation Mechanism of a Hybrid Zr-Based Chemical Conversion Coating with Organic and Copper Compounds for Corrosion Inhibition

Environmental-friendly chromate-free, zirconium (Zr)-based conversion coating is a promising green technology for corrosion protection. Additives in the surface treatment provides critical functionalities and performance improvements; however, mechanistic understanding as of how the additives influence the coatings remains unclear. In this study, a new organic-inorganic hybrid Zrbased conversion coating which combines copper (Cu) compounds and polyamidoamine (PAMAM), taking advantages of a complementary nature of organic and inorganic additives. Here, a multimodal approach combining electron and X-ray characterization is applied to study the interaction of Cu 2+ and PAMAM and the resulting impacts on the coating formation. Adding PAMAM changed the surface morphology, thickness, distribution of Cu in the cluster and void formation of the coatings. High PAMAM (100-200 pm) leads to little conversion coating formation, and low PAMAM (0-25 ppm) shows voids formation under the coatings. Moreover, PAMAM incorporates in the coating in a form of PAMAM-Cu complex with a higher concentration towards the surface, provides an organic layer at the surface of the coating. X-ray absorption near-edge structure (XANES) spectroscopy shows a difference between the conventional and hybrid coating treatments in an alkaline solution to simulate the E-coat process, suggesting the contribution of PAMAM in the enhanced chemical stability in an alkaline environment. Therefore, an intermediate range of addition of PAMAM (50 ppm) is optimal to 1) avoid excessive voids formation, 2) promote some Cu cluster formation and thus enhancing the Zr-based coating formation and 3) incorporate organic components into the coating to improve the adhesion of the subsequent coatings. Overall, this work furthers our knowledge on the formation mechanism of an effective and environmentally friendly hybrid conversion coating for corrosion inhibition, demonstrating a critical processing-structureproperty relationship. This study will benefit future development of green and effective surface treatment technology.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

High sensitive formaldehyde graphene gas sensor modified by atomic layer deposition zinc oxide films

Zinc oxide (ZnO) thin films with various thicknesses were fabricated by Atomic Layer Deposition on Chemical Vapor Deposition grown graphene films and their response to formaldehyde has been investigated. It was found that 0.5 nm ZnO films modified graphene sensors showed high response to formaldehyde with the resistance change up to 52% at the concentration of 9 parts-per-million (ppm) at room temperature. Meanwhile, the detection limit could reach 180 parts-per-billion (ppb) and fast response of 36 s was also obtained. The high sensitivity could be attributed to the combining effect from the highly reactive, top mounted ZnO thin films, and high conductive graphene base network. The dependence of ZnO films surface morphology and its sensitivity on the ZnO films thickness was also investigated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗