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At least 883 records · Page 49

Characterization of zirconium carbide microspheres synthesized via internal gelation

Microspheres of zirconium carbide with grain size 40-320 nm were synthesized using internal gelation techniques and characterized by scanning electron microscopy, synchrotron X-ray diffraction, and neutron total scattering. Compared with a polycrystalline benchmark ZrC sample prepared by plasma vapor phase deposition, the microspheres display lower variance in grain size and considerably lower microstrain representative of a more homogenous internal microstructure. However, excess carbon was present in the microspheres, evident in both the X-ray and neutron diffraction data as well as a corresponding hypostoichiometric ZrC phase. Furthermore, the excess carbon phase is assumed to be pockets of carbon that remained unreacted through the combined internal gelation and subsequent carbothermic reduction synthesis process. Atomic-scale structural characterization with neutron PDF analysis confirmed the presence of localized nano-sized domains of graphite-like carbon material.

36 MATERIALS SCIENCE↗

Three-dimensional multimodal imaging and analysis of biphasic microstructure in a Ti–Ni–Sn thermoelectric material

The three-dimensional microstructure of levitation melted TiNi{sub 1.20}Sn has been characterized using the TriBeam system, a scanning electron microscope equipped with a femtosecond laser for rapid serial sectioning, to map the character of interfaces. By incorporating both chemical data (energy dispersive x-ray spectroscopy) and crystallographic data (electron backscatter diffraction), the grain structure and phase morphology were analyzed in a 155 μm × 178 μm × 210 μm volume and were seen to be decoupled. The predominant phases present in the material, half-Heusler TiNiSn, and full-Heusler TiNi{sub 2}Sn have a percolated structure. The distribution of coherent interfaces and high-angle interfaces has been measured quantitatively.

36 MATERIALS SCIENCE↗

Screen printed silver top electrode for efficient inverted organic solar cells

Highlights: • Screen printing of silver pattern. • X-ray diffraction pattern confirmed the face centered cubic structure of silver. • Uniform surface morphology of silver pattern with sheet resistance of 0.06 Ω/sq. • The power conversion efficiency of fabricated solar cell is found to be 2.58%. - Abstract: The present work is mainly focused on replacement of the vacuum process for top electrode fabrication in organic solar cells. Silver top electrode deposited through solution based screen printing on pre-deposited polymeric thin film. The solution based printing technology provides uniform top electrode without damaging the underlying organic layers. The surface crystallinity and surface morphology of silver top electrode are examined through X-ray diffraction, field-emission scanning electron microscope and atomic force microscope. The purity of silver is examined through X-ray energy dispersive spectroscopy. The top electrode exhibits face centered cubic structure with homogeneous morphology. The sheet resistance of top electrode is found to be 0.06 Ω/sq and an average pattern thickness of ∼15 μm. The power conversion efficiency is 2.58%. Our work demonstrates that the solution based screen printing is a significant role in the replacement of vacuum process for the fabrication of top electrode in organic solar cells.

36 MATERIALS SCIENCE↗

TOP as ligand and solvent to synthesize silver telluride nanosheets

Highlights: • Silver telluride nanosheets were prepared through one-pot synthetic strategy. • TOP as both ligand and solvent favors silver telluride nanosheets growth. • The I–V curve of an Ag{sub 2}Te-nanosheet film indicates that as-prepared Ag{sub 2}Te nanosheets have good electric conductivity. - Abstract: Ag{sub 2}Te nanosheets are synthesized by a simple one-pot route using trioctylphosphine (TOP) as both solvent and stabilizer. Various controlling parameters were examined, such as molar ratios of AgNO{sub 3} to tellurium powder, reaction temperature and time, and precursor concentration. The morphology and composition of the products were characterized by X-ray diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and transmission electron microscopy. On the basis of a series of synthesis and characterizations, the formation mechanism of the Ag{sub 2}Te nanosheets are discussed. The I–V curve of an Ag{sub 2}Te-nan osheet film indicates that as-prepared Ag{sub 2}Te nanosheets have good electric conductivity.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Enhanced Li- and Na-storage in Sb-Graphene nanocomposite anodes

Highlights: • Antimony-graphene nanocomposite (Sb-GNP) was prepared by a wet-chemical approach. • Sb-GNP exhibits the well-dispersed Sb nanoparticles anchored on the graphenes. • Sb-GNP shows highly reversible capacities in both Li- and Na-storage. - Abstract: Antimony-graphene nanocomposite (Sb-GNP) was prepared from commercially available graphene nanoplatelets (GNPs) by a simple wet-chemical route at room temperature, and systematically investigated as an anode material for both lithium- and sodium-ion batteries (LIBs and NIBs). The microstructural features of Sb-GNP, and of pure Sb nanoparticles prepared without addition of GNPs, were characterized using X-ray diffraction, field-emission scanning electron microscopy, and high-resolution transmission electron microscopy. The successful formation of a nanocomposite structure was observed for Sb-GNP; the Sb nanoparticles are well dispersed and anchored on graphene nanoplatelets without significant aggregation of Sb nanoparticles, in contrast to the pure Sb nanoparticles. Furthermore, galvanostatic studies revealed that Sb-GNP displays better Li- and Na-storage performance than the pure Sb nanoparticles when utilized as an anode material. The enhanced electrochemical performance can be attributed to the effects of nanocomposite formation with GNPs.

36 MATERIALS SCIENCE↗

Titania nanotube arrays surface-modified with ZnO for enhanced photocatalytic applications

Highlights: • Heterostructures of TNA/ZnO synthesised through potentiostatic anodisation followed by hydrothermal method. • Evaluation of morphological features of the heterostructure with hydrothermal processing time. • Correlation of photocatalytic activity of the hetrostructure with its morphology and surface texture. - Abstract: Well ordered titanium dioxide nanotube arrays (TNA) of average diameter 129 nm and wall thickness of 25 nm were fabricated through potentiostatic anodisation of titanium (Ti) metal substrates. Such TNA were subsequently surface-modified with various amounts of zinc oxide (ZnO) nanopowders using hydrothermal technique to obtain heterogeneous TNA/ZnO nanostructures. The crystalline phase and surface microstructure of the heterostructures were determined by X-ray diffraction, Raman spectroscopy and scanning electron microscopy respectively. The morphology of the heterostructures strongly depended on the hydrothermal conditions employed. The photocatalytic activity of the heterostructures have also been investigated and correlated with their surface morphology and texture.

36 MATERIALS SCIENCE↗

Growth and characterization of single phase Cu{sub 2}O by thermal oxidation of thin copper films

We report a simple and efficient technique to form high quality single phase cuprous oxide films on glass substrate using thermal evaporation of thin copper films followed by controlled thermal oxidation in air ambient. Crystallographic analysis and oxide phase determination, as well as grain size distribution have been studied using X-ray diffraction (XRD) method, while scanning electron microscopy (SEM) has been utilized to investigate the surface morphology of the as grown oxide films. The formation of various copper oxide phases is found to be highly sensitive to the oxidation temperature and a crystalline, single phase cuprous oxide film can be achieved for oxidation temperatures between 250°C to 320°C. Cu{sub 2}O film surface appeared in a faceted morphology in SEM imaging and a direct band gap of about 2.1 eV has been observed in UV-visible spectroscopy. X-ray photoelectron spectroscopy (XPS) confirmed a single oxide phase formation. Finally, a growth mechanism of the oxide film has also been discussed.

36 MATERIALS SCIENCE↗

Synthesis and characterization of Eu{sup 3+}:Gd{sub 2}O{sub 3} hollow spheres for biomedical applications

Multifunctional magnetic Nanoparticles (MFMNPs) are potentially applicable in both drug delivery systems (DDS) and hyperthermia treatment. Structural, surface morphology and optical property were investigated by X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM) and photoluminescence (PL) measurement. Uniform Eu{sup 3+}:Gd{sub 2}O{sub 3} hollow microspheres of 1.8-2.0 μm diameters were synthesized by template based approach. We found that synthesized Hollow spheres are 100 nm in thickness. FE-SEM images revealed that the synthesized material are hollow in structure with good porous structure and these pores work as pathway for releasing drugs from the hollow particle inside. Luminescent properties of material were studied by room temperature photoluminescence emission spectra under the excitation of 275 nm. Material exhibit bright red emission corresponding to the {sup 5}D{sub 0}-{sup 7}F{sub 2} transition of the activator ions under ultraviolet light excitation, which might find potential applications in fields such as drug delivery or biological labeling because of their excellent luminescence properties.

36 MATERIALS SCIENCE↗

Catalyst-free growth of ZnO nanowires on ITO seed/glass by thermal evaporation method: Effects of ITO seed layer thickness

A seed/catalyst-free growth of ZnO nanowires (ZnO-NWs) on a glass substrate were successfully fabricated using thermal evaporation technique. These nanowires were grown on ITO seed layers of different thicknesses of 25 and 75 nm, which were deposited on glass substrates by radio frequency (RF) magnetron sputtering. Prior to synthesized ITO nanowires, the sputtered ITO seeds were annealed using the continuous wave (CW) CO2 laser at 450 °C in air for 15 min. The effect of seed layer thickness on the morphological, structural, and optical properties of ZnO-NWs were systematically investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and UV-Vis spectrophotometer.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Structural and photocatalytic examination of CoMoO4 nanopowders synthesized by GNP method

Highlights: • Synthesis of CoMoO{sub 4} nanoparticles in a simple, quick, and inexpensive way, by using a glycine nitrate procedure (GNP). • Two different crystal structures of CoMoO{sub 4}, α and β, was confirmed by X-ray diffraction. • BET analysis confirmed significant specific surface areas of CoMoO{sub 4} nanopowder. • CoMoO{sub 4} nanopowders can be promising solutions in photocatalytic processes toward green chemistry and sustainable development. - Abstract: The synthesis route by solution combustion, a glycine nitrate procedure (GNP) of CoMoO{sub 4} nanopowders by a glycine as a fuel and as a complexant was examined concerning the photocatalytic aspects and powder characteristics. The synthesized samples were investigated by differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Ultraviolet-Visible (UV/Vis) spectroscopy and nitrogen adsorption method. In this work, we presented a simple and effective method for controlling the composition and morphology of CoMoO{sub 4}. A single-phase α and β crystalline form of CoMoO{sub 4} compound was confirmed by X-ray diffraction (XRD). The photocatalytic activity of CoMoO{sub 4} nanopowders was estimated by the photocatalytic degradation of crystal violet in aqueous solution. In addition, the obtained specific CoMoO{sub 4} nanopowder demonstrated acceptable specific surface area, which can be of particular importance for the photocatalytic processes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effects of MCC Content on the Structure and Performance of PLA/MCC Biocomposites

Green composites of polylactic acid (PLA) with microcrystalline cellulose (MCC) as reinforcement of the polymer matrix were produced by melt blending to improve the brittleness of PLA. The MCC was prepared by hydrolysis of wheat straw cellulose with sulfuric acid to remove amorphous area. The biocomposites were prepared with different MCC contents (2, 4, 6, 8 wt%). Scanning electron microscopy, thermogravimetric analysis, X-ray diffraction, differential scanning calorimetry, Fourier transform infrared and mechanical testing were used to study the structure and properties of MCC and biocomposites. The tensile modulus and the strength of PLA/MCC biocomposites increased from 206 to 262 MPa and from 67.35 to 73.01 MPa, respectively.

36 MATERIALS SCIENCE↗

Investigation of the Effect of Foaming Agent on the Fabrication of NiTi Foams Using the Self-Propagating, High-Temperature Synthesis Process

Fabrication of NiTi intermetallic foams using the self-propagating, high-temperature synthesis (SHS) process was investigated. Weighed amounts of powders taken from an equimolar mixture of Ni and Ti powders along with 0.5, 1, and 1.5 wt pct of different foaming agents were cold pressed to form cylindrical compacts 10 mm in diameter, 20 mm in height, and 7 to 8 g in weight. A novel, induction-assisted ignition method was used for indirect heating and igniting the compressed mixtures at one end. As a result of intensive exothermic reaction between Ni and Ti and decomposition of foaming agents and liberation of gases, highly porous products were obtained. Characterization of the products was carried out using X-ray diffraction (XRD) and a scanning electron microscope equipped with an energy-dispersive spectroscope (SEM-EDS). The main phase in the products was detected to be B2(NiTi) with minor amounts of NiTi{sub 2} as the secondary phase. Other undesirable phases, such as Ni{sub 4}Ti{sub 3} and Ni{sub 3}Ti, were not detected. The effect of type and percentage of foaming agent on the formation and distribution of pores within the products was studied. Final products with porosities up to ~ 80 vol pct were obtained by adding foaming agent. Under the conditions of this study, CaH{sub 2} proved to be the most effective foaming agent considering its ability to generate a uniform distribution of pores, while TiH{sub 2} was not considered favorable due to its decomposition at relatively low temperatures. In general, the addition of foaming agents in amounts higher than 1wt pct is not recommended; due to the endothermic nature of thermal decomposition reactions of foaming agents, excessive use of these agents can result in suppression of the exothermic reaction.

36 MATERIALS SCIENCE↗

Preparation and characterization of novel foamed porous glass-ceramics

Foamed glass-ceramics without using foaming agent have been synthesized in a novel glass system of SrO-CaO-Al{sub 2}O{sub 3}-TiO{sub 2}-B{sub 2}O{sub 3}-SiO{sub 2}-P{sub 2}O{sub 5}-M{sub x}O{sub y} (where M = Ba, Mg, La, Ce and Ni) by a simple process of powder sintering. The glass and glass-ceramics are characterized by dilatometry, differential scanning calorimetry (DSC), heating stage microscopy (HSM), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), optical microscopy and Fourier transformed infrared spectroscopy (FTIR). All the glasses formed are amorphous and the glass transition temperature and dilatometric softening temperature of these glasses are found to be in the range 673–678 °C and 706–728 °C respectively. The glasses are highly stable as indicated by the DSC evaluated glass stability parameters of the range 195–240 °C. Quantitative sintering study of glass powder compacts revealed swelling in the samples with NiO and CeO{sub 2} corresponding to a geometry change of 75 and 108% around 900 °C respectively. With reference to this finding the glass powder compacts are heated to 900 °C and the foamed glass-ceramics are obtained. Characteristic crystalline silicate phases have been identified in the XRD studies and their microstructures are recorded by FESEM. Optical microscope study of the foamed samples revealed formation of bigger foamed cavity with residual pores in samples with NiO and CeO{sub 2} in comparison to samples with BaO, MgO and La{sub 2}O{sub 3}. The mean pore diameters of the samples with NiO and CeO{sub 2} are determined to be 43 and 32 μm, and their respective porosities are 2.34 and 1.82 cm{sup 3}/g respectively. Thus NiO and CeO{sub 2} are found to be very effective to obtain foamed glass-ceramics without using foaming agent by the viscous flow sintering of fine glass powder compacts along with the reduction of the respective polyvalent ions. - Highlights: • Synthesis of foamed porous glass-ceramics without foaming agent by sintering method • Only powder compact yielded foamed porous glass-ceramics but bulk glass did not. • Glasses containing NiO and CeO{sub 2} exhibited significant foaming efficiency. • Bloating of entrapped gas during viscous flow sintering is the origin of foaming. • Residual void created pores in the sintered glass-ceramics as evidenced in FESEM.

36 MATERIALS SCIENCE↗

Electrodeposition of Fe{sub 2}O{sub 3} nanoparticles and its supercapacitive properties

Fe{sub 2}O{sub 3} metal oxide nanoparticles are synthesized by electrodeposition method on stainless steel substrate. The crystal structure and surface morphological studies of the obtained metal oxide thin film are carried out by using X-ray diffraction (XRD) technique and Scanning Electron Microscopy (SEM) respectively. The electrochemical properties of Fe{sub 2}O{sub 3} thin film like Cyclic Voltammetry (CV), Galvonostatic Charge-Discharge (GCD) and Electrochemical Impedance Spectroscopy (EIS) are studied in a bath of 0.5 M Na{sub 2}SO{sub 4} as electrolyte. The observed specific capacitance shows improved values 135 Fg{sup −1} at 5 mVs{sup −1} scan rate. The electrochemical stability of Fe{sub 2}O{sub 3} electrode is investigated using cyclic voltammetry for 1000 cycles at a scan rate 50 mVs{sup −1}. The Fe{sub 2}O{sub 3} electrode exhibits superior cycling stability with only 4-5% capacitance loss after one thousand cycles. The values of specific power and specific energy of Fe{sub 2}O{sub 3} electrode obtained from Galvonostatic charge discharge studies are 2250 W.kg{sup −1} and 63.15 Wh.kg{sup −1} respectively at current density 1 A/g. From all the electrochemical properties of Fe{sub 2}O{sub 3} electrode, it indicates that it will be promising electrode material for supercapacitor application.

36 MATERIALS SCIENCE↗

Effects of cation stoichiometry on surface morphology and crystallinity of ZnGeN 2 films grown on GaN by metalorganic chemical vapor deposition

ZnGeN 2 films were grown on GaN-on-sapphire templates via metalorganic chemical vapor deposition. Energy dispersive X-ray spectroscopy was used to estimate the Zn/(Zn+Ge) composition ratio in the films. This ratio decreased with increase in growth temperature but increased with increase in total reactor pressure or Zn/Ge precursor flow rate ratio. Systematic mapping of these key growth parameters has allowed us to identify the growth window to achieve ZnGeN 2 with stoichiometric cation composition. Compositional and statistical analyses performed on data acquired from atom probe tomography provided insight into the local compositional homogeneity. The cations Zn and Ge did not demonstrate segregation or clustering at the sub-nanometer level. Based on X-ray diffraction 2θ-ω scan profiles and transmission electron microscope nano-diffraction patterns, the films with near-stoichiometric cation ratios were single crystalline with planar surfaces, whereas zinc-rich or zinc-poor films were polycrystalline with nonplanar surfaces. The growth direction of the single crystalline ZnGeN 2 films on GaN templates was along the c-axis. Room temperature Raman spectra showed features associated with the phonon density of states, indicating the presence of cation disorder in the lattice. A cathodoluminescence peak associated with transitions involving deep level defects was observed around 640 nm. The intensity of this peak increased by almost 2.5 times as the temperature was reduced to 77 K from room temperature. A similar peak was observed in photoluminescence spectra collected at 80 K.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructure and Electrochemical Performance of CeMg{sub 12}/Ni/TiF{sub 3} Composites for Hydrogen Storage

Ball milling was used to prepare CeMg{sub 12}/Ni/TiF{sub 3} composite alloys in this study. Microstructures of experimental alloys were analyzed by scanning electron microcopy (SEM), x-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM) with electron diffraction (ED). The electrochemical and kinetic characteristics of the ball-milled composite alloys were further evaluated based on their galvanostatic charge–discharge measurement, high-rate dischargeability (HRD), hydrogen diffusion behavior, as well as electrochemical impedance spectrum (EIS). Results indicated that the ball-milled alloy with 3 wt.% TiF{sub 3} exhibited the best electrochemical discharge capacity, which was not only related to the formation of amorphous and/or nanocrystalline phase but to the formation of MgF{sub 2} because it can effectively reduce the thermodynamic stability of hydride. With increasing TiF{sub 3}, the cycle degradation rates of the milled alloys were ameliorated remarkably. This improvement was attributed to the formation of an amorphous phase (which possesses strong anticorrosive and antioxidation abilities) as well as the formation of MgF{sub 2} and TiNi secondary phases. The ball-milled alloy with 3 wt.% TiF{sub 3} additive exhibited the strongest electrochemical kinetic properties, related to the highest hydrogen diffusion rate in the alloy (which was associated with multiple defects and grain boundary of amorphous and/or nanocrystalline phases) and the electrochemical reaction on the surface of alloy (which was related to the lowest apparent activation energy).

36 MATERIALS SCIENCE↗

XRD, Electron Microscopy and Vibrational Spectroscopy Characterization of Simulated High-Fe/Al HLW Glasses - 15666

Sample glasses have been made using SB6 high level waste (HLW) simulant (high in both Al and Fe) with 12 different frit compositions at a constant waste loading of 36 wt.%. As follows from X-ray diffraction (XRD) and optical and scanning electron microscopy (SEM) data, all the samples are composed of primarily glass and minor concentration of spinel phases which form both isometric grains and fine cubic (∼1 μm) crystals. Infrared (IR) spectra of all the glasses within the range of 400-1600 cm-1 consist of the bands due to stretching and bending modes in silicon-oxygen, boron-oxygen, aluminum-oxygen and iron-oxygen structural groups. Raman spectra showed that for the spectra of all the glasses within the range of 850-1200 cm{sup -1} the best fit is achieved by suggestion of overlapping of three major components with maxima at 911-936 cm{sup -1}, 988-996 cm{sup -1} and 1020-1045 cm{sup -1}. The structural network is primarily composed of metasilicate chains and possibly rings with embedded AlO{sub 4} and FeO{sub 4} tetrahedra. Major BO{sub 4} tetrahedra and BO{sub 3} triangles form complex borate units and are present as separate constituents. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

In Vitro and In Silico Studies of Chitin and Chitosan Based Nanocarriers for Curcumin and Insulin Delivery

The evaluation of drug delivery potential, molecular interactions of the polymeric nanoparticles with the drug molecule and release kinetics encounters more time consumption and also cost. In this study, we have adopted the combination of in vitro and in silico approaches to evaluate the drug delivery property of the polymeric nanoparticles viz. chitin and chitosan. Herein, two different therapeutic agents such as curcumin (a hydrophobic drug) and insulin (a therapeutic protein) were used to study the delivery potential of chitin and chitosan nanoparticles. The drug loaded chitin and chitosan nanoparticles were prepared and characterized using Fourier transform infra red spectroscopy, X-ray diffraction, dynamic light scattering and scanning electron microscopy analysis. In the in vitro drug delivery experiments, chitosan nanoparticles exhibited better encapsulation efficiency, drug loading capacity and prolonged release of the drug molecules than that of the chitin nanoparticles to both curcumin and insulin. Meanwhile the in silico experiments such as molecular docking and molecular dynamics predicted the molecular interactions and binding energy involved between the nanoparticles and the drug molecules. From this study, we suggest that the chitosan nanoparticles could be used as a carrier molecule for both curcumin and insulin. Graphical Abstract: .

77 NANOSCIENCE AND NANOTECHNOLOGY↗