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At least 559 records · Page 31

Lithium modified zeolite synthesis for conversion of biodiesel-derived glycerol to polyglycerol

Basic zeolite has received significant attention in the catalysis community. These zeolites modified with alkaline are the potential replacement for existing zeolite catalysts due to its unique features with added advantages. The present paper covers the preparation of lithium modified zeolite Y (Li-ZeY) and its activity for solvent free conversion of biodiesel-derived glycerol to polyglycerol via etherification process. The modified zeolite was well characterized by X-ray diffraction (XRD), Scanning Electron Microscope (SEM) and Nitrogen Adsorption. The SEM images showed that there was no change in morphology of modified zeolite structure after lithium modification. XRD patterns showed that the structure of zeolite was sustained after lithium modification. The surface properties of parent and modified zeolite was also observed N{sub 2} adsortion-desorption technique and found some changes in surface area and pore size. In addition, the basic strength of prepared materials was measured by Hammet indicators and found that basic strength of Li-ZeY was highly improved. This modified zeolite was found highly thermal stable and active heterogamous basic catalyst for conversion of solvent free glycerol to polyglycerol. This reaction was conducted at different temperatures and 260 °C was found most active temperature for this process for reaction time from 6 to 12 h over this basic catalyst in the absence of solvent.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comparative study of NiFe{sub 2−x}Al{sub x}O{sub 4} ferrite nanoparticles synthesized by chemical co-precipitation and sol–gel combustion techniques

Graphical abstract: AFM images of NiFe{sub 2}O{sub 4} ferrite nanoparticles at room temperature synthesized by sol–gel technique. Highlights: ► Particle size reduces to less than 30 nm. ► DC electrical resistivity increases with substitution of Cr{sup 3+}. ► Dielectric constant decreases. -- Abstract: A series of aluminum substituted Ni-ferrite nanoparticles have been synthesized by chemical co-precipitation and sol–gel techniques. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscope (AFM), Fourier transform infrared spectroscopy (FTIR), DC electrical resistivity and dielectric properties. Analysis of the X-ray diffraction pattern of all the samples confirmed the formation of spinel structure. The crystallite sizes remain within the range 25–41 ± 3 nm. FTIR measurements show two fundamental absorption bands, assigned to the vibration of tetrahedral and octahedral sites. DC electrical resistivity increases from 6.60 × 10{sup 7} to 6.9 × 10{sup 10} Ω cm as the Al{sup 3+} concentration increases from 0.00 to 0.50. The dielectric constant and loss tangent decreases with increasing Al{sup 3+} concentration from 22 to 14, 0.354 to 0.27 respectively at 5 MHz for all the samples. Impedance measurements as a function of frequency (1 kHz–5 MHz) at room temperature further helped in analyzing the electrical properties of the prepared samples.

36 MATERIALS SCIENCE↗

Tribological interaction between polytetrafluoroethylene and silicon oxide surfaces

We investigated the tribological interaction between polytetrafluoroethylene (PTFE) and silicon oxide surfaces. A simple rig was designed to bring about a friction between the surfaces via sliding a piece of PTFE on a thermally oxidized silicon wafer specimen. A very mild inclination (∼0.5°) along the sliding motion was also employed in order to monitor the tribological interaction in a gradual manner as a function of increasing contact force. Additionally, some patterns were sketched on the silicon oxide surface using the PTFE tip to investigate changes produced in the hydrophobicity of the surface, where the approximate water contact angle was 45° before the transfer. The nature of the transferred materials was characterized by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). XPS results revealed that PTFE was faithfully transferred onto the silicon oxide surface upon even at the slightest contact and SEM images demonstrated that stable morphological changes could be imparted onto the surface. The minimum apparent contact pressure to realize the PTFE transfer is estimated as 5 kPa, much lower than reported previously. Stability of the patterns imparted towards many chemical washing processes lead us to postulate that the interaction is most likely to be chemical. Contact angle measurements, which were carried out to characterize and monitor the hydrophobicity of the silicon oxide surface, showed that upon PTFE transfer the hydrophobicity of the SiO{sub 2} surface could be significantly enhanced, which might also depend upon the pattern sketched onto the surface. Contact angle values above 100° were obtained.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cold plasma finite element wave model for helicon waves

Helicon waves have been recently proposed as an off-axis current drive actuator due to their expected high current drive efficiency in the mid-radius region in high beta tokamaks. This current drive efficiency has mostly been calculated ignoring the effects of the plasma in the scrape-off-layer (SOL) in the modeling. The net core current drive efficiency will decrease if helicon power is lost to the SOL. Previous efforts to estimate the loss of helicon power in the SOL have used the hot plasma code AORSA. The large computational cost of AORSA prevents large parametric scans, so to further the understanding of helicon power loss in the SOL, a reduced finite element, full wave plasma model with effective collision frequency for collisional and Landau damping has been developed to study the helicon wave power lost to the SOL. It will be shown that the reduced finite element model (FEM) can reproduce the magnitude and trends of helicon |E| field patterns and power loss in the SOL of the hot plasma AORSA model. The reduced FEM provides significant advantages over AORSA in reducing the computational time and memory requirements, and in simulating arbitrary tokamak vessel geometry. Parametric scans of antenna parallel refractive index, antenna location, minimum SOL density, SOL density gradient, and vacuum vessel geometry will be carried out to determine the dependencies of the helicon power lost to the SOL as a function of important parameters. Subsequently, the helicon cutoff density is shown to be an important quantity in determining helicon power lost to the SOL. Furthermore, losses due to antenna loading and wave accessibility are also observed at different antenna and plasma parameters.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Fabrication of Si surface pattern by Ar beam irradiation and annealing method

The fabrication process of crater structures on Si crystal has been studied by an irradiation of Ar beam and a thermal annealing at 600 Degree-Sign C. The fabricated surface was measured by field emission scanning electron microscope and atomic force microscope. The results have shown the controllability of specifications of crater formation such as density, diameter and depth by changing two irradiation parameters, fluence and energy of Ar ions. By changing the fluence over a range of 1 {approx} 10 Multiplication-Sign 10{sup 16}/cm{sup 2}, we could control a density of crater 0 {approx} 39 counts/100{mu}m{sup 2}. By changing the energy over a range of 90 {approx} 270 keV, we could control a diameter and a depth of crater in 0.8 {approx} 4.1{mu}m and 99 {approx} 229nm, respectively. The present result is consistent with the previously proposed model that the crater structure would be arising from an exfoliated surface layer of silicon. The present result has indicated the possibility of the crater production phenomena as a hopeful method to fabricate the surface pattern on a micro-nano meter scale.

36 MATERIALS SCIENCE↗

Effects of TiO{sub 2} addition and electron irradiation on superconducting and mechanical properties of Bi{sub 2}Sr{sub 2}CaCu{sub 2}O{sub 8} (Bi-2212) superconductor

Titanium Oxide (TiO{sub 2}) compounds having very high melting point with lower heat capacity, is an excellent candidate for reinforcement of brittle materials such as superconductor ceramics. In addition to high melting point, the TiO{sub 2} is also capable of establishing flux pinning centers in bismuth-based superconductors such as the Bi-2212. To further enhance the flux pinning properties, irradiation is one of the techniques that can be used to re-create the required point defects. In this study, the effects of TiO{sub 2} addition and electron irradiation on Bi-2212 superconductor were studied. TiO{sub 2} added Bi-2212 superconductor samples with 5%, 10% and 15% weight percentage addition respectively, were prepared using the conventional solid-state reaction method. The samples were irradiated with electron beam with radiation dose of 100 KGray. Characterization was performed by X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The transition temperature (T{sub c}) and the critical current density (J{sub c}) of the samples were also measured. The XRD patterns for all the samples show well-defined peaks all of which could be indexed on the basis of a Bi-2212 phase structure. In addition, the XRD patterns indicate that electron irradiation did not change the structure of Bi-2212 superconducting phase. Results of SEM micrographs show disorientation in the texture of the microstructure for samples that are subjected to electron irradiation. The grains are seen to align randomly with higher degree of orientation. With regard to TiO{sub 2} additions, only small TiO{sub 2} addition sustained the superconducting properties upon irradiation. Addition of more than 5% weight percentage of TiO{sub 2} degrades the superconducting properties of the irradiated samples. Formation of weak-links may result in higher grain boundaries orientation within the superconducting grains and thus deteriorates the inter-grains connectivity and resulted in lower T{sub c} and degradation of J{sub c}. The strength of the superconductor reduced significantly when subjected to electron irradiation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Primary Beam Air Kerma Dependence on Distance from Cargo and People Scanners

The distance dependence of air kerma or dose rate of the primary radiation beam is not obvious for security scanners of cargo and people in which there is relative motion between a collimated source and the person or object being imaged. To study this problem, one fixed line source and three moving-source scan-geometry cases are considered, each characterized by radiation emanating perpendicular to an axis. The cases are 1) a stationary line source of radioactive material, e.g., contaminated solution in a pipe; 2) a moving, uncollimated point source of radiation that is shuttered or off when it is stationary; 3) a moving, collimated point source of radiation that is shuttered or off when it is stationary; and 4) a translating, narrow “pencil” beam emanating in a flying-spot, raster pattern. Each case is considered for short and long distances compared to the line source length or path traversed by a moving source. The short distance model pertains mostly to dose to objects being scanned and personnel associated with the screening operation. The long distance model pertains mostly to potential dose to bystanders. For radionuclide sources, the number of nuclear transitions that occur a) per unit length of a line source, or b) during the traversal of a point source, is a unifying concept. The “universal source strength” of air kerma rate at a meter from the source can be used to describe x-ray machine or radionuclide sources. For many cargo and people scanners with highly collimated fan or pencil beams, dose varies as the inverse of the distance from the source in the near field and with the inverse square of the distance beyond a critical radius. Ignoring the inverse square dependence and using inverse distance dependence is conservative in the sense of tending to overestimate dose.

Beam↗

Transmission X-ray scattering as a probe for complex liquid-surface structures

The need for functional materials calls for increasing complexity in self-assembly systems. As a result, the ability to probe both local structure and heterogeneities, such as phase-coexistence and domain morphologies, has become increasingly important to controlling self-assembly processes, including those at liquid surfaces. The traditional X-ray scattering methods for liquid surfaces, such as specular reflectivity and grazing-incidence diffraction, are not well suited to spatially resolving lateral heterogeneities due to large illuminated footprint. A possible alternative approach is to use scanning transmission X-ray scattering to simultaneously probe local intermolecular structures and heterogeneous domain morphologies on liquid surfaces. To test the feasibility of this approach, transmission small- and wide-angle X-ray scattering (TSAXS/TWAXS) studies of Langmuir films formed on water meniscus against a vertically immersed hydrophilic Si substrate were recently carried out. First-order diffraction rings were observed in TSAXS patterns from a monolayer of hexagonally packed gold nanoparticles and in TWAXS patterns from a monolayer of fluorinated fatty acids, both as a Langmuir monolayer on water meniscus and as a Langmuir–Blodgett monolayer on the substrate. The patterns taken at multiple spots have been analyzed to extract the shape of the meniscus surface and the ordered-monolayer coverage as a function of spot position. These results, together with continual improvement in the brightness and spot size of X-ray beams available at synchrotron facilities, support the possibility of using scanning-probe TSAXS/TWAXS to characterize heterogeneous structures at liquid surfaces.

Fukuto, Masafumi↗

All-optical lithography process for contacting nanometer precision donor devices

In this article, we describe an all-optical lithography process that can make electrical contact to nanometer-precision donor devices fabricated in silicon using scanning tunneling microscopy (STM). This is accomplished by implementing a cleaning procedure in the STM that allows the integration of metal alignment marks and ion-implanted contacts at the wafer level. Low-temperature transport measurements of a patterned device establish the viability of the process.

36 MATERIALS SCIENCE↗

Optical Control of Adaptive Nanoscale Domain Networks

Adaptive networks can sense and adjust to dynamic environments to optimize their performance. Understanding their nanoscale responses to external stimuli is essential for applications in nanodevices and neuromorphic computing. However, it is challenging to image such responses on the nanoscale with crystallographic sensitivity. Here, the evolution of nanodomain networks in (PbTiO 3 ) n /(SrTiO 3 ) n superlattices (SLs) is directly visualized in real space as the system adapts to ultrafast repetitive optical excitations that emulate controlled neural inputs. The adaptive response allows the system to explore a wealth of metastable states that are previously inaccessible. Their reconfiguration and competition are quantitatively measured by scanning x-ray nanodiffraction as a function of the number of applied pulses, in which crystallographic characteristics are quantitatively assessed by assorted diffraction patterns using unsupervised machine-learning methods. The corresponding domain boundaries and their connectivity are drastically altered by light, holding promise for light-programable nanocircuits in analogy to neuroplasticity. Phase-field simulations elucidate that the reconfiguration of the domain networks is a result of the interplay between photocarriers and transient lattice temperature. The demonstrated optical control scheme and the uncovered nanoscopic insights open opportunities for the remote control of adaptive nanoscale domain networks.

36 MATERIALS SCIENCE↗

Protective effects of Sapindus mukorossi Gaertn against fatty liver disease induced by high fat diet in rats

Highlights: • AESM is able to prevent the elevation of ALT and AST, and to decreased LDL-C level. • AESM demonstrates the effects of down-regulating blood fat level and protecting liver. • AESM consistent with the efficacy of simvastatin in NAFLD. - Abstract: Objectives: Study the effects of alcohol extract of Sapindus mukorossi Gaertn (AESM) on the metabolism of blood fat, morphology of fenestrated liver sinusoidal endothelial cells (LSEC), and the ultrastructure of liver cells of the rats with non-alcoholic fatty liver disease (NAFLD). Methods: Divide SD rats into control group, model group, simvastatin (7.2 mg/kg) group, and S.mukorossi Gaertn group with high dosage (0.5 g/kg), moderate dosage (0.1 g/kg), and low dosage (0.05 g/kg). After feeding with fat-rich nutrients for 3 weeks and establishing the model of hepatic adipose, conduct intragastric administration and provide the rats with fat-rich nutrients at the same time. At the 43rd day, take blood sample and measure aminotransferase and different indexes of blood fat; take hepatic tissue for pathological section, and observe the hepatic morphological patterns under light microscope; obtain and fix the hepatic tissue after injecting perfusate into the body, and observe the changes of fenestrated LSEC under scanning electron microscope; observe the ultrastructure of liver cells under transmission electron microscope. Results: High-dosage alcohol extracts of S.mukorossi Gaertn can alleviate the AST, ALT, TC, TG, LDL, γ-GT, and ALP level, as well as raise the HDL and APN level in the serum of NAFLD-rat model. In addition, through the observation from light microscope and electron microscopes, the morphology of the hepatic tissue and liver cells as well as the recovery of the fenestrated LSEC in the treatment group has become normal. Conclusions: Alcohol extracts of S.mukorossi Gaertn can regulate the level of blood fat and improve the pathological changes of the hepatic tissues in NAFLD-rat model, which demonstrates the effects of down-regulating fat level and protecting liver.

60 APPLIED LIFE SCIENCES↗

Oriented Y-type hexagonal ferrite thin films prepared by chemical solution deposition

Thin films of Ba{sub 2}Zn{sub 2}Fe{sub 12}O{sub 22} (Y) hexaferrite were prepared through the chemical solution deposition method on SrTiO{sub 3}(1 1 1) (ST) single crystal substrates using epitaxial SrFe{sub 12}O{sub 19} (M) hexaferrite thin layer as a seed template layer. The process of crystallization was mainly investigated by means of X-ray diffraction and atomic force microscopy. A detailed inspection revealed that growth of seed layer starts through the break-up of initially continuous film into isolated grains with expressive shape anisotropy and hexagonal habit. The vital parameters of the seed layer, i.e. thickness, substrate coverage, crystallization conditions and temperature ramp were optimized with the aim to obtain epitaxially crystallized Y phase. X-ray diffraction Pole figure measurements and Φ scans reveal perfect parallel in-plane alignment of SrTiO{sub 3} substrate and both hexaferrite phases. - Graphical abstract: XRD pole figure and AFM patterns of Ba{sub 2}Zn{sub 2}Fe{sub 12}O{sub 22} thin film epitaxially grown on SrTiO{sub 3}(1 1 1) single crystal using seeding layer templating. - Highlights: • Single phase Y-type hexagonal ferrite thin films were prepared by CSD method. • Seed M layer breaks into isolated single crystal islands and serves as a template. • Large seed grains grow by consuming the grains within the bulk of recoated film. • We explained the observed orientation relation of epitaxial domains. • Epitaxial growth on SrTiO{sub 3}(1 1 1) with relation (0 0 1){sub M,Y}//(1 1 1){sub ST}+[1 0 0]{sub M,Y}//[2 −1 −1]{sub ST}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In situ formation of sintered cordierite–mullite nano–micro composites by utilizing of waste silica fume

Highlights: ► We succeeded to obtain in situ formed sintered cordierite–mullite nano–macro composites from waste and pure materials at 1400 °C. ► Their sinterability was greatly dependent on both firing temperature and composition. ► XRD patterns showed that the optimum temperature required for formation of sintered cordierite–mullite nano–macro composites was achieved at 1400 °C. ► The batch containing 70 wt.% cordierite and 30 wt.% mullite exhibited the best properties. ► Microstructures of the densified composites were composed of nano–macro cordierite–mullite structures. -- Abstract: This study aims at in situ formation of sintered cordierite–mullite nano–macro composites having high technological properties using waste silica fume, calcined ball clay, calcined alumina, and magnesia as starting materials. The starting materials were mixed in different ratios to obtain different cordierite–mullite composite batches in which the cordierite contents ranged from 50 to 100 wt.%. The batches were uni-axially pressed at 100 MPa and sintered at 1350, 1400 and 1450 °C to select the optimum temperature required for cordierite–mullite nano–macro composites formation. The formed phases were identified by X-ray diffraction (XRD) pattern. The sintering parameters in terms of bulk density (BD) and apparent porosity (AP) were determined. The microstructure of composites has been investigated by scanning electron microscope (SEM). Cold crushing strength (CCS) of the sintered batches was evaluated. The result revealed that the cordierite–mullite nano–macro composites were in-situ formed at 1400 °C. The batch containing 70 wt.% cordierite showed good physical and mechanical properties.

36 MATERIALS SCIENCE↗

The importance of temporal and spatial incoherence in quantitative interpretation of 4D-STEM

Recent developments in pixelated detectors, when combined with aberration correction of probe forming optics have greatly enhanced the field of scanning electron diffraction. Differential phase contrast is now routine and deep learning has been proposed as a method to extract maximum information from diffraction patterns. This study examines the effects of temporal and spatial incoherence on convergent beam electron diffraction patterns and demonstrates that simple center of mass measurements cannot be naively interpreted. The inclusion of incoherence in deep learning data sets is also discussed.

36 MATERIALS SCIENCE↗

Soft magnetic composites manufactured by warm co-extrusion of bulk metallic glass and steel powders

Soft magnetic composites of Fe-based bulk metallic glass and low-alloy steel have been manufactured by warm co-extrusion of precursor powders at temperatures within the supercooled liquid region of the glass. Composites were manufactured with amorphous volume fractions of 75%, 67%, and 100%. Full consolidation of the constituent powders was observed with the bulk metallic glass remaining substantially amorphous. The composite electrical resistivity was observed to be anisotropic with a resistivity of 79 {mu}{Omega} cm measured transverse to the extrusion axis in a sample with 75% amorphous volume fraction. A 0-3 connectivity pattern with the low-resistivity steel phase embedded in a 3-dimensionally connected high-resistivity bulk metallic glass phase was observed with scanning electron microscopy. This confirms that the flow characteristics of the bulk metallic glass and the steel powders were comparable during extrusion at these temperatures. The saturation magnetization of 1.3 T was consistent with the volume weighted average of the saturation magnetization of the two phases. A relatively high quasistatic coercivity of 8 Oe was measured and is likely due to slight crystallization of the bulk metallic glass as well as domain wall pinning at prior particle boundaries. Careful control of the thermal environment during the extrusion process is required to minimize glass crystallization and achieve the desired balance of magnetic and electrical properties.

36 MATERIALS SCIENCE↗

Dislocation engineering in SiGe on periodic and aperiodic Si(001) templates studied by fast scanning X-ray nanodiffraction

Fast-scanning X-ray nanodiffraction microscopy is used to directly visualize the misfit dislocation network in a SiGe film deposited on a pit-patterned Si substrate at the beginning of plastic relaxation. X-ray real-space diffracted intensity maps are compared to topographic atomic force microscopy images, in which crosshatch lines can be seen. The change in intensity distribution as a function of the incidence angle shows localized variations in strain within the SiGe film. These variations, which reflect the order imposed by the substrate pattern, are attributed to the presence of both bunches of misfit dislocations and defect-free regions.

36 MATERIALS SCIENCE↗

Structural and optical properties of DC reactive magnetron sputtered zinc aluminum oxide thin films

Highly transparent conductive Zinc Aluminum Oxide (ZAO) thin films have been deposited on glass substrates using DC reactive magnetron sputtering method. The thin films were deposited at 200 °C and post-deposition annealing from 15 to 90 min. XRD patterns of ZAO films exhibit only (0 0 2) diffraction peak, indicating that they have c-axis preferred orientation perpendicular to the substrate. Scanning electron microscopy (SEM) is used to study the surface morphology of the films. The grain size obtained from SEM images of ZAO thin films are found to be in the range of 20 - 26 nm. The minimum resistivity of 1.74 × 10{sup −4} Ω cm and an average transmittance of 92% are obtained for the thin film post annealed for 30 min. The optical band gap of ZAO thin films increased from 3.49 to 3.60 eV with the increase of annealing time due to Burstein-Moss effect. The optical constants refractive index (n) and extinction coefficient (k) were also determined from the optical transmission spectra.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Synthesis and characterization of porous structured ZnO thin film for dye sensitized solar cell applications

Zinc oxide (ZnO) and zinc oxide/eosin yellow (ZnO/EY) thin films were potentiostatically deposited onto fluorine doped tin oxide (FTO) glass substrate. Effect of eosin yellow dye on structural, morphological and optical properties was studied. X-ray diffraction patterns, micro Raman spectra and photoluminescence (PL) spectra reveal hexagonal wurtzite structure with less atomic defects in 101 plane orientation of the ZnO/EY film. Scanning electron microscopy (SEM) images show flower for ZnO and porous like structure for ZnO/EY thin film, respectively. DSSC was constructed and evaluated by measuring the current density verses voltage curve.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗