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At least 253 records · Page 14

Synthesis and Properties of Porous Ti-20 wt.% HA Nanocomposites

In the present study, porous titanium-20 wt.% hydroxyapatite nanocomposites were produced by the combination of mechanical alloying and powder metallurgical process with the addition of titanium hydride particles as the blowing agent. The powder mixture of Ti, HA and spacer particles were milled, pressed and heat-treated to decompose the hydride particles and to sinter into highly porous Ti-HA materials. The resulting microstructures were characterized using x-ray diffraction and scanning electron microscope with energy-dispersive spectrometry. The porosity, compressive strength and corrosion resistance of the porous nanocomposites were investigated. The results show that the compressive strength of porous Ti-HA can be tailored between 210 and 497 MPa by changing the content of blowing agent between 25 and 75%. The increase in the weight ratio of titanium hydride (from 25 to 75%) causes almost a twofold increase in the porosity and decreases the corrosion resistance (by almost two orders of magnitude). The present study has demonstrated that the porous Ti-HA nanocomposites are promising scaffold biomaterials for bone tissue engineering by virtue of their appropriate mechanical and corrosion properties and highly porous structure.

36 MATERIALS SCIENCE↗

Impact of Li Addition in Al-Rich Alloys on Hydrogen Production in Water

In this study, three types of aluminum alloys (Al-Li, Al-Ga-In-Sn and Al-Li-Ga-In-Sn alloys) were prepared via vacuum arc melting technology. The microstructures of the alloys were examined by x-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDX). The water discharge method was used to evaluate the water–aluminum reaction. The results show that the Al-Li alloy is inert in aqueous ambience, whereas the Al-Ga-In-Sn alloy and Al-Li-Ga-In-Sn alloy rapidly react with water. Meanwhile, the Li addition hinders the aluminum–water reaction mainly due to the formation of AlLi and Li{sub 5}Sn{sub 2} intermetallic compounds, which causes a lower H{sub 2} generation rate and a lower H{sub 2} yield of the Al-Li-Ga-In-Sn alloy than those of the Al-Ga-In-Sn alloy.

36 MATERIALS SCIENCE↗

Anion-exchange membranes derived from quaternized polysulfone and exfoliated layered double hydroxide for fuel cells

Layered double hydroxides (LDH) are prepared by controlling urea assisted homogeneous precipitation conditions. Morphology and crystallinity of LDHs are confirmed by X-ray diffraction and scanning electron microscope. After LDHs are incorporated into quaternized polysulfone membranes, transmission electron microscope is used to observe the exfoliated morphology of LDH sheets in the membranes. The properties of the nanocomposite membranes, including water uptake, swelling ratio, mechanical property and ionic conductivity are investigated. The nanocomposite membrane containing 5% LDH sheets shows more balanced performances, exhibiting an ionic conductivity of 2.36×10{sup −2} S cm{sup −1} at 60 °C. - Graphical abstract: Anion-exchange membrane based on quaternized polysulfone and exfoliated layered double hydroxide is optically transparent and has good ionic properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Growth of different phases and morphological features of MnS thin films by chemical bath deposition: Effect of deposition parameters and annealing

Manganese sulfide thin films have been deposited on glass slides by chemical bath deposition (CBD) method. The effects of preparative parameters such as deposition time, bath temperature, concentration of precursors, multi-layer deposition, different source of manganese, different complexing agent and thermal annealing on structural and morphological film properties have been investigated. The prepared thin films have been characterized using the X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). It exhibit the metastable forms of MnS, the hexagonal γ-MnS wurtzite phase with preferential orientation in the (002) plane or the cubic β-MnS zinc blende with preferential orientation in the (200) plane. Microstructural studies revealed the formation of MnS crystals with different morphologies, such as hexagons, spheres, cubes or flowers like. - Graphical Abstract: We report the preparation of different phases of manganese sulfide thin films (γ, β and α-MnS) by chemical bath deposition method. The effects of deposition parameters such as deposition time and temperature, concentrations of precursors and multi-layer deposition on MnS thin films structure and morphology were investigated. The influence of thermal annealing under nitrogen atmosphere at different temperature on MnS properties was also studied. Different manganese precursors as well as different complexing agent were also used. - Highlights: • γ and β-MnS films were deposited on substrate using the chemical bath deposition. • The effect of deposition parameters on MnS film properties has been investigated. • Multi-layer deposition was also studied to increase film thickness. • The effect of annealing under N{sub 2} at different temperature was investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High efficiency of isopropanol combustion over cobalt oxides modified ZSM-5 zeolite membrane catalysts on paper-like stainless steel fibers

Catalytic performances of isopropanol combustion and bed pressure drop in structured fixed bed reactor composed of cobalt oxides modified ZSM-5 zeolite membrane catalysts on paper-like stainless steel fibers (Co/ZSM-5/PSSF) and traditional granular ZSM-5 zeolites catalysts were investigated in this paper. Both of the catalyst samples were fabricated by wetness impregnation method and were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectrometer (EDS) mapping and the N{sub 2} adsorption/desorption isotherm analyses. The result of EDS mapping revealed that cobalt oxides dispersed well on ZSM-5/PSSF. The Co/ZSM-5/PSSF catalyst display superior catalytic activity to granular Co/ZSM-5 catalyst, 50% and 90% isopropanol conversion temperatures over Co/ZSM-5/PSSF reduced 107 °C and 51 °C, respectively, compared with those over granular Co/ZSM-5 catalysts. The apparent activation energy for isopropanol combustion over Co/ZSM-5/PSSF (90 kJ/mol) was much lower than that over granular Co/ZSM-5 (134 kJ/mol). When the face velocity increased to 14.9 cm/s, the bed pressure drop of reactor filled with only Co/ZSM-5/PSSF catalysts was 9.5% of that of reactor filled with only granular Co/ZSM-5 catalysts. The ZSM-5 zeolite membrane on paper-like stainless steel fibers support provide good dispersion for cobalt oxides and Co/ZSM-5/PSSF show superior catalytic efficiency of isopropanol combustion and produced lower bed pressure drop in reactor compared with granular ZSM-5 zeolites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Fabrication of Al-Zn solid solution via friction stir processing

Highlights: • Thermomechanical nature of FSP was utilized for mechanical alloying. • Zn particles dissolved in Al during FSP to form solid solution. • Second pass of FSP lead to homogenization and partial decomposition of the solid solution. • Processed alloy exhibited improved hardness over base and FSPed metal. • The process can be adopted for site specific property enhancement. - Abstract: The present study demonstrates that friction stir processing (FSP) can be used as a mechanical alloying tool to process solid solution. Zn was incorporated in commercially pure aluminium by multi-pass FSP leading to its dissolution and formation of supersaturated solid solution which was confirmed by X-ray diffraction and scanning electron microscopy. The hardness across the stir zone matched with the distribution of Zn and was significantly improved compared to the base metal. The supersaturated solid solution that formed in the first pass, partially decomposed during the second pass, leading to the formation of fine Al-Zn precipitates. Thermal stability of the microstructure against abnormal grain growth was also improved after the second pass due to the pinning effect of the grain boundary precipitates. FSP also caused grain refinement of the alloy yielding fine equiaxed grains in the range of 4–6 μm with a high fraction (> 67%) of high angle grain boundaries. Such microstructure is conducive for isotropic properties and the fact that the microstructure is stable against thermal cycles make the process suitable for selective alloying for location specific property enhancement.

36 MATERIALS SCIENCE↗

Formation of Cu{sub 2}O and ZnO Crystal Layers by Magnetron Assisted Sputtering and Their Optical Characterization

Copper (I) oxide and zinc oxide films are formed on silicon and glassy quartz substrates by magnetron assisted sputtering. The thickness of the films is tens and hundreds of nanometers. The films are grown at different substrate temperatures and different oxygen pressures in the working chamber. The film samples are studied by the X-ray diffraction technique, scanning electron microscopy, and optical methods. It is established that an increase in the substrate temperature yields a change in the surface morphology of copper (I) oxide films towards the formation of well-pronounced crystallites. The reflectance and Raman spectra suggest that the quality of such films is close to that of bulk Cu{sub 2}O crystals produced by the oxidation of copper. As concerns ZnO films, an increase in the substrate temperature and an increase in the partial oxygen pressure make it possible to produce films, for which a sharp exciton structure is observed in the reflectance spectra and the emission of excitons bound at donors is observed in the luminescence spectra.

36 MATERIALS SCIENCE↗

Corrosion-induced microstructural developments in 316 stainless steel during exposure to molten Li 2 BeF 4 (FLiBe) salt

The microstructural evaluation and characterization of 316 stainless steel samples that were tested in molten Li 2 BeF 4 (FLiBe) salt were investigated in this study for evaluating its performance in high-temperature molten fluoride salts. Recently, 316 stainless steel and FLiBe salt are being actively considered as the main structural alloy and primary coolant of fluoride salt-cooled high-temperature reactor (FHR), a leading nuclear reactor concept for the next generation nuclear plants (NGNP). In support of the materials development for the FHR, high-temperature corrosion tests of 316 stainless steel in molten FLiBe salt at 700°C have been conducted in both bare graphite crucibles and 316 stainless steel-lined crucibles in an inert atmosphere for up to 3000 hours. The microstructure of the tested samples was comprehensively characterized using scanning electron microscopy (SEM) in conjunction with energy dispersive x-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD), and scanning transmission electron microscopy (STEM) with EDS. In addition to the noticeable intergranular corrosion attack on surface, the corrosion in terms of the Cr depletion along high angle grain boundaries (15-180º) extended to 22µm in depth after 3000-hour exposure to molten FLiBe salt in graphite crucible. The coherent Σ3 grain boundary appeared high resistance to the Cr depletion. The substantial Cr depletion from the near-to-surface layer induced phase transformation from γ-martensite to α-ferrite phase (FeNi x ) during corrosion at 700ºC. Furthermore, the presence of graphite in the molten salt doubled the corrosion attack depth and led to the formation of round Mo2C, hexagonal Cr 7 C 3 and needle-like Al 4 C 3 phase within the alloy as deep as 50 µm after 3000-hour corrosion testing. Based on the microstructural analysis, the corrosion mechanisms of 316 stainless steel in molten FLiBe salt in different corrosion crucibles were illuminated through schematic diagrams. Additionally, a thermal diffusion controlled corrosion model was developed and validated by experimental data for predicting the long-term corrosion attack depth.

36 MATERIALS SCIENCE↗

Relative Role of Particle Size and Shape on the Magnetic and Catalytic Behavior of Nanozinc Chromite

The purpose of this study is to define an effective synthesis for spinel-type zinc chromite (ZnCr{sub 2}O{sub 4}) nanoparticles by a simple microwave combustion method. The synthesized material was analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and from optical properties. A magnetic property for the material was examined through the vibrating sample magnetism. The distribution of the external magnetic lines of force and the self-generated magnetic field of ferromagnetic materials was taken into account in the presence of an external magnetic field. Zinc chromite showed good performances in catalytic oxidation, and the role of particle size and shape is highlighted.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Dielectric Properties and Oxidation Roasting of Molybdenite Concentrate by Using Microwave Energy at 2.45 GHz Frequency

Conversion of electromagnetic energy into heat depends largely on the dielectric properties of the material being treated. Therefore, determining the dielectric properties of molybdenite concentrate and its microwave power penetration depth in relation to a temperature increment at the commercial frequency of 2.45 GHz is necessary to design industrial microwave processing units. In this study, the dielectric constants increased as the temperature increased in the entire experimental range. The loss factor presented an opposite trend, except for 298 K to 373 K (25 °C to 100 °C) in which a cavity perturbation resonator was used. The plots of nonlinear surface fitting indicate that the increase in dielectric loss causes a considerable decrease in penetration depth, but the dielectric constants exert a small positive effect. The thermogravimetric analysis (TGA-DSC) of the molybdenite concentrate was carried out to track its thermal decomposition process, aim to a dielectric analysis during the microwave heating. MoO{sub 3} was prepared from molybdenite concentrate through oxidation roasting in a microwave heating system and a resistance furnace, respectively. The phase transitions and morphology evolutions during oxidation roasting were characterized through X-ray diffraction and scanning electron microscopy. Results show that microwave thermal technique can produce high-purity molybdenum trioxide.

36 MATERIALS SCIENCE↗

Sulfate performance of blended cements (limestone and illite calcined clay) exposed to aggressive environment after casting

This paper evaluates how early aggressive exposure affects the sulfate resistance of blended cements containing limestone filler and/or calcined clay. Mortar and cement paste specimens were elaborated with different combinations of limestone filler and two different illitic calcined clays and exposed to a sodium sulfate solution shortly after casting. Assessment of sulfate resistance was based on expansion, mass variation, and compressive strength. Microscale evolution and distribution were examined by mercury intrusion porosimetry, X-ray diffraction, and scanning electron microscopy with energy-dispersive spectrometry measurements. Results prove superior sulfate resistance of compositions with high calcined clay content over limestone filler addition. Furthermore, the results reported suggest that the pozzolanic reaction progresses enough to reduce the sulfate ingress even at early exposure conditions. Therefore, calcined clay replacement can still provide effective pore refinement to limit sulfate penetration, increase strength, and reduce available CH to limit expansive phase formation.

36 MATERIALS SCIENCE↗

Effect of reaction atmosphere on structural and optical properties of hexagonal molybdenum oxide (h-MoO{sub 3})

The present work aims to synthesize single phase h-MoO{sub 3} nanocrytals by chemical precipitation method exposed under different reaction atmospheres. The reaction atmosphere have been successfully tuned as air, nitrogen and argon and studied its effects on structural, functional, morphology and optical properties by using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and diffuse reflectance spectroscopy (DRS) measurements. The XRD result indicates that the sample exhibits characteristic hexagonal phase of MoO{sub 3}. The crystallite size is estimated by well known Scherrer’s method. The crystallite size is relative small in the case of sample prepared at argon atmosphere. The functional groups such as Mo-O, N-H and O-H are identified from FT-IR spectroscopy. The particle exhibits rod like morphology with perfect hexagonal cross-section. The optical absorption observed at 420-450 nm corresponds to fundamental optical absorption by h-MoO{sub 3}. The band gap values are estimated using Kublka-Munk (K-M) function and found to be 2. 87 eV, 2.93 eV and 2.97 eV for samples synthesized under air, nitrogen and argon, respectively.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

In situ XAS study of the local structure of the nano-Li 2 FeSiO 4 /C cathode

Despite the challenges in achieving its full theoretical capacity of reversible extraction of two Li ions, the Li 2 FeSiO 4 (LFS) cathode shows a remarkable cycling stability once its low electronic conductivity is addressed. By studying the local structure around the iron during electrochemical cycling using in situ x-ray absorption spectroscopy (XAS), it is possible to gain insight into the factors which determine the electrochemical properties of this material. In order to practically perform in situ XAS studies, the charge/discharge of LFS was maximized using two approaches: (a) reducing the particle size of LFS samples from micro-scale to nano-scale in order to reduce the diffusion path for intercalating ions; and (b) applying a conductive coating to each nanoparticle to facilitate electron transfer. A family of LFS materials was synthesized and characterized using x-ray diffraction, and scanning electron microscopy with energy dispersive analysis for structural and morphological analysis, as well as cyclic voltammetry and cycling tests for electrochemical performance diagnosis. This material was then characterized by in situ XAS. The results provide insight into the stable electrochemical performance of LFS and suggest new synthetic routes to reaching the theoretical capacity.

25 ENERGY STORAGE↗

Effect of the Oxygen Content on the Local Environment of Fe Atoms in Anion-Deficient SrFeO{sub 3 – δ}

The specific features of the structure in a polycrystalline anion-deficient strontium ferrite SrFeO{sub 3 – δ} have been studied at different oxygen contents by the Mössbauer spectroscopy, X-ray diffraction, and scanning electron microscopy. Three compounds with different compositions have been prepared in the dependence on the condition of heat treatment. Within each of the structures, there are several nonequivalent positions of Fe corresponding to different valence states of Fe and different local oxygen environments, the relation and the degree of distortion of which are changed in the dependence on the oxygen content. Based on the Mössbauer data, the oxygen content in each of the structures is estimated. Yet another ideal Sr{sub 16}Fe{sub 16}O{sub 45} composition of the SrFeO{sub 3 – δ} compound is proposed for an intermediate composition in addition to those available in the literature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Benchmark Analysis on Magnetic and Photoluminescence Properties of Selective Metal Ions Doped ZnS Nanoparticles

The creation of diluted magnetic semiconductors (DMSs) at lower dimensions that exhibit room temperature ferromagnetism (RTFM) has been given immense significance for the fabrication of a new class of spintronic devices through utilizing spin degrees of freedom besides charge nature of electrons. In this view, nanocrystals of ZnS doped with 4% concentration of Fe, Co, Ni, Cr, Mn, Sr, Cu, and Ce have been synthesized at room temperature (RT) by chemical co-precipitation method. The samples were examined by various characterization techniques like energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM), and photoluminescence (PL). EDS spectra revealed the existence of parent elements in the prepared samples. XRD characterization disclosed hexagonal structures of nanocrystals, and no secondary phases were observed in all the samples except for Cu and Ni doped ZnS. FTIR data confirmed the proper substitution of dopants in the host lattice as all the graphs have almost same stretchings. The magnetic nature of each sample was evaluated from M-H graphs of VSM, and it corroborated the transition of magnetic properties due to doping. Pristine ZnS showed diamagnetic nature, while Fe and Sr doped ZnS evinced strong ferromagnetic and anti-ferromagnetic properties, respectively. Photoluminescence studies on Ce, Sr and Mn doped ZnS samples revealed strong emission peaks with enhanced luminescence properties compared to bare ZnS. Cu, Cr and Mn doped ZnS exhibited a red shift in emission wavelengths, whereas Co doped ZnS showed emission peak shifted towards the blue region as compared to the host lattice.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Exotic Long-Range Surface Reconstruction on La 0.7 Sr 0.3 MnO 3 Thin Films

Due to an extremely diverse phase space, La 1–x Sr x MnO 3 , as with other manganites, offers a wide range of tunability and applications including colossal magnetoresistance and use as spin-polarized electrodes. Here, we study an unprecedented, exotic surface reconstruction (6 × 6) in La 1–x Sr x MnO 3 (x = 0.3) observed via low-energy electron diffraction (LEED). Scanning tunneling microscopy (STM) shows the surface is relatively flat, with unit-cell step heights, and X-ray photoelectron spectroscopy (XPS) reveals a strong degree of Sr segregation at the surface. By combining electron diffraction and first-principles computations, we propose that the long-range surface reconstruction consists of a Sr-segregated surface with La (6 × 6) ordering. This study expands our understanding of manganite systems and underscores their ability to form interesting surface reconstructions, driven largely by cation segregation that can potentially be controlled for tuning surface ordering.

36 MATERIALS SCIENCE↗

Antibacterial and Structural Properties and Printability of Starch/Clay/Polyethylene Composite Films

A composite of thermoplastic starch (TPS), low-density polyethylene (LDPE) and citric acid-modified montmorillonite (CMMT) was prepared in a twin screw extruder for packaging film application. Starch was first converted to the thermoplastic state by using sorbitol and water. Composite films were produced on a chill roll system and then were modified for printability by grafting of acrylonitrile onto the starch backbone. Antimicrobial property and printability of the films were studied from which the sample with the highest antimicrobial property and the best printability was selected. This optimal sample was then characterized by Fourier transform infrared, thermal gravimetric analysis, differential scanning calorimetry, X-ray diffraction, and scanning electron microscopy. The composite film showed a matrix/dispersed morphology in which LDPE formed a continuous phase and TPS/CMMT nanocomposite particles appeared as dispersed phase. Biodegradability, water absorption, oxygen permeability, tensile strength and transparency of optimal film were also studied. The results indicated very good properties of the produced composite film for packaging application. Graphical Abstract: .

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effect of Y{sub 2}BaCuO{sub 5} Nanoparticle Doping on Critical Current Density of YBa{sub 2}Cu{sub 3}O{sub 7-δ} Bulk Superconductor

This study presents the effect of Y{sub 2}BaCuO{sub 5} (Y211) nanoparticle doping on critical current density and critical temperature of YBa{sub 2}Cu{sub 3}O{sub 7-δ} (YBCO) superconductor. Y211 nanoparticles with different particle sizes ranging from 34 to 455 nm were synthesized by a sol-gel method, then doped into the YBCO superconductor by 0.5, 1, and 2 wt.%. Samples were characterized using X-ray diffraction and scanning electron microscope measurements. The standard four-probe technique was used to measure the critical current density at 77 K. The results showed that in the all-doped samples, critical current density was higher than that of the pure sample. It was found that in the samples containing 1 and 2 wt.% of Y211 nanoparticles, by increasing the size of nanoparticles, the J{sub c} was increased, but in samples containing 0.5 wt.%, the J{sub c} decreased. The maximum critical current density of 64 A/cm {sup 2} was obtained for the samples doped with 2 wt.% of 455 nm Y211 nanoparticles. Also, it was observed that the critical temperature slightly decreased with nanoparticle doping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗