Search results for: X-Ray Diffraction

Authors: Chang-Hung Hsu, Yeong-Hwa Chang, Chun-Yao Lee, Chia-Shiang Yao, Yan-Lou He, Huei-Lung Chu, Chia-Wen Chang, Wei-Shou Chan

Abstract:

This study reports the preparation of soft magnetic ribbons of Fe-based amorphous alloys using the single-roller melt-spinning technique. Ribbon width varied from 142 mm to 213 mm and, with a thickness of approximately 22 μm ± 2 μm. The microstructure and magnetic properties of the ribbons were characterized by differential scanning calorimeter (DSC), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and electrical resistivity measurements (ERM). The amorphous material properties dependence of the cooling rate and nozzle pressure have uneven surface in ribbon thicknesses are investigated. Magnetic measurement results indicate that some region of the ribbon exhibits good magnetic properties, higher saturation induction and lower coercivity. However, due to the uneven surface of 213 mm wide ribbon, the magnetic responses are not uniformly distributed. To understand the transformer magnetic performances, this study analyzes the measurements of a three-phase 2 MVA amorphous-cored transformer. Experimental results confirm that the transformer with a ribbon width of 142 mm has better magnetic properties in terms of lower core loss, exciting power, and audible noise.

Keywords: Amorphous ribbon, uneven surface, magnetic properties, and rapid solidification

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Authors: A. M. Metak, T. T. Ajaal

Abstract:

Commercial nanocomposite food packaging type nano-silver containers were characterised using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The presence of nanoparticles consistent with the incorporation of 1% nano-silver (Ag) and 0.1% titanium dioxide (TiO₂) nanoparticle into polymeric materials formed into food containers was confirmed. Both nanomaterials used in this type of packaging appear to be embedded in a layered configuration within the bulk polymer. The dimensions of the incorporated nanoparticles were investigated using X-ray diffraction (XRD) and determined by calculation using the Scherrer Formula; these were consistent with Ag and TiO₂ nanoparticles in the size range 20-70nm both were spherical shape nanoparticles. Antimicrobial assessment of the nanocomposite container has also been performed and the results confirm the antimicrobial activity of Ag and TiO₂ nanoparticles in food packaging containers. Migration assessments were performed in a wide range of food matrices to determine the migration of nanoparticles from the packages. The analysis was based upon the relevant European safety Directives and involved the application of inductively coupled plasma mass spectrometry (ICP-MS) to identify the range of migration risk. The data pertain to insignificance levels of migration of Ag and TiO₂ nanoparticles into the selected food matrices.

Keywords: Nano-silver, antimicrobial food packaging, migration, titanium dioxide.

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Authors: Roozbeh Mansouri, Hassan Hadidi

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Truss spars are used for oil exploitation in deep and ultra-deep water if storage crude oil is not needed. The linear hydrodynamic analysis of truss spar in random sea wave load is necessary for determining the behaviour of truss spar. This understanding is not only important for design of the mooring lines, but also for optimising the truss spar design. In this paper linear hydrodynamic analysis of truss spar is carried out in frequency domain. The hydrodynamic forces are calculated using the modified Morison equation and diffraction theory. Added mass and drag coefficients of truss section computed by transmission matrix and normal acceleration and velocity component acting on each element and for hull section computed by strip theory. The stiffness properties of the truss spar can be separated into two components; hydrostatic stiffness and mooring line stiffness. Then, platform response amplitudes obtained by solved the equation of motion. This equation is non-linear due to viscous damping term therefore linearised by iteration method [1]. Finally computed RAOs and significant response amplitude and results are compared with experimental data.

Keywords: Truss Spar, Hydrodynamic analysis, Wave spectrum, Frequency Domain

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Authors: A. I. M. Ismail, N. Ryden

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This paper is concerned with the study of mineralogy and engineering characteristics of soil materials derived from the eastern part of Nile Delta. The clay minerals of the studied soil by using X- ray diffraction are mainly illite (average 72.6 %) and kaolinite (average 2.6 %), expandable portion in illite-smectite mixed layer (average 7 %). Smectite is more abundant in fluviatile clays, whereas kaolinite is more abundant in lagoonal clays. On the other hand, illite and illite-smectite are more abundant in marine clays. The geotechnical results show that the soil under study consists mainly of about 0.3 % gravel, 5 % sand, 51.5 % silt and 42.2 % clay in average. The average shrinkage limit attains 11 % whereas the average value of the plasticity index is 23.4 %. The free swelling ranges from 40 % to 75 % and has a value of 55 % giving an indication about the inadequacy of such soil under foundations. From a construction point of view, the soil under investigation poses many problems even under light foundations due to the swelling and shrinkage. Such swelling and shrinkage is due to the high content of soil materials in the expandable clay minerals of illite and smectite. Based on the results of the present and earlier studies, trial application of soil stabilisation is recommended.

Keywords: Engineering Geological Investigations, Nile Delta, Swelling, Shrinkage

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Authors: Sefiu A. Bello, Nasirudeen K. Raji, Jeleel A. Adebisi, Sadiq A. Raji

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Pure metals are not used in most cases for structural applications because of their limited properties. Presently, high entropy alloys (HEAs) are emerging by mixing comparative proportions of metals with the aim of maximizing the entropy leading to enhancement in structural and mechanical properties. Aluminum Silicon Nickel Iron Vanadium (AlSiNiFeV) alloy was developed using stir cast technique and analysed. Results obtained show that the alloy grade G0 contains 44 percentage by weight (wt%) Al, 32 wt% Si, 9 wt% Ni, 4 wt% Fe, 3 wt% V and 8 wt% for minor elements with tensile strength and elongation of 106 Nmm^-2 and 2.68%, respectively. X-ray diffraction confirmed intermetallic compounds having hexagonal closed packed (HCP), orthorhombic and cubic structures in cubic dendritic matrix. This affirmed transformation from the cubic structures of elemental constituents of the HEAs to the precipitated structures of the intermetallic compounds. A maximum tensile strength of 188 Nmm^-2 with 4% elongation was noticed at 10wt% of silica addition to the G0. An increase in tensile strength with an increment in silica content could be attributed to different phases and crystal geometries characterizing each HEA.

Keywords: High entropy alloys, phases, model, tensile strength.

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Authors: S. U. Khan, T. Ayub, N. Shafiq

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The properties of locally produced metakaolin (MK) as cement replacing material and the comparison of reactivity with commercially available micro-silica have been investigated. Compressive strength, splitting tensile strength, and load-deflection behaviour under bending are the properties that have been studied. The amorphous phase of MK with micro-silica was compared through X-ray diffraction (XRD) pattern. Further, interfacial transition zone of concrete with micro-silica and MK was observed through Field Emission Scanning Electron Microscopy (FESEM). Three mixes of concrete were prepared. One of the mix is without cement replacement as control mix, and the remaining two mixes are 10% cement replacement with micro-silica and MK. It has been found that MK, due to its irregular structure and amorphous phase, has high reactivity with portlandite in concrete. The compressive strength at early age is higher with MK as compared to micro-silica. MK concrete showed higher splitting tensile strength and higher load carrying capacity as compared to control and micro-silica concrete at all ages respectively.

Keywords: Metakaolin, compressive strength, splitting tensile strength, load deflection, interfacial transition zone.

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Authors: B. Dikici, I. Ozdemir, M. Topuz

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The corrosion behaviour of 316L stainless steel coatings obtained by cold spray method was investigated in this study. 316L powders were deposited onto Al5052 aluminum substrates. The coatings were produced using nitrogen (N₂) process gas. In order to further improve the corrosion and mechanical properties of the coatings, heat treatment was applied at 250 and 750 °C. The corrosion performances of the coatings were compared using the potentiodynamic scanning (PDS) technique under in-vitro conditions (in Ringer’s solution at 37 °C). In addition, the hardness and porosity tests were carried out on the coatings. Microstructural characterization of the coatings was carried out by using scanning electron microscopy attached with energy dispersive spectrometer (SEM-EDS) and X-ray diffraction (XRD) technique. It was found that clean surfaces and a good adhesion were achieved for particle/substrate bonding. The heat treatment process provided both elimination of the anisotropy in the coating and resulting in healing-up of the incomplete interfaces between the deposited particles. It was found that the corrosion potential of the annealed coatings at 750 °C was higher than that of commercially 316 L stainless steel. Moreover, the microstructural investigations after the corrosion tests revealed that corrosion preferentially starts at inter-splat boundaries.

Keywords: 316L, biomaterials, cold spray, heat treatment.

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Authors: Rana Th. A. Al-Rubaye, Burcin Atilgan, Richard J. Holmes, Arthur A. Garforth

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Structured catalysts formed from the growth of zeolites on substrates is an area of increasing interest due to the increased efficiency of the catalytic process, and the ability to provide superior heat transfer and thermal conductivity for both exothermic and endothermic processes. However, the generation of structured catalysts represents a significant challenge when balancing the relationship variables between materials properties and catalytic performance, with the Na2O, H2O and Al2O3 gel composition paying a significant role in this dynamic, thereby affecting the both the type and range of application. The structured catalyst films generated as part of this investigation have been characterised using a range of techniques, including X-ray diffraction (XRD), Electron microscopy (SEM), Energy Dispersive X-ray analysis (EDX) and Thermogravimetric Analysis (TGA), with the transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces being demonstrated using both SEM and XRD. The robustness of the coatings has been ascertained by subjecting these to thermal cycling (ambient to 550oC), with the results indicating that the synthesis time and gel compositions have a crucial effect on the quality of zeolite growth on the FeCrAlloy wires. Finally, the activity of the structured catalyst was verified by a series of comparison experiments with standard zeolite Y catalysts in powdered pelleted forms.

Keywords: FeCrAlloy, Structured catalyst, and Zeolite Y.

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Authors: S. Guettala, B. Mezghiche

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In this paper, the effect of addition the dune sand powder (DSP) on development of compressive strength and hydration of cement pastes was investigated as a function of water/binder ratio, was varied, on the one hand, the percentage of DSP and on the other, the fineness of DSP. In order to understand better the pozzolanic effect of dune sand powder in cement pastes, we followed the mixtures hydration (50% Pure Lime + 50% DSP) by X-ray diffraction. These mixtures the pastes present a hydraulic setting which is due to the formation of a C-S-H phase (calcium silicate hydrate). The latter is semi-crystallized. This study is a simplified approach to that of the mixtures (80% ordinary Portland cement + 20% DSP), in which the main reaction is the fixing of the lime coming from the cement hydration in the presence of DSP, to form calcium silicate hydrate semi-crystallized of second generation. The results proved that up to (20% DSP) as Portland cement replacement could be used with a fineness of 4000 cm²/g without affecting adversely the compressive strength. After 28 days, the compressive strength at 5, 10 and 15% DSP is superior to Portland cement, with an optimum effect for a percentage of the order of 5% to 10% irrespective of the w/b ratio and fineness of DSP.

Keywords: Ordinary Portland Cement, Pure Lime, Dune Sand Powder, Compressive Strength, Hydration.

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Authors: Z. Abdolldhi, A. A. Ziaee M., A. Afshar

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In this paper the combination of thermal oxidation and electrochemical anodizing processes is used to produce titanium oxide layers. The response of titanium alloy Ti6Al4V to oxidation processes at various temperatures and electrochemical anodizing in various voltages are investigated. Scanning electron microscopy (SEM); X-Ray Diffraction (XRD) and porosity determination have been used to characterize the oxide layer thickness, surface morphology, oxide layer-substrate adhesion and porosity. In the first experiment, samples modified by thermal oxidation process then followed by electrochemical anodizing. Second experiment consists of surfaces modified by electrochemical anodizing process and then followed by thermal oxidation. The first method shows better properties than other one. In second experiment, Surfaces modified were achieved by thicker and more adherent thick oxide layers on titanium surface. The existence of an electrochemical anodized oxide layer did not improve the adhesion of thermal oxide layer. The high temperature, thermal formation of an oxide layer leads to a coarse oxide grain morphology and a complete oxidative particle. In addition, in high temperature oxidation porosity content is increased. The oxide layer of thermal oxidation and electrochemical anodizing processes; on Ti–6Al–4V substrate was covered with different colored oxide layers.

Keywords: Electrochemically anodizing, Porosity, Thermaloxidation, Ti6Al4 alloy.

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Authors: D.N Awang Sh'ri, E. Hamzah

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The deposition of diamond films on a Si3N4 substrate is an attractive technique for industrial applications because of the excellent properties of diamond. Pretreatment of substrate is very important prior to diamond deposition to promote nucleation and adhesion between coating and substrate. Deposition of nanocrystalline diamonds films on silicon nitride substrate have been carried out by HF-CVD technique using mixture of methane and hydrogen gases. Different pretreatment of substrate including chemical etching consists of hot acid etching and basic etching and mechanical etching were used to study the quality of diamond formed on the substrate. The structure and morphology of diamond coating have been studied using X-ray Diffraction (XRD) and Scanning Electron Microscope (SEM) while diamond film quality has been characterized using Raman spectroscopy. AFM was used to investigate the effect of chemical etching and mechanical pretreatment on the surface roughness of the substrates and the resultant morphology of nanocrystalline diamond. It was found that diamond film deposited on as-received, basic etched and grinded substrate shows the morphology of cauliflower while blasted and acidic etched substrates produce smooth, continuous diamond film. However, the Raman investigation did not show any deviation in quality of diamond film for any pretreatment.

Keywords: Nanocrystalline diamond, Chemical VaporDeposition, Pretreatment, Silicon Nitride

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Authors: Martin Klaumünzer, Jakob Hübner, Denis Spitzer

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Within this paper, latest results on processing of energetic nanomaterials by means of the Spray Flash Evaporation technique are presented. This technology constitutes a highly effective and continuous way to prepare fascinating materials on the nano- and micro-scale. Within the process, a solution is set under high pressure and sprayed into an evacuated atomization chamber. Subsequent ultrafast evaporation of the solvent leads to an aerosol stream, which is separated by cyclones or filters. No drying gas is required, so the present technique should not be confused with spray dying. Resulting nanothermites, insensitive explosives or propellants and compositions are foreseen to replace toxic (according to REACH) and very sensitive matter in military and civil applications. Diverse examples are given in detail: nano-RDX (n-Cyclotrimethylentrinitramin) and nano-aluminum based systems, mixtures (n-RDX/n-TNT - trinitrotoluene) or even cocrystalline matter like n-CL-20/HMX (Hexanitrohexaazaisowurtzitane/ Cyclotetra-methylentetranitramin). These nanomaterials show reduced sensitivity by trend without losing effectiveness and performance. An analytical study for material characterization was performed by using Atomic Force Microscopy, X-Ray Diffraction, and combined techniques as well as spectroscopic methods. As a matter of course, sensitivity tests regarding electrostatic discharge, impact, and friction are provided.

Keywords: Continuous synthesis, energetic material, nanoscale, nanothermite, nanoexplosive.

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Authors: Seyed Mohammad Hosseini, Amirhossein Moghanian

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The main purpose of this research was to design a biomimetic system by freeze-drying method for evaluating the effect of adding 5 and 10 mol. % of zinc (Zn) in 58S bioactive glass and gelatin (5ZnBG/G and 10ZnBG/G) in terms of structural and biological changes. The structural analyses of samples were performed by X-Ray Diffraction (XRD), scanning electron microscopy (SEM) and Fourier-transform infrared (FTIR) spectroscopy. Also, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and alkaline phosphatase (ALP) activity tests were carried out for investigation of MC3T3-E1 cell behaviors. The SEM results demonstrated the spherical shape of the formed hydroxyapatite (HA) phases and also HA characteristic peaks were detected by XRD spectroscopy after 3 days of immersion in the simulated body fluid (SBF) solution. Meanwhile, FTIR spectra proved that the intensity of P–O peaks for 5ZnBG/G was more than 10ZnBG/G and control samples. Moreover, the results of ALP activity test illustrated that the optimal amount of Zn (5ZnBG/G) caused a considerable enhancement in bone cell growth. Taken together, the scaffold with 5 mol.% Zn was introduced as an optimal sample because of its higher biocompatibility, in vitro bioactivity and growth of MC3T3-E1 cells in comparison with other samples in bone tissue engineering.

Keywords: Scaffold, gelatin, modified bioactive glass, ALP, bone tissue engineering.

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Authors: Savvas Varitis, Panagiotis Kavouras, George Vourlias, Eleni Pavlidou, Theodoros Karakostas, Philomela Komninou

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A chromium-loaded ash originating from incineration of tannery sludge under anoxic conditions was mixed with low grade soda-lime glass powder coming from commercial glass bottles. The relative weight proportions of ash over glass powder tested were 30/70, 40/60 and 50/50. The solid mixtures, formed in green state compacts, were sintered at the temperature range of 800o C up to 1200o C. The resulting products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDXS) and micro-indentation. The above methods were employed to characterize the various phases, microstructure and hardness of the produced materials. Thermal treatment at 800o C and 1000o C produced opaque ceramic products composed of a variety of chromium-containing and chromium-free crystalline phases. Thermal treatment at 1200o C gave rise to composite products, where only chromium-containing crystalline phases were detected. Hardness results suggest that specific products are serious candidates for structural applications.

Keywords: Chromium-rich tannery residues, glass-ceramic materials, mechanical properties, microstructure

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Authors: Chun-Ying Lee, Kuan-Hui Cheng, Mei-Wen Wu

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The nickel-manganese (Ni-Mn) alloy coating prepared from DC electrodeposition process in sulphamate bath was studied. The effects of process parameters, such as current density and electrolyte composition, on the cathodic current efficiency, microstructure, internal stress and mechanical properties were investigated. Because of its crucial effect on the application to the electroforming of microelectronic components, the development of low internal stress coating with high leveling power was emphasized. It was found that both the coating’s manganese content and the cathodic current efficiency increased with the raise in current density. In addition, the internal stress of the deposited coating showed compressive nature at low current densities while changed to tensile one at higher current densities. Moreover, the metallographic observation, X-ray diffraction measurement, and polarization curve measurement were conducted. It was found that the Ni-Mn coating consisted of nano-sized columnar grains and the maximum hardness of the coating was associated with (111) preferred orientation in the microstructure. The grain size was refined along with the increase in the manganese content of the coating, which accordingly, raised its hardness and resistance to annealing softening. In summary, the Ni-Mn coating prepared at lower current density of 1-2 A/dm2 had low internal stress, high leveling power, and better corrosion resistance.

Keywords: DC plating, internal stress, leveling power, Ni-Mn coating.

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Authors: Hoda Aleali, Nastaran Mansour, Maryam Mirzaie

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In this paper, we study the optical nonlinearities of Silver sulfide (Ag2S) nanostructures dispersed in the Dimethyl sulfoxide (DMSO) under exposure to 532 nm, 15 nanosecond (ns) pulsed laser irradiation. Ultraviolet–visible absorption spectrometry (UV-Vis), X-ray diffraction (XRD), and transmission electron microscopy (TEM) are used to characterize the obtained nanocrystal samples. The band gap energy of colloid is determined by analyzing the UV–Vis absorption spectra of the Ag2S NPs using the band theory of semiconductors. Z-scan technique is used to characterize the optical nonlinear properties of the Ag2S nanoparticles (NPs). Large enhancement of two photon absorption effect is observed with increase in concentration of the Ag2S nanoparticles using open Zscan measurements in the ns laser regime. The values of the nonlinear absorption coefficients are determined based on the local nonlinear responses including two photon absorption. The observed aperture dependence of the Ag2S NP limiting performance indicates that the nonlinear scattering plays an important role in the limiting action of the sample. The concentration dependence of the optical liming is also investigated. Our results demonstrate that the optical limiting threshold decreases with increasing the silver sulfide NPs in DMSO.

Keywords: Nanoscale materials, Silver sulfide nanoparticles, Nonlinear absorption, Nonlinear scattering, Optical limiting.

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Authors: Gul Afreen, Sreedevi Upadhyayula, Mahendra K. Sunkara

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One-dimensional (1D) nanostructures like nanowires, nanotubes, and nanorods find variety of practical application owing to their unique physico-chemical properties. In this work, TiO₂ nanowires were synthesized by direct oxidation of titanium particles in a unique microwave plasma jet reactor. The prepared TiO₂ nanowires manifested the flexible features, and were characterized by using X-ray diffraction, Brunauer-Emmett-Teller (BET) surface area analyzer, UV-Visible and FTIR spectrophotometers, Scanning electron microscope, and Transmission electron microscope. Further, the photodegradation efficiency of these nanowires were tested against toxic organic dye like methylene blue (MB) and the results were compared with the commercial TiO₂. It was found that TiO₂ nanowires exhibited superior photocatalytic performance (89%) as compared to commercial TiO₂ (75%) after 60 min of reaction. This is attributed to the lower recombination rate and increased interfacial charge transfer in TiO₂ nanowire. Pseudo-first order kinetic modelling performed with the experimental results revealed that the rate constant of photodegradation in case of TiO₂ nanowire was 1.3 times higher than that of commercial TiO₂. Superoxide radical (O₂˙⁻) was found to be the major contributor in the photodegradation mechanism. Based on the trapping experiments, a plausible mechanism of the photocatalytic reaction is discussed.

Keywords: Heterogeneous catalysis, photodegradation, reactive oxygen species, TiO2 nanowires.

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: Ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy.

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Authors: Xingwen Lu, Kaimin Shih

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This study investigated a strategy of blending lead-laden sludge and Al-rich precursors to reduce the release of metals from the stabilized products. Using PbO as the simulated lead-laden sludge to sinter with γ-Al2O3 by Pb:Al molar ratios of 1:2 and 1:12, PbAl2O4 and PbAl12O19 were formed as final products during the sintering process, respectively. By firing the PbO + γ-Al2O3 mixtures with different Pb/Al molar ratios at 600 to 1000 °C, the lead transformation was determined through X-ray diffraction (XRD) data. In Pb/Al molar ratio of 1/2 system, the formation of PbAl2O4 is initiated at 700 °C, but an effective formation was observed above 750 °C. An intermediate phase, Pb9Al8O21, was detected in the temperature range of 800-900 °C. However, different incorporation behavior for sintering PbO with Al-rich precursors at a Pb/Al molar ratio of 1/12 was observed during the formation of PbAl12O19 in this system. In the sintering process, both temperature and time effect on the formation of PbAl2O4 and PbAl12O19 phases were estimated. Finally, a prolonged leaching test modified from the U.S. Environmental Protection Agency-s toxicity characteristic leaching procedure (TCLP) was used to evaluate the durability of PbO, Pb9Al8O21, PbAl2O4 and PbAl12O19 phases. Comparison for the leaching results of the four phases demonstrated the higher intrinsic resistance of PbAl12O19 against acid attack.

Keywords: Sludge, Lead, Stabilization, Leaching behavior

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Authors: G.Vinitha, A.Ramalingam

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TiO2 nanoparticles were synthesized by hydrothermal method at 180°C from TiOSO4 aqueous solution with1m/l concentration. The obtained products were coated with silica by means of a seeded polymerization technique for a coating time of 1440 minutes to obtain well defined TiO2@SiO2 core-shell structure. The uncoated and coated nanoparticles were characterized by using X-Ray diffraction technique (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) to study their physico-chemical properties. Evidence from XRD and FTIR results show that SiO2 is homogenously coated on the surface of titania particles. FTIR spectra show that there exists an interaction between TiO2 and SiO2 and results in the formation of Ti-O-Si chemical bonds at the interface of TiO2 particles and SiO2 coating layer. The non linear optical limiting properties of TiO2 and TiO2@SiO2 nanoparticles dispersed in ethylene glycol were studied at 532nm using 5ns Nd:YAG laser pulses. Three-photon absorption is responsible for optical limiting characteristics in these nanoparticles and it is seen that the optical nonlinearity is enhanced in core-shell structures when compared with single counterparts. This effective three-photon type absorption at this wavelength, is of potential application in fabricating optical limiting devices.

Keywords: hydrothermal method, optical limiting devicesseeded polymerization technique, three-photon type absorption

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Authors: Chen-Fu Wang, Lin-Ya Kung

Abstract:

For traditional painting materials, the artisan used to combine the pigments with different binders to create colors. As time goes by, the materials used for painting evolved from natural to chemical materials. The vast variety of ingredients used in chemical materials has complicated restoration work; it makes conservation work more difficult. Conservation work also becomes harder when the materials cannot be easily identified; therefore, it is essential that we take a more scientific approach to assist in conservation work. Paintings materials are high molecular weight polymer, and their analysis is very complicated as well other contamination such as smoke and dirt can also interfere with the analysis of the material. The current methods of composition analysis of painting materials include Fourier transform infrared spectroscopy (FT-IR), mass spectrometer, Raman spectroscopy, X-ray diffraction spectroscopy (XRD), each of which has its own limitation. In this study, FT-IR was used to analyze the components of the paint coating. We have taken the most commonly seen materials as samples and deteriorated it. The aged information was then used for the database to exam the temple painting materials. By observing the FT-IR changes over time, we can tell all of the painting materials will be deteriorated by the UV light, but only the speed of its degradation had some difference. From the deterioration experiment, the acrylic resin resists better than the others. After collecting the painting materials aging information on FT-IR, we performed some test on the paintings on the temples. It was found that most of the artisan used tune-oil for painting materials, and some other paintings used chemical materials. This method is now working successfully on identifying the painting materials. However, the method is destructive and high cost. In the future, we will work on the how to know the painting materials more efficiently.

Keywords: Temple painting, painting material, conservation, FT-IR.

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: Ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements.

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Authors: Erfan Asghari Fesaghandis, Reza Ghaffari Adli, Abbas Kianvash, Hossein Aghajani, Homa Homaie

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NiTi alloys possess magnificent superelastic, shape memory, high strength and biocompatible properties. For improving mechanical properties, foremost, superelasticity behavior, heat treatment process is carried out. In this paper, two different heat treatment methods were undertaken: (1) solid solution, and (2) aging. The effect of each treatment in a constant time is investigated. Five samples were prepared to study the structure and optimize mechanical properties under different time and temperature. For measuring the upper plateau stress, lower plateau stress and residual strain, tensile test is carried out. The samples were aged at two different temperatures to see difference between aging temperatures. The sample aged at 500 °C has a bigger crystallite size and lower amount of Ni which causes the mentioned sample to possess poor pseudo elasticity behaviour than the other aged sample. The sample aged at 460 °C has shown remarkable superelastic properties. The mentioned sample’s higher plateau is 580 MPa with the lowest residual strain (0.17%) while other samples have possessed higher residual strains. X-ray diffraction was used to investigate the produced phases.

Keywords: Heat treatment, phase transformation, superelasticity, NiTi alloy.

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Authors: N. H. Abd Raof, H. Abu Hassan, S.K. Mohd Bakhori, S. S. Ng, Z. Hassan

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Quaternary InxAlyGa1-x-yN semiconductors have attracted much research interest because the use of this quaternary offer the great flexibility in tailoring their band gap profile while maintaining their lattice-matching and structural integrity. The structural and optical properties of InxAlyGa1-x-yN alloys grown by molecular beam epitaxy (MBE) is presented. The structural quality of InxAlyGa1-x-yN layers was characterized using high-resolution X-ray diffraction (HRXRD). The results confirm that the InxAlyGa1-x-yN films had wurtzite structure and without phase separation. As the In composition increases, the Bragg angle of the (0002) InxAlyGa1-x-yN peak gradually decreases, indicating the increase in the lattice constant c of the alloys. FWHM of (0002) InxAlyGa1-x-yN decreases with increasing In composition from 0 to 0.04, that could indicate the decrease of quality of the samples due to point defects leading to non-uniformity of the epilayers. UV-VIS spectroscopy have been used to study the energy band gap of InxAlyGa1-x-yN. As the indium (In) compositions increases, the energy band gap decreases. However, for InxAlyGa1-x-yN with In composition of 0.1, the band gap shows a sudden increase in energy. This is probably due to local alloy compositional fluctuations in the epilayer. The bowing parameter which appears also to be very sensitive on In content is investigated and obtained b = 50.08 for quaternary InxAlyGa1-x-yN alloys. From photoluminescence (PL) measurement, green luminescence (GL) appears at PL spectrum of InxAlyGa1-x-yN, emitted for all x at ~530 nm and it become more pronounced as the In composition (x) increased, which is believed cause by gallium vacancies and related to isolated native defects.

Keywords: HRXRD, nitrides, PL, quaternary, UV-VIS.

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Authors: Waranya Pongpaiboon, Warangkana Srichamnong, Supat Chaiyakul

Abstract:

Enzymatic modification of rice flour can produce highly functional derivatives use in food industries. This study aimed to evaluate the physical properties and resistant starch content of rice flour residues hydrolyzed by α-amylase. Rice flour hydrolyzed by α-amylase (60 and 300 u/g) for 1, 24 and 48 hours were investigated. Increasing enzyme concentration and hydrolysis time resulted in decreased rice flour residue’s lightness (L*) but increased redness (a*) and yellowness (b*) of rice flour residues. The resistant starch content and peak viscosity increased when hydrolysis time increased. Pasting temperature, trough viscosity, breakdown, final viscosity, setback and peak time of the hydrolyzed flours were not significantly different (p>0.05). The morphology of native flour was smooth without observable pores and polygonal with sharp angles and edges. However, after hydrolysis, granules with a slightly rough and porous surface were observed and a rough and porous surface was increased with increasing hydrolyzed time. The X-ray diffraction patterns of native flour showed A-type configuration, which hydrolyzed flour showed almost 0% crystallinity indicated that both amorphous and crystalline structures of starch were simultaneously hydrolyzed by α-amylase.

Keywords: α-Amylase, Enzymatic hydrolysis, Pasting properties, Resistant starch

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Authors: Oyugi Ngure Robert, Tabitha A. Amollo, Kallen Mulilo Nalyanya

Abstract:

Nanomaterials have attracted significant attention in research because of their exemplary properties, making them suitable for diverse applications. This paper reports the successful synthesis as well as the structural and optical properties of silver sulfide-reduced graphene oxide (Ag2S-rGO) nanocomposite. The nanocomposite was synthesized by the chemical reduction method. Scanning electron microscopy (SEM) showed that the reduced graphene oxide (rGO) sheets were intercalated within the Ag2S nanoparticles during the chemical reduction process. The SEM images also showed that Ag2S had the shape of nanowires. Further, SEM energy dispersive X-ray (SEM EDX) showed that Ag2S-rGO is mainly composed of C, Ag, O, and S. X-ray diffraction analysis manifested a high crystallinity for the nanowire-shaped Ag2S nanoparticles with a d-spacing ranging between 1.0 Å and 5.2 Å. Thermal gravimetric analysis (TGA) showed that rGO enhances the thermal stability of the nanocomposite. Ag2S-rGO nanocomposite exhibited strong optical absorption in the UV region. The formed nanocomposite is dispersible in polar and non-polar solvents, qualifying it for solution-based device processing. Thus, the surface plasmon resonance effect associated with metallic nanoparticles, strong optical absorption, thermal stability crystallinity and hydrophilicity of the nanocomposite suits it for solar energy conversion applications.

Keywords: Silver sulfide, reduced graphene oxide, nanocomposite, structural properties, optical properties.

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Authors: Keiji Komatsu, Tetsuo Sekiya, Ayumu Toyama, Atsushi Nakamura, Ikumi Toda, Shigeo Ohshio, Hiroyuki Muramatsu, Hidetoshi Saitoh, Atsushi Nakamura, Ariyuki Kato

Abstract:

Yttrium oxide (Y2O3) films have been successfully deposited with yttrium-ethylenediamine tetraacetic acid (EDTA·Y·H) complexes prepared by various milling techniques. The effects of the properties of the EDTA·Y·H complex on the properties of the deposited Y2O3 films have been analyzed. Seven different types of the raw EDTA·Y·H complexes were prepared by various commercial milling techniques such as ball milling, hammer milling, commercial milling, and mortar milling. The milled EDTA·Y·H complexes exhibited various particle sizes and distributions, depending on the milling method. Furthermore, we analyzed the crystal structure, morphology and elemental distribution profile of the metal oxide films deposited on stainless steel substrate with the milled EDTA·Y·H complexes. Depending on the milling technique, the flow properties of the raw powders differed. The X-ray diffraction pattern of all the samples revealed the formation of Y2O3 crystalline phase, irrespective of the milling technique. Of all the different milling techniques, the hammer milling technique is considered suitable for fabricating dense Y2O3 films.

Keywords: Powder sizes and distributions, Flame spray coating techniques, Yttrium oxide.

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Authors: S. Palaniyappan, P. K. Chennam, M. Trautmann, H. Ahmad, T. Mehner, T. Lampke, G. Wagner

Abstract:

In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al₂O₃)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al₂O₃ respectively. Raman spectroscopic analyses produced no characteristic bands of Al₂O₃, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.

Keywords: Al2O3 insulation coating, reactive sputtering, SiC single fiber sensor, single fiber tensile test.

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Authors: S. Sharma, U. Batra, S. Kapoor, A. Dua

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In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the assynthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p<0.0001, two way ANOVA), however, these were independent of TEA addition (p>0.15, two way ANOVA). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p<0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.

Keywords: Capping agent, hydroxyapatite, regression analysis, sol-gel, 2- sample t-test, two-way ANOVA.

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Authors: Rana Th. A. Al-Rubaye, Arthur A. Garforth

Abstract:

This work details the generation of thin films of structured zeolite catalysts (ZSM–5 and Y) onto the surface of a metal substrate (FeCrAlloy) using in-situ hydrothermal synthesis. In addition, the zeolite Y is post-synthetically modified by acidified ammonium ion exchange to generate US-Y. Finally the catalytic activity of the structured ZSM-5 catalyst films (Si/Al = 11, thickness 146 0m) and structured US–Y catalyst film (Si/Al = 8, thickness 230m) were compared with the pelleted powder form of ZSM–5 and USY catalysts of similar Si/Al ratios. The structured catalyst films have been characterised using a range of techniques, including X-ray diffraction (XRD), Electron microscopy (SEM), Energy Dispersive X–ray analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-onalloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550oC). The cracking of n–heptane over the pellets and structured catalysts for both ZSM–5 and Y zeolite showed very similar product selectivities for similar amounts of catalyst with an apparent activation energy of around 60 kJ mol-1. This paper demonstrates that structured catalysts can be manufactured with excellent zeolite adherence and when suitably activated/modified give comparable cracking results to the pelleted powder forms. These structured catalysts will improve temperature distribution in highly exothermic and endothermic catalysed processes.

Keywords: FeCrAlloy, Structured catalyst, and Zeolite Y, Zeolite ZSM-5.

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