Determination of the Zinc Oxide and Boric Acid Optimum Molar Ratio on the Ultrasonic Synthesis of Zinc Borates

Zinc borates are used as a multi-functional flame retardant additive for its high dehydration temperature. In this study, the method of ultrasonic mixing was used in the synthesis of zinc borates. The reactants of zinc oxide (ZnO) and boric acid (H3BO3) were used at the constant reaction parameters of 90°C reaction temperature and 55 min of reaction time. Several molar ratios of ZnO:H3BO3 (1:1, 1:2, 1:3, 1:4 and 1:5) were conducted for the determination of the optimum reaction ratio. Prior to synthesis the characterization of the synthesized zinc borates were made by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). From the results Zinc Oxide Borate Hydrate [Zn3B6O12.3.5H2O], were synthesized optimum at the molar ratio of 1:3, with a reaction efficiency of 95.2%.

Ni-B Coating Production on Magnesium Alloy by Electroless Deposition

The use of magnesium alloys is limited due to their susceptibility to corrosion although they have many attractive physical and mechanical properties. To increase mechanical and corrosion properties of these alloys, many deposition method and coating types are used. Electroless Ni–B coatings have received considerable interest recently due to its unique properties such as cost-effectiveness, thickness uniformity, good wear resistance, lubricity, good ductility and corrosion resistance, excellent solderability and electrical properties and antibacterial property. In this study, electroless Ni-B coating could been deposited on AZ91 magnesium alloy. The obtained coating exhibited a harder and rougher structure than the substrate.

Inventive Synthesis and Characterization of a Cesium Molybdate Compound: CsBi(MoO4)2

Cesium molybdates with general formula CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich polymorphism, and crystallize in a layered structure. These properties cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differantial thermal analysis (TG/DTA).

Photocatalytic Degradation of Organic Pollutant Reacting with Tungstates: Role of Microstructure and Size Effect on Oxidation Kinetics

The aim of this study was to investigate the photocatalytic activity of polycrystalline phases of bismuth tungstate of formula Bi2WO6. Polycrystalline samples were elaborated using a coprecipitation technique followed by a calcination process at different temperatures (300, 400, 600 and 900°C). The obtained polycrystalline phases have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Crystal cell parameters and cell volume depend on elaboration temperature. High-resolution electron microscopy images and image simulations, associated with X-ray diffraction data, allowed confirming the lattices and space groups Pca21. The photocatalytic activity of the as-prepared samples was studied by irradiating aqueous solutions of Rhodamine B, associated with Bi2WO6 additives having variable crystallite sizes. The photocatalytic activity of such bismuth tungstates increased as the crystallite sizes decreased. The high specific area of the photocatalytic particles obtained at 300°C seems to condition the degradation kinetics of RhB.

Synthesizing CuFe2O4 Spinel Powders by a Combustion-Like Process for Solid Oxide Fuel Cell Interconnect Coatings

The synthesis of CuFe2O4 spinel powders by an optimized combustion-like process followed by calcination is described herein. The samples were characterized using X-ray diffraction (XRD), differential thermal analysis (TG/DTA), scanning electron microscopy (SEM), dilatometry and 4-probe DC methods. Different glycine to nitrate (G/N) ratios of 1 (fuel-deficient), 1.48 (stoichiometric) and 2 (fuel-rich) were employed. Calcining the asprepared powders at 800 and 1000°C for 5 hours showed that the G/N ratio of 2 results in the formation of the desired copper spinel single phase at both calcination temperatures. For G/N=1, formation of CuFe2O4 takes place in three steps. First, iron and copper nitrates decompose to iron oxide and pure copper. Then, copper transforms to copper oxide and finally, copper and iron oxides react with each other to form a copper ferrite spinel phase. The electrical conductivity and the coefficient of thermal expansion of the sintered pelletized samples were 2 S.cm-1 (800°C) and 11×10-6 °C-1 (25-800°C), respectively.

A Preliminary X-Ray Study on Human-Hair Microstructures for a Health-State Indicator

We present a preliminary x-ray study on human-hair microstructures for a health-state indicator, in particular a cancer case. As an uncomplicated and low-cost method of x-ray technique, the human-hair microstructure was analyzed by wide-angle x-ray diffractions (XRD) and small-angle x-ray scattering (SAXS). The XRD measurements exhibited the simply reflections at the d-spacing of 28 Å, 9.4 Å and 4.4 Å representing to the periodic distance of the protein matrix of the human-hair macrofibrous and the diameter and the repeated spacing of the polypeptide alpha helixes of the photofibrils of the human-hair microfibrous, respectively. When compared to the normal cases, the unhealthy cases including to the breast- and ovarian-cancer cases obtained higher normalized ratios of the x-ray diffracting peaks of 9.4 Å and 4.4 Å. This likely resulted from the varied distributions of microstructures by a molecular alteration. As an elemental analysis by x-ray fluorescence (XRF), the normalized quantitative ratios of zinc(Zn)/calcium(Ca) and iron(Fe)/calcium(Ca) were determined. Analogously, both Zn/Ca and Fe/Ca ratios of the unhealthy cases were obtained higher than both of the normal cases were. Combining the structural analysis by XRD measurements and the elemental analysis by XRF measurements exhibited that the modified fibrous microstructures of hair samples were in relation to their altered elemental compositions. Therefore, these microstructural and elemental analyses of hair samples will be benefit to associate with a diagnosis of cancer and genetic diseases. This functional method would lower a risk of such diseases by the early diagnosis. However, the high-intensity x-ray source, the highresolution x-ray detector, and more hair samples are necessarily desired to develop this x-ray technique and the efficiency would be enhanced by including the skin and fingernail samples with the human-hair analysis.

The Incorporation of In in GaAsN as a Means of N Fraction Calibration

InGaAsN and GaAsN epitaxial layers with similar nitrogen compositions in a sample were successfully grown on a GaAs (001) substrate by solid source molecular beam epitaxy. An electron cyclotron resonance nitrogen plasma source has been used to generate atomic nitrogen during the growth of the nitride layers. The indium composition changed from sample to sample to give compressive and tensile strained InGaAsN layers. Layer characteristics have been assessed by high-resolution x-ray diffraction to determine the relationship between the lattice constant of the GaAs1-yNy layer and the fraction x of In. The objective was to determine the In fraction x in an InxGa1-xAs1-yNy epitaxial layer which exactly cancels the strain present in a GaAs1-yNy epitaxial layer with the same nitrogen content when grown on a GaAs substrate.

Effect of Heat Treatment on the Portevin-Le Chatelier Effect of Al-2.5%Mg Alloy

An experimental study is presented on the effect of microstructural change on the Portevin-Le Chatelier effect behaviour of Al-2.5%Mg alloy. Tensile tests are performed on the as received and heat treated (at 400 ºC for 16 hours) samples for a wide range of strain rates. The serrations observed in the stress-time curve are investigated from statistical analysis point of view. Microstructures of the samples are characterized by optical metallography and X-ray diffraction. It is found that the excess vacancy generated due to heat treatment leads to decrease in the strain rate sensitivity and the increase in the number of stress drop occurrences per unit time during the PLC effect. The microstructural parameters like domain size, dislocation density have no appreciable effect on the PLC effect as far as the statistical behavior of the serrations is considered.

Characterization of Biodegradable Nanocomposites with Poly (Lactic Acid) and Multi-Walled Carbon Nanotubes

In this study, structural, mechanical, thermal and electrical properties of poly (lactic acid) (PLA) nanocomposites with low-loaded (0-1.5 wt%) untreated, heat and nitric acid treated multiwalled carbon nanotubes (MWCNTs) were studied. Among the composites, untreated 0.5 wt % MWCNTs and acid-treated 1.0 wt% MWCNTs reinforced PLA show the tensile strength and modulus values higher than the others. These two samples along with pure PLA exhibit the stable orthorhombic α-form, whilst other samples reveal the less stable orthorhombic β-form, as demonstrated by X-ray diffraction study. Differential scanning calorimetry reveals the evolution of the mentioned different phases by controlled cooling and discloses an enhancement of PLA crystallization by nanotubes incorporation. Thermogravimetric analysis shows that the MWCNTs loaded sample degraded faster than PLA. Surface resistivity of the nanocomposites is found to be dropped drastically by a factor of 1013 with a low loading of MWCNTs (1.5 wt%).

Experimental Study of Adsorption Properties of Acid and Thermal Treated Bentonite from Tehran (Iran)

The Iranian bentonite was first characterized by Scanning Electron Microscopy (SEM), Inductively Coupled Plasma mass spectrometry (ICP-MS), X-ray fluorescence (XRF), X-ray Diffraction (XRD) and BET. The bentonite was then treated thermally between 150°C-250°C at 15min, 45min and 90min and also was activated chemically with different concentration of sulphuric acid (3N, 5N and 10N). Although the results of thermal activated-bentonite didn-t show any considerable changes in specific surface area and Cation Exchange Capacity (CEC), but the results of chemical treated bentonite demonstrated that such properties have been improved by acid activation process.

Effect of Bentonite on the Properties of Liquid Insulating Oil

Bentonitic material from South Aswan, Egypt was evaluated in terms of mineral-ogy and chemical composition as bleaching clay in refining of transformer oil before and after acid activation and thermal treatment followed by acid leaching using HCl and H2SO4 for different contact times. Structural modification and refining power of bento-nite were investigated during modification by means of X-ray diffraction and infrared spectroscopy. The results revealed that the activated bentonite could be used for refining of transformer oil. The oil parameters such as; dielectric strength, viscosity and flash point had been improved. The dielectric breakdown strength of used oil increased from 29 kV for used oil treated with unactivated bentonite to 74 kV after treatment with activated bentonite. Kinematic Viscosity changed from 19 to 11 mm2 /s after treatment with activated bentonite. However, flash point achieved 149 ºC.

Global and Local Structure of Supported Pd Catalysts

The supported Pd catalysts were analyzed by X-ray diffraction and X-ray absorption spectroscopy in order to determine their global and local structure. The average particle size of the supported Pd catalysts was determined by X-ray diffraction method. One of the main purposes of the present contribution is to focus on understanding the specific role of the Pd particle size determined by X-ray diffraction and that of the support oxide. Based on X-ray absorption fine structure spectroscopy analysis we consider that the whole local structure of the investigated samples are distorted concerning the atomic number but the distances between atoms are almost the same as for standard Pd sample. Due to the strong modifications of the Pd cluster local structure, the metal-support interface may influence the electronic properties of metal clusters and thus their reactivity for absorption of the reactant molecules.

Structural and Optical Properties ofInxAlyGa1-x-yN Quaternary Alloys

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.

Computer Aided X-Ray Diffraction Intensity Analysis for Spinels: Hands-On Computing Experience

The mineral having chemical compositional formula MgAl2O4 is called “spinel". The ferrites crystallize in spinel structure are known as spinel-ferrites or ferro-spinels. The spinel structure has a fcc cage of oxygen ions and the metallic cations are distributed among tetrahedral (A) and octahedral (B) interstitial voids (sites). The X-ray diffraction (XRD) intensity of each Bragg plane is sensitive to the distribution of cations in the interstitial voids of the spinel lattice. This leads to the method of determination of distribution of cations in the spinel oxides through XRD intensity analysis. The computer program for XRD intensity analysis has been developed in C language and also tested for the real experimental situation by synthesizing the spinel ferrite materials Mg0.6Zn0.4AlxFe2- xO4 and characterized them by X-ray diffractometry. The compositions of Mg0.6Zn0.4AlxFe2-xO4(x = 0.0 to 0.6) ferrites have been prepared by ceramic method and powder X-ray diffraction patterns were recorded. Thus, the authenticity of the program is checked by comparing the theoretically calculated data using computer simulation with the experimental ones. Further, the deduced cation distributions were used to fit the magnetization data using Localized canting of spins approach to explain the “recovery" of collinear spin structure due to Al3+ - substitution in Mg-Zn ferrites which is the case if A-site magnetic dilution and non-collinear spin structure. Since the distribution of cations in the spinel ferrites plays a very important role with regard to their electrical and magnetic properties, it is essential to determine the cation distribution in spinel lattice.

Non-Isothermal Kinetics of Crystallization and Phase Transformation of SiO2-Al2O3-P2O5-CaO-CaF Glass

The crystallization kinetics and phase transformation of SiO2.Al2O3.0,56P2O5.1,8CaO.0,56CaF2 glass have been investigated using differential thermal analysis (DTA), x-ray diffraction (XRD), and scanning electron microscopy (SEM). Glass samples were obtained by melting the glass mixture at 14500С/120 min. in platinum crucibles. The mixture were prepared from chemically pure reagents: SiO2, Al(OH)3, H3PO4, CaCO3 and CaF2. The non-isothermal kinetics of crystallization was studied by applying the DTA measurements carried out at various heating rates. The activation energies of crystallization and viscous flow were measured as 348,4 kJ.mol–1 and 479,7 kJ.mol–1 respectively. Value of Avrami parameter n ≈ 3 correspond to a three dimensional of crystal growth mechanism. The major crystalline phase determined by XRD analysis was fluorapatite (Ca(PO4)3F) and as the minor phases – fluormargarite (CaAl2(Al2SiO2)10F2) and vitlokite (Ca9P6O24). The resulting glass-ceramic has a homogeneous microstructure, composed of prismatic crystals, evenly distributed in glass phase.

Microstructure Changes of Machined Surfaceson Austenitic 304 Stainless Steel

This paper presents a experiment to estimate the influences of cutting conditions in microstructure changes of machining austenitic 304 stainless steel, especially for wear insert. The wear insert were prefabricated with a width of 0.5 mm. And the forces, temperature distribution, RS, and microstructure changes were measured by force dynamometer, infrared thermal camera, X-ray diffraction, XRD, SEM, respectively. The results told that the different combinations of machining condition have a significant influence on machined surface microstructure changes. In addition to that, the ANOVA and AOMwere used to tell the different influences of cutting speed, feed rate, and wear insert.