Mechanical and Thermal Properties Characterisation of Vinyl Ester Matrix Nanocomposites Based On Layered Silicate: Effect of Processing Parameters

The mechanical properties including flexural and tensile of neat vinyl ester and polymer based on layered silicate nanocomposite materials of two different methodologies are discussed. Methodology 1 revealed that the addition of layered silicate into the polymer matrix increased the mechanical and thermal properties up to 1 wt.% clay loading. The incorporation of more clay resulted in decreasing the properties which was traced to the existence of aggregation layers. The aggregation layers imparted a negative impact on the overall mechanical and thermal properties. On the other hand, methodology 2 increased the mechanical and thermal properties up to 4 wt.% clay loading. The different amounts of improvements were assigned to the various preparation parameters. Wide Angle X-ray Diffraction, Scanning Electron Microscopy and Transmission Electron Microscopy were utilized in order to characterize the interlamellar structure of nanocomposites.

Anomalous Thermal Behavior of CuxMg1-xNb2O6 (x=0,0.4,0.6,1) for LTCC Substrate

LTCC (Low Temperature Co-fired Ceramics) being the most advantageous technology towards the multilayer substrates for various applications, demands an extensive study of its raw materials. In the present work, a series of CuxMg1-xNb2O6 (x=0,0.4,0.6,1) has been prepared using sol-gel synthesis route and sintered at a temperature of 900°C to study its applicability for LTCC technology as the firing temperature is 900°C in this technology. The phase formation has been confirmed using X-ray Diffraction. Thermal properties like thermal conductivity and thermal expansion being very important aspect as the former defines the heat flow to avoid thermal instability in layers and the later provides the dimensional congruency of the dielectric material and the conductors, are studied here over high temperature up to the firing temperature. Although the values are quite satisfactory from substrate requirement point view, results have shown anomaly over temperature. The anomalous thermal behavior has been further analyzed using TG-DTA.

Effect of Processing Methods on Texture Evolution in AZ31 Mg Alloy Sheet

Textures of AZ31 Mg alloy sheets were evaluated by using neutron diffraction method in this study. The AZ31 sheets were fabricated either by conventional casting and subsequent hot rolling or strip casting. The effect of warm rolling was investigated using the AZ31 Mg alloy sheet produced by conventional casting. Warm rolling of 30% thickness reduction per pass was possible without any side-crack at temperatures as low as 200oC under the roll speed of 30 m/min. The initial microstructure of conventionally cast specimen was found to be partially recrystallized structures. Grain refinement was found to occur actively during the warm rolling. The (0002),(10-10) (10-11),and (10-12) complete pole figures were measured using the HANARO FCD (Neutron Four Circle Diffractometer) and ODF were calculated. The major texture of all specimens can be expressed by ND//(0001) fiber texture. Texture of hot rolled specimen showed the strongest fiber component, while that of strip cast sheet seemed to be similar to random distribution.

Green-Reduction of Covalently Functionalized Graphene Oxide with Varying Stoichiometry

Graphene-based materials were prepared by chemical reduction of covalently functionalized graphene oxide with environmentally friendly agents. Two varying stoichiometry of graphene oxide (GO) induced by using different chemical preparation conditions, further covalent functionalization of the GO materials with 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride / N-hydroxysuccinimide and ascorbic acid and sodium bisulfite as reducing agents were exploited in order to obtain controllable properties of the final solution-based graphene materials. The obtained materials were characterized by thermo-gravimetric analysis, Fourier transform infrared and Raman spectroscopy and X-ray diffraction. The results showed successful functionalization of the GO materials, while a comparison of the deoxygenation efficiency of the two-type functionalized graphene oxide suspensions by the different reducing agents has been made, revealing the strong dependence of their properties on the GO structure and reducing agents.

Combined Hydrothermal Synthesis of Zinc and Magnesium Borates at 100oC Using ZnO, MgO and H3BO3

Magnesium borate(MB) istechnical ceramic for high heat-resisting, corrosion-resisting, super mechanical strength, superinsulation, light weight, high strength, and high coefficient of elasticity. Zinc borate (ZB) can be used as multi-functional synergistic additives with flame retardant additives in polymers. The most important properties are low solubility in water and high dehydration temperature. ZB dehydrates above 290°C and anhydrous ZB has thermal resistance about 400°C. In this study, the raw materials of ZnO, MgO and H3BO3 were used with mole ratio of 1:1:9. With the starting materials hydrothermal method was applied at a temperature of 100oC. The reaction time was determined as 30, 60, 90 and 120 minutes after some preliminary experiments. After the synthesis, the crystal structure and the morphology of the products were examined by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). As a result, the forms of Zinc Oxide Borate Hydrate [Zn3B6O12.3.5H2O], Admontite [MgO(B2O3)3.7(H2O)] and Mcallisterite [Mg2(B6O7(OH)6)2.9(H2O)] were synthesized.

Phase Transition Characteristics of Flame-Synthesized Gamma-Al2O3 Nanoparticles with Heat Treatment

In this study, the phase transition characteristics of flame-synthesized γ-Al2O3 nanoparticles to α-Al2O3 have been investigated. The nanoparticles were synthesized by using a coflow hydrogen diffusion flame. The phase transition and particle characteristics of the Al2O3 nanoparticles were determined by examining the crystalline structure and the shape of the collected nanoparticles before and after the heat treatment. The morphology and crystal structure of the Al2O3 nanoparticles were determined from SEM images and XRD analyses, respectively. The measured specific surface area and averaged particle size were 63.44m2/g and 23.94nm, respectively. Based on the scanning electron microscope images and x-ray diffraction patterns, it is believed that the onset temperature of the phase transition to α-Al2O3 was existed near 1200oC. The averaged diameters of the sintered particles heat treated at 1,260oC were approximately 80nm.

EBSD Investigation of Friction Stir Welded Duplex Stainless Steel

Electron back-scattered diffraction was used to follow the evolution of microstructure from the base metal to the stir zone (SZ) in a duplex stainless steel subjected to friction stir welding. In the stir zone (SZ), a continuous dynamic recrystallization (CDRX) was evidenced for ferrite, while it was suggested that a static recrystallization together with CDRX may occur for austenite. It was found that ferrite and austenite grains in the SZ take a typical shear texture of bcc and fcc materials respectively.

Effect of Surface Pretreatments on Nanocrystalline Diamond Deposited On Silicon Nitride Substrates

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.

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.

Synthesis and Characterization of Gallosilicate Sodalite Containing NO2- Ions

Pure phase gallosilicate nitrite sodalite has been synthesized in a single step by low temperature (373 oK) hydrothermal technique. The product obtained was characterized using a combination of techniques including X-ray powder diffraction, IR, Raman spectroscopy, SEM, MAS NMR spectroscopy as well as thermogravimetry. Sodalite with an ideal composition was obtained after synthesis at 3730K and seven days duration using alkaline medium. The structural features of the Na8[GaSiO4]6(NO2)2 sodalite were investigated by IR, MAS NMR spectroscopy of 29Si and 23Na nuclei and by Reitveld refinement of X-ray powder diffraction data. The crystal structure of this sodalite has been refined in the space group P 4 3n; with a cell parameter 8.98386Å, V= 726.9 Å, (Rwp= 0.077 and Rp=0.0537) and Si-O-Ga angle is found to be 132.920 . MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. The surface area of single entity with stoichiometry Na8[GaSiO4]6(NO2)2 was found to be 8.083 x10-15 cm2/g.

The Effect of Waste Magnesium to Boric Acid Ratio in Hydrothermal Magnesium Borate Synthesis at 70oC

Magnesium wastes are produced by many industrial activities. This waste problem is becoming a future problem for the world. Magnesium borates have many advantages such as; high corrosion resistance, heat resistance, high coefficient of elasticity and can also be used in the production of material against radiation. Addition, magnesium borates have great potential in sectors including ceramic and detergents industry and superconducting materials. In this study, using the starting materials of waste magnesium and H3BO3 the hydrothermal method was applied at a moderate temperature of 70oC. Several mole ratios of waste magnesium to H3BO3 are selected as; 1:2, 1:4, 1:6, 1:8, 1:10. Reaction time was determined as 1 hour. After the synthesis, X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques are applied to products. As a result the forms of mcallisterite “Mg2(B6O7(OH)6)2.9(H2O)”, admontite “MgO(B2O3)3.7(H2O)” and magnesium boron hydrate (MgO(B2O3)3.6(H2O)” are obtained. 

Microwave Assisted Fast Synthesis of Flower-like ZnO Based Guanidinium Template for Photodegradation of Azo Dye Congo Red

ZnO nanostructure were synthesized via microwave method using zinc acetate as starting material, guanidinium as structure directing agents, and water as solvent.. This work investigates the photodegradation of azo dyes using the ZnO Flowerlike in aqueous solutions. As synthesized ZnO samples were characterized using X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), and FTIR spectroscopy.In this work photodecolorization of congored azo dye under UV irradiation by nano ZnO was studied.

Growing Zeolite Y on FeCrAlloy Metal

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.

Investigation of the Effect of Milling Time on the Mechanochemical Synthesis of Fe3Al/ Al2O3 Nanocomposite

In this study, the effect of mechanical activation on the synthesis of Fe3Al/Al2O3 nanocomposite has been investigated by using mechanochemical method. For this purpose, Aluminum powder and hematite as precursors, with stoichiometric ratio, have been utilized and other effective parameters in milling process were kept constant. Phase formation analysis, crystallite size measurement and lattice strain were studied by X-ray diffraction (XRD) by using Williamson-Hall method as well as microstructure and morphology were explored by Scanning electron microscopy (SEM). Also, Energy-dispersive X-ray spectroscopy (EDX) analysis was used in order to probe the particle distribution. The results showed that after 30-hour milling, the reaction was started, combustibly done and completed.

Effect of Silver Nanoparticles Size Prepared by Photoreduction Method on Optical Absorption Spectra of TiO2/Ag/N719 Dye Composite Films

TiO2/Ag composite films were prepared by incorporating Ag in the pores of mesoporous TiO2 films using a photoreduction method. The Ag nanoparticle sizes were in a range of 3.66-38.56 nm. The TiO2/Ag composite films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscropy (TEM). The TiO2 films and TiO2/Ag composite films were immersed in a 0.3 mM N719 dye solution and characterized by UV-Vis spectrophotometer. The TiO2/Ag/N719 composite film showed that an optimal size of Ag nanoparticles was 19.12 nm and, hence, gave the maximum optical absorption spectra. The improved absorption was due to surface plasmon resonance induced by the Ag nanoparticles to enhance the absorption coefficient of the dye.

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.

Static Recrystallization Behavior of Mg Alloy Single Crystals

Single crystals of Magnesium alloys such as pure Mg, Mg-1Zn-0.5Y, Mg-0.1Y, and Mg-0.1Ce alloys were successfully fabricated in this study by employing the modified Bridgman method. To determine the exact orientation of crystals, pole figure measurement using X-ray diffraction were carried out on each single crystal. Hardness and compression tests were conducted followed by subsequent recrysatllization annealing. Recrystallization kinetics of Mg alloy single crystals has been investigated. Fabricated single crystals were cut into rectangular shaped specimen and solution treated at 400oC for 24 hrs, and then deformed in compression mode by 30% reduction. Annealing treatment for recrystallization has been conducted on these cold-rolled plates at temperatures of 300oC for various times from 1 to 20 mins. The microstructure observation and hardness measurement conducted on the recrystallized specimens revealed that static recrystallization of ternary alloy single crystal was very slow, while recrystallization behavior of binary alloy single crystals appeared to be very fast.

Synthesis of ZnO Nanostructures via Gel-casting Method

In this study, ZnO nano rods and ZnO ultrafine particles were synthesized by Gel-casting method. The synthesized ZnO powder has a hexagonal zincite structure. The ZnO aggregates with rod-like morphology are typically 1.4 μm in length and 120 nm in diameter, which consist of many small nanocrystals with diameters of 10 nm. Longer wires connected by many hexahedral ZnO nanocrystals were obtained after calcinations at the temperature over 600° C.The crystalline structures and morphologies of the powder have been characterized by X-ray diffraction(XRD) and Scaning electron microscopy (SEM).The result shows that the different preparation conditions such as concentration H2O, calcinations time and calcinations temperature have a lot of influences upon the properties of nano ZnO powders, an increase in the temperature of the calcinations results in an increase of the grain size and also the increase of the calcinations time in high temperature makes the size of the grains bigger. The existences of extra watter prevent nano grains from improving like rod morphology. We have obtained the smallest grain size of ZnO powder by controlling the process conditions. Finally In a suitable condition, a novel nanostructure, namely bi-rod-like ZnO nano rods was found which is different from known ZnO nanostructures.