Search results for: Energy Dispersive X-Ray Spectroscopy

Authors: Hanan Alenezi

Abstract:

Membrane performance depends on the kind of solvent used in preparation. A membrane made by Polyetherimide (PEI) was evaluated for gas separation using X-Ray Diffraction (XRD), Scanning electron microscope (SEM), and Energy Dispersive X-Ray Spectroscopy (EDS). The purity and the thickness are detected to evaluate the membrane in order to optimize PEI membrane preparation.

Keywords: Energy Dispersive X-Ray Spectroscopy, EDS, membrane, Polyetherimide, PEI, Scanning electron microscope, SEM, Solvent, X-Ray Diffraction, XRD.

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Authors: Abdelkader Benzian

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Spectroscopy is the study of the spectrum produced by the radiation-matter interaction which requires the study of electromagnetic radiation (or electrons) emitted, absorbed, or scattered by matter. Thus, the spectral analysis is using spectrometers which enables us to obtain curves that express the distribution of the energy emitted (spectrum). Analysis of emission spectra can therefore constitute several methods depending on the range of radiation energy. The most common methods used are Auger electron spectroscopy (AES) and Electron Energy Losses Spectroscopy (EELS), which allow the determination of the atomic structure on the surface. This paper focalized essentially on the Electron Energy Loss Spectroscopy.

Keywords: Dielectric, plasmon, mean free path, spectroscopy of electron energy losses.

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Authors: Maribel G. Guzmán, Jean Dille, Stephan Godet

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Silver nanoparticles were prepared by chemical reduction method. Silver nitrate was taken as the metal precursor and hydrazine hydrate as a reducing agent. The formation of the silver nanoparticles was monitored using UV-Vis absorption spectroscopy. The UV-Vis spectroscopy revealed the formation of silver nanopart├¡cles by exhibing the typical surface plasmon absorption maxima at 418-420 nm from the UV–Vis spectrum. Comparison of theoretical (Mie light scattering theory) and experimental results showed that diameter of silver nanoparticles in colloidal solution is about 60 nm. We have used energy-dispersive spectroscopy (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and, UV–Vis spectroscopy to characterize the nanoparticles obtained. The energy-dispersive spectroscopy (EDX) of the nanoparticles dispersion confirmed the presence of elemental silver signal no peaks of other impurity were detected. The average size and morphology of silver nanoparticles were determined by transmission electron microscopy (TEM). TEM photographs indicate that the nanopowders consist of well dispersed agglomerates of grains with a narrow size distribution (40 and 60 nm), whereas the radius of the individual particles are between 10 and 20 nm. The synthesized nanoparticles have been structurally characterized by X-ray diffraction and transmission high-energy electron diffraction (HEED). The peaks in the XRD pattern are in good agreement with the standard values of the face-centered-cubic form of metallic silver (ICCD-JCPDS card no. 4-0787) and no peaks of other impurity crystalline phases were detected. Additionally, the antibacterial activity of the nanopart├¡culas dispersion was measured by Kirby-Bauer method. The nanoparticles of silver showed high antimicrobial and bactericidal activity against gram positive bacteria such as Escherichia Coli, Pseudimonas aureginosa and staphylococcus aureus which is a highly methicillin resistant strain.

Keywords: Silver nanoparticles, surface plasmon, UV-Vis absorption spectrum, chemicals reduction.

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Authors: Faten. A. Khorshid, Gehan. A. Raouf, Salem. M. El-Hamidy, Gehan. S. Al-amri, Nourah. A. Alotaibi, Taha A. Kumosani

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Cancer becomes one of the leading cause of death in many countries over the world. Fourier-transform infrared (FTIR) spectra of human lung cancer cells (A549) treated with PMF (natural product extracted from PM 701) for different time intervals were examined. Second derivative and difference method were taken in comparison studies. Cesium (Cs) and Rubidium (Rb) nanoparticles in PMF were detected by Energy Dispersive X-ray attached to Scanning Electron Microscope SEM-EDX. Characteristic changes in protein secondary structure, lipid profile and changes in the intensities of DNA bands were identified in treated A549 cells spectra. A characteristic internucleosomal ladder of DNA fragmentation was also observed after 30 min of treatment. Moreover, the pH values were significantly increases upon treatment due to the presence of Cs and Rb nanoparticles in the PMF fraction. These results support the previous findings that PMF is selective anticancer agent and can produce apoptosis to A549 cells.

Keywords: Apoptosis, FTIR spectroscopy, pH therapy, Scanning Electron Microscope- Energy Dispersive X-ray (SEMEDX).

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Authors: Nazli Darkhal

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The use of gems and ornaments has been common in Iran since the beginning of history. The prosperity of the country, the wealth, and the interest of the people of this land in a luxurious and glorious life, combined with beauty, have always attracted the attention of Iranian people to gems and jewelry. Iranians are famous in the world for having a long history of collecting and recognizing precious stones. In this case, we can use the unique treasure of national jewelry. Raman spectroscopy method is one of the oscillating spectroscopy methods that is classified in the group of nondestructive study methods, and like other methods, in addition to several advantages, it also has disadvantages and problems. Micro Raman spectroscopy is one of the different types of Raman spectroscopy in which an optical microscope is combined with a Raman device to provide more capabilities and advantages than its original method. In this way, with the help of Raman spectroscopy and a light microscope, while observing more details from different parts of the historical sample, natural or artificial pigments can be identified in a small part of it. The EDX (Energy Dispersive X ray) electron microscope also functions as the basis for the interaction of the electron beam with the matter. The beams emitted from this interaction can be used to examine samples. In this article, in addition to introducing the micro-Raman spectroscopy method, studies have been conducted on the structure of three samples of existing stones in the historic citadel of Bam. Using this method of study on precious and semi-precious stones, in addition to requiring a short time, can provide us with complete information about the structure and theme of these samples. The results of experiments and gemology of the stones showed that the selected beads are agate and jasper, and they can be placed in the chalcedony group.

Keywords: Bam citadel, precious stones, semi-precious stones, Raman spectroscopy, scanning electron microscope.

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Authors: Mohammadhosein Rahimi, Mohammad Raouf Hosseini, Mehran Bakhshi, Alireza Baghbanan

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Silver ions (Ag⁺) and their compounds are consequentially toxic to microorganisms, showing biocidal effects on many species of bacteria. Silver-phosphate (or silver orthophosphate) is one of these compounds, which is famous for its antimicrobial effect and catalysis application. In the present study, a green method was presented to synthesis silver-phosphate nanoparticles using Sporosarcina pasteurii. The composition of the biosynthesized nanoparticles was identified as Ag₃PO₄ using X-ray Diffraction (XRD) and Energy Dispersive Spectroscopy (EDS). Also, Fourier Transform Infrared (FTIR) spectroscopy showed that Ag₃PO₄ nanoparticles was synthesized in the presence of biosurfactants, enzymes, and proteins. In addition, UV-Vis adsorption of the produced colloidal suspension approved the results of XRD and FTIR analyses. Finally, Transmission Electron Microscope (TEM) images indicated that the size of the nanoparticles was about 20 nm.

Keywords: Bacteria, biosynthesis, silver-phosphate, Sporosarcina pasteurii, nanoparticle.

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Authors: Y. Li, K. Buddharaju, X. P. Wang

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The mechanism of nickel (Ni) metallization in silicon-germanium (Si_0.5Ge_0.5) alloy nanowire (NW) was studied. Transmission electron microscope imaging with in-situ annealing was conducted at temperatures of 200^oC to 600°C. During rapid formation of Ni germanosilicide, loss of material from from the SiGe NW occurred which led to the formation of a thin Ni germanosilicide filament and eventual void. Energy dispersive X-ray spectroscopy analysis along the SiGe NW before and after annealing determined that Ge atoms tend to out-diffuse from the Ni germanosilicide towards the Ni source in the course of annealing. A model for the Ni germanosilicide formation in SiGe NW is proposed to explain this observation.

Keywords: SiGe, nanowires, germanosilicide.

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Authors: Kamyar Shameli, Mansor Bin Ahmad, Wan Md Zin Wan Yunus, Nor Azowa Ibrahim, Maryam Jokar, Majid Darroudi

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Silver/polylactide nanocomposites (Ag/PLA-NCs) were synthesized via chemical reduction method in diphase solvent. Silver nitrate and sodium borohydride were used as a silver precursor and reducing agent in the polylactide (PLA). The properties of Ag/PLA-NCs were studied as a function of the weight percentages of silver nanoparticles (8, 16 and 32 wt% of Ag-NPs) relative to the weight of PLA. The Ag/PLA-NCs were characterized by Xray diffraction (XRD), transmission electron microscopy (TEM), electro-optical microscopy (EOM), UV-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FT-IR). XRD patterns confirmed that Ag-NPs crystallographic planes were face centered cubic (fcc) type. TEM images showed that mean diameters of Ag-NPs were 3.30, 3.80 and 4.80 nm. Electro-optical microscopy revealed excellent dispersion and interaction between Ag-NPs and PLA films. The generation of silver nanoparticles was confirmed from the UVvisible spectra. FT-IR spectra showed that there were no significant differences between PLA and Ag/PLA-NCs films. The synthesized Ag/PLA-NCs were stable in organic solution over a long period of time without sign of precipitation.

Keywords: Nanocomposites, Polylactide, Silver Nanoparticles, Sodium Borohydride, Transmission Electron Microscopy.

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: Energy dispersive X-ray spectroscopy, high strength concrete, interfacial transition zone, mixing procedure, normal strength concrete, scanning electron microscopy.

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

Abstract:

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: F. Kurtuluş, G. Çelik Gül

Abstract:

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).

Keywords: Cesium bismuth dimolybdate, microwave synthesis, powder x-ray diffraction, rare earth dimolybdates.

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Authors: Haleh Rezaei Zanjirabadi, Fatemeh Saberi, Bahman Rahimzadeh, Fariborz Masoudi, Mohammad Rahgosha

Abstract:

In this study, apatite minerals from the iron-phosphate deposit of Yazd have been investigated within the microcontinent zone of Iran in the Zagros structural zone. The geological units in the Esfordi area belong to the pre-Cambrian to lower-Cambrian age, consisting of a succession of carbonate rocks (dolomite), shale, tuff, sandstone, and volcanic rocks. In addition to the mentioned sedimentary and volcanic rocks, the granitoid mass of Bahabad, which is the largest intrusive mass in the region, has intruded into the eastern part of this series and has caused its metamorphism and alteration. After collecting the available data, various samples of Esfordi’s apatite were prepared, and their mineralogy and crystallography were investigated using laboratory methods such as petrographic microscopy, Raman spectroscopy, EDS (Energy Dispersive Spectroscopy), and Scanning Electron Microscopy (SEM). In non-destructive Raman spectroscopy, the molecular structure of apatite minerals was revealed in four distinct spectral ranges. Initially, the spectra of phosphate and aluminum bonds with O2HO, OH, were observed, followed by the identification of Cl, OH, Al, Na, Ca and hydroxyl units depending on the type of apatite mineral family. In SEM analysis, based on various shapes and different phases of apatites, their constituent major elements were identified through EDS, indicating that the samples from the Esfordi mining area exhibit a dense and coherent texture with smooth surfaces. Based on the elemental analysis results by EDS, the apatites in the Esfordi area are classified into the calcic apatite group.

Keywords: Petrology, apatite, Esfordi, EDS, SEM, Scanning Electron Microscopy, Raman spectroscopy.

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Authors: T. Abdallah, K. Easawi, A. Khalid, S. Negm, H. Talaat

Abstract:

Nanocrystals (NC) alloyed composite CdSxSe1-x(x=0 to 1) have been prepared using the chemical solution deposition technique. The energy band gap of these alloyed nanocrystals of approximately the same size, have been determined by scanning tunneling spectroscopy (STS) technique at room temperature. The values of the energy band gap obtained directly using STS are compared to those measured by optical spectroscopy. Increasing the molar fraction ratio x from 0 to 1 causes clearly observed increase in the band gap of the alloyed composite nanocrystal. Vegard-s law was applied to calculate the parameters of the effective mass approximation (EMA) model and the dimension obtained were compared to the values measured by STM. The good agreement of the calculated and measured values is a direct result of applying Vegard's law in the nanocomposites.

Keywords: Alloy semiconductor nanocrystals, STM.

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Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

The first laboratory synthesis of hard materials such as diamond proceeded to attack of developing materials with high hardness to compete diamond. Boron rich solids are good candidates owing to their short interatomic bond lengths and strong covalent character. Boron containing hard material was synthesized by modifiedmicrowave method under nitrogen atmosphere by using a fuel (glycine or urea), amorphous boron and/or boric acid in 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/differential thermal analysis (TG/DTA).

Keywords: Boron containing materials, hard materials, microwave synthesis, powder X-ray diffraction.

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Authors: Noor Ul Ain Bhatti, M. Junaid Khan, Javed Ahmad, Murtaza Saleem, Shahid M. Ramay, Saadat A. Siddiqi

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Manganese oxide is being recently used as electrode material for rechargeable batteries. In this study, Al incorporated Mn₂O₃ compositions were synthesized to study the effect of Al doping on electrochemical performance of host material. Structural studies were carried out using X-ray diffraction analysis to confirm the phase stability and explore the lattice parameters, crystallite size, lattice strain, density and cell volume. Morphology and composition were analyzed using field emission scanning electron microscope and energy dispersive X-ray spectroscopy, respectively. Dynamic light scattering analysis was performed to observe the average particle size of the compositions. FTIR measurements exhibit the O-Al-O and O-Mn-O and Al-O bonding and with increasing the concentration of Al, the vibrational peaks of Mn-O become sharper. An enhanced electrochemical performance was observed in compositions with higher Al content.

Keywords: Mn2O3, electrode materials, energy storage and conversion, electrochemical performance.

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

Abstract:

The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO2 nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO2 nanoparticles was characterized from 30 nm to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were: water, SBF and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: B. Ghasemi, A. A. Najafzadeh Khoee

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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.

Keywords: hematite, mechanochemical, milling, nanocomposite

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Authors: K. B. Dermenci, B. Ebin, S.Gürmen

Abstract:

Noble metal participation in nanostructured semiconductor catalysts has drawn much interest because of their improved properties. Recently, it has been discussed by many researchers that Ag participation in TiO2, CuO, ZnO semiconductors showed improved photocatalytic and optical properties. In this research, Ag/ZnO nanocomposite particles were prepared by Ultrasonic Spray Pyrolysis(USP) Method. 0.1M silver and zinc nitrate aqueous solutions were used as precursor solutions. The Ag:Zn atomic ratio of the solution was selected 1:1. Experiments were taken place under constant air flow of 400 mL/min at 800°C furnace temperature. Particles were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM) and Energy Dispersive Spectroscopy (EDS). The crystallite sizes of Ag and ZnO in composite particles are 24.6 nm, 19.7 nm respectively. Although, spherical nanocomposite particles are in a range of 300- 800 nm, these particles are formed by the aggregation of primary particles which are in a range of 20-60 nm.

Keywords: Ag/ZnO nanocatalysts, Nanotechnology, USP

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Authors: A. Karsenty, A. Chelly

Abstract:

Ultrathin (UTD) and Nanoscale (NSD) SOI-MOSFET devices, sharing a similar W/L but with a channel thickness of 46nm and 1.6nm respectively, were fabricated using a selective “gate recessed” process on the same silicon wafer. The electrical transport characterization at room temperature has shown a large difference between the two kinds of devices and has been interpreted in terms of a huge unexpected series resistance. Electrical characteristics of the Nanoscale device, taken in the linear region, can be analytically derived from the ultrathin device ones. A comparison of the structure and composition of the layers, using advanced techniques such as Focused Ion Beam (FIB) and High Resolution TEM (HRTEM) coupled with Energy Dispersive X-ray Spectroscopy (EDS), contributes an explanation as to the difference of transport between the devices.

Keywords: Nanoscale Devices, SOI MOSFET, Analytical Model, Electron Transport.

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Authors: Merve Küçük, M. Lütfi Öveçoğlu

Abstract:

Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.

Keywords: Dip coating, polyester fabrics, sol-gel, zinc oxide.

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Authors: Richard E. Miller

Abstract:

12.7-mm thick plates of 6061-T6511 aluminum alloy and high hardness steel (528 HV) were successfully joined by a friction stir bonding process using a tungsten-rhenium stir tool. Process parameter variation experiments, which included tool design geometry, plunge and traverse rates, tool offset, spindle tilt, and rotation speed, were conducted to develop a parameter set which yielded a defect free joint. Laboratory tensile tests exhibited yield stresses which exceed the strengths of comparable AA6061-to-AA6061 fusion and friction stir weld joints. Scanning electron microscopy and energy dispersive X-ray spectroscopy analysis also show atomic diffusion at the material interface region.

Keywords: Dissimilar materials, friction stir, welding.

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Authors: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

Abstract:

Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: Ceramics, microstructure, electrochemical measurements, energy storage, transmission electron microscope.

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Authors: N. Tugrul, N. Baran Acarali, A. S. Kipcak, E. Moroydor Derun, S. Piskin

Abstract:

Turkey has 72 % of total world boron reserves on the basis of B2O3.Borates that is a refined form of boron minerals have a wide range of applications. Zinc borates can be used as multifunctional synergistic additives. The most important properties are low solubility in water and high dehydration temperature. Zinc borates dehydrate above 290°C and anhydrous zinc borate has thermal resistance about 400°C. Zinc borates can be synthesized using several methods such as hydrothermal and solid-state processes. In this study, the solid-state method was applied between 500 and 800°C using the starting materials of ZnO and H3BO3 with 1:4 mole ratio. The reaction time was determined as 4 hours after some preliminary experiments. After the synthesis, the crystal structure and the morphology of the products were examined by XRay Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman Spectrometer. As a result the form of ZnB4O7 was synthesized with the highest crystal score at 800°C.

Keywords: Raman, solid-state method, zinc borate, XRD.

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Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA). 

Keywords: Colemanite, conventional synthesis, powder x-ray diffraction, borates.

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Authors: Jayesh P. Ruparelia, Bhavna D. Soni

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Electrochemical-oxidation of Reactive Black-5 (RB- 5) was conducted for degradation using DSA type Ti/RuO2-SnO2- Sb2O5 electrode. In the study, for electro-oxidation, electrode was indigenously fabricated in laboratory using titanium as substrate. This substrate was coated using different metal oxides RuO2, Sb2O5 and SnO2 by thermal decomposition method. Laboratory scale batch reactor was used for degradation and decolorization studies at pH 2, 7 and 11. Current density (50mA/cm2) and distance between electrodes (8mm) were kept constant for all experiments. Under identical conditions, removal of color, COD and TOC at initial pH 2 was 99.40%, 55% and 37% respectively for initial concentration of 100 mg/L RB-5. Surface morphology and composition of the fabricated electrode coatings were characterized using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) respectively. Coating microstructure was analyzed by X-ray diffraction (XRD). Results of this study further revealed that almost 90% of oxidation occurred within 5-10 minutes.

Keywords: Electrochemical-oxidation, RB- dye, Decolorization.

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Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd₂Zr₃(MoO₄)₉ which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd2Zr3(MoO4)9, solid state synthesis, powder x-ray diffraction, zirconium molybdates.

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Authors: Mohanapriya Subramanian, V. Raj

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Direct methanol fuel cells (DMFCs) are considered to be one of the most promising candidates for portable and stationary applications in the view of their advantages such as high energy density, easy manipulation, high efficiency and they operate with liquid fuel which could be used without requiring any fuel-processing units. Electrolyte membrane of DMFC plays a key role as a proton conductor as well as a separator between electrodes. Increasing concern over environmental protection, biopolymers gain tremendous interest owing to their eco-friendly bio-degradable nature. Pectin is a natural anionic polysaccharide which plays an essential part in regulating mechanical behavior of plant cell wall and it is extracted from outer cells of most of the plants. The aim of this study is to develop and demonstrate pectin based polymer composite membranes as methanol impermeable polymer electrolyte membranes for DMFCs. Pectin based nanocomposites membranes are prepared by solution-casting technique wherein pectin is blended with chitosan followed by the addition of optimal amount of sulphonic acid modified Titanium dioxide nanoparticle (S-TiO2). Nanocomposite membranes are characterized by Fourier Transform-Infra Red spectroscopy, Scanning electron microscopy, and Energy dispersive spectroscopy analyses. Proton conductivity and methanol permeability are determined into order to evaluate their suitability for DMFC application. Pectin-chitosan blends endow with a flexible polymeric network which is appropriate to disperse rigid S-TiO2 nanoparticles. Resulting nanocomposite membranes possess adequate thermo-mechanical stabilities as well as high charge-density per unit volume. Pectin-chitosan natural polymeric nanocomposite comprising optimal S-TiO2 exhibits good electrochemical selectivity and therefore desirable for DMFC application.

Keywords: Biopolymers, fuel cells, nanocomposite, methanol crossover.

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Authors: C.S. Jawalkar, Apurbba Kumar Sharma, Pradeep Kumar

Abstract:

Electro Chemical Discharge Machining (ECDM) is an emerging hybrid machining process used in precision machining of hard and brittle non-conducting materials. The present paper gives a critical review on materials machined by ECDM under the prevailing machining conditions; capability indicators of the process are reported. Some results obtained while performing experiments in micro-channeling on soda lime glass using ECDM are also presented. In these experiments, Tool Wear (TW) and Material Removal (MR) were studied using design of experiments and L–4 orthogonal array. Experimental results showed that the applied voltage was the most influencing parameter in both MR and TW studies. Field emission scanning electron microscopy (FESEM) results obtained on the microchannels confirmed the presence of micro-cracks, primarily responsible for MR. Chemical etching was also seen along the edges. The Energy dispersive spectroscopy (EDS) results were used to detect the elements present in the debris and specimens.

Keywords: ECDM, applied-voltage, FESEM, EDS.

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Authors: Balwinder Singh

Abstract:

The present research is a paper on the characterization of aluminum alloy-6063 hybrid metal matrix composites using three different reinforcement materials (SiC, red mud, and fly ash) through stir casting method. The red mud was used in solid form, and particle size range varies between 103-150 µm. During this investigation, fly ash is received from Guru Nanak Dev Thermal Plant (GNDTP), Bathinda. The study has been done by using Taguchi’s L9 orthogonal array by taking fraction wt.% (SiC 5%, 7.5%, and 10% and Red Mud and Fly Ash 2%, 4%, and 6%) as input parameters with their respective levels. The study of the mechanical properties (tensile strength, impact strength, and microhardness) has been done by using Analysis of Variance (ANOVA) with the help of MINITAB 17 software. It is revealed that silicon carbide is the most significant parameter followed by red mud and fly ash affecting the mechanical properties, respectively. The fractured surface morphology of the composites using Field Emission Scanning Electron Microscope (FESEM) shows that there is a good mixing of reinforcement particles in the matrix. Energy-dispersive X-ray spectroscopy (EDS) was performed to know the presence of the phases of the reinforced material.

Keywords: Reinforcement, silicon carbide, fly ash, red mud.

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Authors: Amoljit S. Gill, Sanjeev Kumar

Abstract:

In this study, Electrical Discharge Machining (EDM) is used to modify the surface of high carbon steel En31 with the help of tool electrode (Copper-Chromium-Nickel) manufactured by powder metallurgy (PM) process. The effect of EDM on surface roughness during surface alloying is studied. Taguchi’s Design of experiment (DOE) and L18 orthogonal array is used to find the best level of input parameters in order to achieve high surface finish. Six input parameters are considered and their percentage contribution towards surface roughness is investigated by analysis of variances (ANOVA). Experimental results show that an hard alloyed surface (1.21% carbon, 2.14% chromium and 1.38% nickel) with surface roughness of 3.19µm can be generated using EDM with PM tool. Additionally, techniques like Scanning Electron Microscope (SEM) and Energy Dispersive Spectroscopy (EDS) are used to analyze the machined surface and EDMed layer composition, respectively. The increase in machined surface micro-hardness (101%) may be related to the formation of carbides containing chromium.

Keywords: Electrical Discharge Machining, Surface Roughness, Powder metallurgy compact tools, Taguchi DOE technique.

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