Search results for: X-ray Diffraction.

Authors: Loai Nasrat, Mervat S. Hassan

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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.

Keywords: Dielectric strength, unactivated bentonite, X-ray diffraction, SEM image

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Authors: A. A. Akande, B. P. Dhonge, B. W. Mwakikunga, A. G. J. Machatine

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This article presents gate-voltage controlled humidity sensing performance of vanadium dioxide nanoparticles prepared from NH₄VO₃ precursor using microwave irradiation technique. The X-ray diffraction, transmission electron diffraction, and Raman analyses reveal the formation of VO₂ (B) with V₂O₅ and an amorphous phase. The BET surface area is found to be 67.67 m²/g. The humidity sensing measurements using the patented lateral-gate MOSFET configuration was carried out. The results show the optimum response at 5 V up to 8 V of gate voltages for 10 to 80% of relative humidity. The dose-response equation reveals the enhanced resilience of the gated VO₂ sensor which may saturate above 272% humidity. The response and recovery times are remarkably much faster (about 60 s) than in non-gated VO₂ sensors which normally show response and recovery times of the order of 5 minutes (300 s).

Keywords: VO2, VO2 (B), V2O5, MOSFET, gate voltage, humidity sensor.

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Authors: Zhypargul Abdullaeva, Emil Omurzak, Tsutomu Mashimo

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Copper sulfide nanoparticles (CuS) were successfully synthesized by the pulsed plasma in liquid method, using two copper rod electrodes submerged in molten sulfur. Low electrical energy and no high temperature were applied for synthesis. Obtained CuS nanoparticles were then analyzed by means of X-ray diffraction, Low and High Resolution Transmission Electron Microscopy, Electron Diffraction, X-ray Photoelectron, Raman Spectroscopies and Field Emission Scanning Electron Microscopy. XRD analysis revealed peaks for CuS with hexagonal phase composition. TEM and HRTEM studies showed that sizes of CuS nanoparticles ranged between 10-60 nm, with the average size of about 20 nm. Copper sulfide nanoparticles have short nanorod-like structure. Raman spectroscopy found peak for CuS at 474.2cm-1of Raman region.

Keywords: Copper sulfide, Nanoparticles, Pulsed plasma, Synthesis.

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Authors: Ashok V. Borhade, Sanjay G. Wakchaure

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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.

Keywords: Gallosilicate, hydrothermal, nitrite, Reitveldrefinement.

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Authors: Ridzuan Ramli, Norhafzan Junadi, Mohammad D.H. Beg, Rosli M. Yunus

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In this study, microcrystalline cellulose (MCC) was extracted from oil palm empty fruit bunch (EFB) cellulose which was earlier isolated from oil palm EFB fibre. In order to isolate the cellulose, the chlorination method was carried out. Then, the MCC was prepared by simultaneous ultrasonic and alkali treatment from the isolated α-cellulose. Based on mass balance calculation, the yields for MCC obtained from EFB was 44%. For fiber characterization, it is observed that the chemical composition of the hemicellulose and lignin for all samples decreased while composition for cellulose increased. The structural property of the MCC was studied by X-ray diffraction (XRD) method and the result shows that the MCC produced is a cellulose-I polymorph, with 73% crystallinity.

Keywords: Oil palm empty fruit bunch, microcrystalline cellulose, ultrasonic, alkali treatment, X-ray diffraction.

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Authors: Joon Ho Kim, Tae Kwon Ha

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Effect of aging treatment on microstructural aspects of interfacial layers of the Cu/Al clad sheet produced by differential speed rolling (DSR) process were studied by electron back scattered diffraction (EBSD). Clad sheet of Al/Cu has been fabricated by using DSR, which caused severe shear deformation between Al and Cu plate to easily bond to each other. Rolling was carried out at 100^oC with speed ratio of 2, in which the total thickness reduction was 45%. Interface layers of clad sheet were analyzed by EBSD after subsequent annealing at 400^oC for 30 to 120min. With increasing annealing time, thickness of interface layer and fraction of high angle grain boundary were increased and average grain size was decreased.

Keywords: Aluminum/Copper clad sheet, differential speed rolling, interface layer, microstructure, annealing, electron back scattered diffraction.

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Authors: Gülşah Çelik Gül, Figen Kurtuluş

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Magnesium containing boron compounds with hexagonal structure have been drawn much attention due to their superconductive nature. The main target of this work is new modified microwave oven by on our own has an ability about passing through a gas in the oven medium for attainment of oxygen-free compounds such as c-BN.  Mg containing boride was synthesized by modified-microwave method under nitrogen atmosphere using amorphous boron and magnesium source in appropriate molar ratio. Microwave oven with oxygen free environment has been modified to aimed to obtain magnesium boride without oxygen. Characterizations were done by powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Mg containing boride, generally named magnesium boride, with amorphous character without oxygen is obtained via designed microwave oven system.

Keywords: Magnesium containing boron compounds, modified microwave synthesis, powder X-ray diffraction, FTIR.

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Authors: E. Moroydor Derun, N. Tugrul, F. T. Senberber, A. S. Kipcak, S. Piskin

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In this research, copper borates are synthesized by the reaction of copper sulfate pentahydrate (CuSO4.5H2O) and tincalconite (Na2O4B7.10H2O). The experimental parameters are selected as 80oC reaction temperature and 60 of reaction time. The effect of mole ratio of CuSO4.5H2O to Na2O4B7.5H2O is studied. For the identification analyses X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques are used. At the end of the experiments, synthesized copper borate is matched with the powder diffraction file of “00-001-0472” [Cu(BO2)2] and characteristic vibrations between B and O atoms are seen. The proper crystals are obtained at the mole ratio of 3:1. This study showed that simplified synthesis process is suitable for the production of copper borate minerals.

Keywords: Hydrothermal synthesis, copper borates, copper sulfate, tincalconite.

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Authors: G. Çelik Gül, F. Kurtuluş

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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: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq

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Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si₃N₄ confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N₂ plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: Crystallinity, glow discharge, nitriding, sputtering.

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Authors: T.K. Tan, P.S. Khiew, W.S. Chiu, S.Radiman, R.Abd-Shukor, N.M. Huang, H.N. Lim

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In our recent study, we have used ZnO nanoparticles assisted with UV light irradiation to investigate the photocatalytic degradation of Phenol Red (PR). The ZnO photocatalyst was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), specific surface area analysis (BET) and UVvisible spectroscopy. X-ray diffractometry result for the ZnO nanoparticles exhibit normal crystalline phase features. All observed peaks can be indexed to the pure hexagonal wurtzite crystal structures, with the space group of P63mc. There are no other impurities in the diffraction peak. In addition, TEM measurement shows that most of the nanoparticles are rod-like and spherical in shape and fairly monodispersed. A significant degradation of the PR was observed when the catalyst was added into the solution even without the UV light exposure. In addition, the photodegradation increases with the photocatalyst loading. The surface area of the ZnO nanomaterials from the BET measurement was 11.9 m2/g. Besides the photocatalyst loading, the effect of some parameters on the photodegradation efficiency such as initial PR concentration and pH were also studied.

Keywords: Nanostructures, phenol red, zinc oxide, heterogeneous photocatalyst.

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Authors: Wen-Chi Hung, Tung-Kai Liu, Ming-Shan Tsai, Chun-Che Lee, I-Min Jiang

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This study investigates a voltage-controllable liquid crystals lens with a Fresnel zone electrode. When applying a proper voltage on the liquid crystal cell, a Fresnel-zone-distributed electric field is induced to direct liquid crystals aligned in a concentric structure. Owing to the concentrically aligned liquid crystals, a Fresnel lens is formed. We probe the Fresnel liquid crystal lens using a polarized incident beam with a wavelength of 632.8 nm, finding that the diffraction efficiency depends on the applying voltage. A remarkable diffraction efficiency of ~39.5 % is measured at the voltage of 0.9V. Additionally, a dual focus lens is fabricated by attaching a plane-convex lens to the Fresnel liquid crystals cell. The Fresnel LC lens and the dual focus lens may be applied for DVD/CD pick-up head, confocal microscopy system, or electrically-controlling optical systems.

Keywords: Liquid Crystals Lens, Fresnel Lens, and Dual focus

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Authors: Suresh Sagadevan, A. Veeralakshmi

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Cadmium oxide (CdO) nanoparticles have been prepared by chemical coprecipitation method. The synthesized nanoparticles were characterized by X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV analysis, and dielectric studies. The crystalline nature and particle size of the CdO nanoparticles were characterized by Powder X-ray diffraction analysis (XRD). The morphology of prepared CdO nanoparticles was studied by scanning electron microscopy. The particle size was studied using the transmission electron microscopy (TEM).The optical properties were obtained from UV-Vis absorption spectrum. The dielectric properties of CdO nanoparticles were studied in the frequency range of 50 Hz–5 MHz at different temperatures. The frequency dependence of the dielectric constant and dielectric loss is found to decrease with an increase in the frequency at different temperatures. The ac conductivity of CdO nanoparticle has been studied.

Keywords: Cadmium Oxide (CdO), XRD, SEM, Dielectric constant and Dielectric loss.

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Authors: G. Çelik Gül, F. Kurtuluş

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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: Kechida Ahmed, Drai Redouane, Khelil Mohamed

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In this paper we present a new approach to detecting a flaw in T.O.F.D (Time Of Flight Diffraction) type ultrasonic image based on texture features. Texture is one of the most important features used in recognizing patterns in an image. The paper describes texture features based on 2D Gabor functions, i.e., Gaussian shaped band-pass filters, with dyadic treatment of the radial spatial frequency range and multiple orientations, which represent an appropriate choice for tasks requiring simultaneous measurement in both space and frequency domains. The most relevant features are used as input data on a Fuzzy c-mean clustering classifier. The classes that exist are only two: 'defects' or 'no defects'. The proposed approach is tested on the T.O.F.D image achieved at the laboratory and on the industrial field.

Keywords: 2D Gabor Functions, flaw detection, fuzzy c-mean clustering, non destructive testing, texture analysis, T.O.F.D Image (Time of Flight Diffraction).

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Authors: Taposh Roy, Anna Paradowska, Ralph Abrahams, Quan Lai, Michael Law, Peter Mutton, Mehdi Soodi, Wenyi Yan

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In this investigation, a laser cladding process with a powder feeding was used to deposit stainless steel 410L (high strength, excellent resistance to abrasion and corrosion, and great laser compatibility) onto railhead (higher strength, heat treated hypereutectoid rail grade manufactured in accordance with the requirements of European standard EN 13674 Part 1 for R400HT grade), to investigate the development and controllability of process-induced residual stress in the cladding, heat-affected zone (HAZ) and substrate and to analyse their correlation with hardness profile during two different laser cladding directions (across and along the track). Residual stresses were analysed by neutron diffraction at OPAL reactor, ANSTO. Neutron diffraction was carried out on the samples in longitudinal (parallel to the rail), transverse (perpendicular to the rail) and normal (through thickness) directions with high spatial resolution through the thickness. Due to the thick rail and thin cladding, 4 mm thick reference samples were prepared from every specimen by Electric Discharge Machining (EDM). Metallography across the laser claded sample revealed four distinct zones: The clad zone, the dilution zone, HAZ and the substrate. Compressive residual stresses were found in the clad zone and tensile residual stress in the dilution zone and HAZ. Laser cladding in longitudinally cladding induced higher tensile stress in the HAZ, whereas transversely cladding rail showed lower tensile behavior.

Keywords: Laser cladding, residual stress, neutron diffraction, HAZ.

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Authors: E. I. Akpan, S. O. Adeosun, G. I. Lawal, S. A. Balogun, X. D. Chen

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The characterisation of agro-wastes fibres for composite applications from Nigeria using X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM) has been done. Fibres extracted from groundnut shell, coconut husk, rice husk, palm fruit bunch and palm fruit stalk are processed using two novel cellulose fibre production methods developed by the authors. Cellulose apparent crystallinity calculated using the deconvolution of the diffractometer trace shows that the amorphous portion of cellulose was permeable to hydrolysis yielding high crystallinity after treatment. All diffratograms show typical cellulose structure with well-defined 110, 200 and 040 peaks. Palm fruit fibres had the highest 200 crystalline cellulose peaks compared to others and it is an indication of rich cellulose content. Surface examination of the resulting fibres using SEM indicates the presence of regular cellulose network structure with some agglomerated laminated layer of thin leaves of cellulose microfibrils. The surfaces were relatively smooth indicating the removal of hemicellulose, lignin and pectin.

Keywords: X-ray diffraction, SEM, cellulose, deconvolution, crystallinity.

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Authors: Shiyang Zhu, Guo-Qiang Lo, Dim-Lee Kwong

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Although silicon photonic devices provide a significantly larger bandwidth and dissipate a substantially less power than the electronic devices, they suffer from a large size due to the fundamental diffraction limit and the weak optical response of Si. A potential solution is to exploit Si plasmonics, which may not only miniaturize the photonic device far beyond the diffraction limit, but also enhance the optical response in Si due to the electromagnetic field confinement. In this paper, we discuss and summarize the recently developed metal-insulator-Si-insulator-metal nanoplasmonic waveguide as well as various passive and active plasmonic components based on this waveguide, including coupler, bend, power splitter, ring resonator, MZI, modulator, detector, etc. All these plasmonic components are CMOS compatible and could be integrated with electronic and conventional dielectric photonic devices on the same SOI chip. More potential plasmonic devices as well as plasmonic nanocircuits with complex functionalities are also addressed.

Keywords: Silicon nanoplasmonics, Silicon nanophotonics, Onchip integration, CMOS

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Authors: Jung-Ho Moon, Tae Kwon Ha

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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 200^oC 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.

Keywords: Mg alloy, texture, pole figure, ODF, neutron diffraction, warm rolling.

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Authors: Adriana Souza M. Batista, Cláubia Pereira, Luiz O. Faria

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The irradiation of polymeric materials has received much attention because it can produce diverse changes in chemical structure and physical properties. Thus, studying the chemical and structural changes of polymers is important in practice to achieve optimal conditions for the modification of polymers. The effect of gamma irradiation on the crystalline structure of poly(vinylidene fluoride) (PVDF) has been investigated using differential scanning calorimetry (DSC) and X-ray diffraction techniques (XRD). Gamma irradiation was carried out in atmosphere air with doses between 100 kGy at 3,000 kGy with a Co-60 source. In the melting thermogram of the samples irradiated can be seen a bimodal melting endotherm is detected with two melting temperature. The lower melting temperature is attributed to melting of crystals originally present and the higher melting peak due to melting of crystals reorganized upon heat treatment. These results are consistent with those obtained by XRD technique showing increasing crystallinity with increasing irradiation dose, although the melting latent heat is decreasing.

Keywords: Differential scanning calorimetry, gamma irradiation, PVDF, X-ray diffraction technique.

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Authors: M. Yildirim, A. S. Kipcak, F. T. Senberber, M. O. Asensio, E. M. Derun, S. Piskin

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Potassium borates, which are widely used in welding and metal refining industry, as a lubricating oil additive, cement additive, fiberglass additive and insulation compound, are one of the important groups of borate minerals. In this study the production of a potassium borate mineral via hydrothermal method is aimed. The potassium source of potassium nitrate (KNO3) was used along with a sodium source of sodium hydroxide (NaOH) and boron source of boric acid (H3BO3). The constant parameters of reaction temperature and reaction time were determined as 80°C and 1 h, respectively. The molar ratios of 1:1:3 (as KNO3:NaOH:H3BO3), 1:1:4, 1:1:5, 1:1:6 and 1:1:7 were used. Following the synthesis the identifications of the produced products were conducted by X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman Spectroscopy. The results of the experiments and analysis showed in the ratio of 1:1:6, the Santite mineral with powder diffraction file number (pdf no.) of 01-072-1688, which is known as potassium pentaborate (KB5O8·4H2O) was synthesized as best.

Keywords: Hydrothermal synthesis, potassium borate, potassium nitrate, santite.

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Authors: Gyo Woo Lee

Abstract:

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 1200^oC. The averaged diameters of the sintered particles heat treated at 1,260^oC were approximately 80nm.

Keywords: BET Specific Surface Area, Gamma-Al2O3 Nanoparticles, Flame Synthesis, Phase Transition, X-ray Diffraction.

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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: Rania Mustafa

Abstract:

This audit was conducted at Manchester University NHS Foundation Trust, Wythenshawe Hospital Radiology and Accident and Emergency [A&E] Department to assess the appropriateness of clinical information in X-ray requests, specifically in cases of acute ankle injuries. As per the Ottawa Ankle Rules and the recommendations of National Institute for Health and Care Excellence [NICE] and the Royal College of Radiology, we aimed to evaluate the appropriateness of referrals and the thoroughness of clinical information provided by Emergency Department [ED] clinicians for ankle radiography. Our goal was to achieve 100% compliance with these guidelines. The audit involved a comprehensive analysis spanning the period from August 2022 to January 2023, encompassing patient records, radiographic orders, and clinical assessments. Data collection included patient demographics, presenting complaints, clinical assessments, adherence to Ottawa Ankle Rules criteria, and subsequent radiography orders. Here we conducted two audit cycles, involving 38 patients in the first cycle and 86 patients in the second cycle. The data were furtherly filtered to include all patients who were referred from the ED for an ankle Xray with a history of acute trauma and age of more than 18 years. The key finding was that in August 2022, 60% of cases met the Ottawa Ankle Rules criteria accurately, indicating a need for improvement in adherence. However, by January 2023, there was a notable improvement, with 95% of cases accurately meeting the criteria. This significant change reflects an increased alignment with best practices for ankle radiography referrals.

Keywords: Ankle, injuries, Ottawa Ankle Rule, X-rays.

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Authors: Jana P. Vejpravova, Daniel Niznansky, Vaclav Vales, Barbara Bittova, Vaclav Tyrpekl, Stanislav Danis, Vaclav Holy, Stephen Doyle

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The aim of our work is to study phase composition, particle size and magnetic response of Fe2O3/TiO2 nanocomposites with respect to the final annealing temperature. Those nanomaterials are considered as smart catalysts, separable from a liquid/gaseous phase by applied magnetic field. The starting product was obtained by an ecologically acceptable route, based on heterogeneous precipitation of the TiO2 on modified g-Fe2O3 nanocrystals dispersed in water. The precursor was subsequently annealed on air at temperatures ranging from 200 oC to 900 oC. The samples were investigated by synchrotron X-ray powder diffraction (S-PXRD), magnetic measurements and Mössbauer spectroscopy. As evidenced by S-PXRD and Mössbauer spectroscopy, increasing the annealing temperature causes evolution of the phase composition from anatase/maghemite to rutile/hematite, finally above 700 oC the pseudobrookite (Fe2TiO5) also forms. The apparent particle size of the various Fe2O3/TiO2 phases has been determined from the highquality S-PXRD data by using two different approaches: the Rietveld refinement and the Debye method. Magnetic response of the samples is discussed in considering the phase composition and the particle size.

Keywords: X-ray diffraction, profile analysis, Mössbauer spectroscopy, magnetic properties, TiO2, Fe2O3, Fe2TiO5

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Authors: Nuridayanti Che Khalib, Kaliyaperumal Thanigaimani, Suhana Arshad, Ibrahim Abdul Razak

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The 1:1 cocrystal of 2-amino-4-chloro-6- methylpyrimidine (2A4C6MP) with 4-methylbenzoic acid (4MBA) (I) has been prepared by slow evaporation method in methanol, which was crystallized in monoclinic C2/c space group, Z = 8, and a = 28.431 (2) Å, b = 7.3098 (5) Å, c = 14.2622 (10) Å and β = 109.618 (3)°. The presence of unionized –COOH functional group in cocrystal I was identified both by spectral methods (1H and 13C NMR, FTIR) and X-ray diffraction structural analysis. The 2A4C6MP molecule interact with the carboxylic group of the respective 4MBA molecule through N—H⋯O and O—H⋯N hydrogen bonds, forming a cyclic hydrogen–bonded motif R2 2(8). The crystal structure was stabilized by Npyrimidine—H⋯O=C and C=O—H⋯Npyrimidine types hydrogen bonding interactions. Theoretical investigations have been computed by HF and density function (B3LYP) method with 6–311+G (d,p)basis set. The vibrational frequencies together with 1H and 13C NMR chemical shifts have been calculated on the fully optimized geometry of cocrystal I. Theoretical calculations are in good agreement with the experimental results. Solvent–free formation of this cocrystal I is confirmed by powder X-ray diffraction analysis.

Keywords: Supramolecular Cocrystal, 2-amino-4-chloro-6- methylpyrimidine, Hartree-Fock and DFT Studies, Spectroscopic Analysis.

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Authors: Débora N. Zambrano, Marina O. Gosatti, Leandro M. Dufou, Daniel A. Serrano, M. Mónica Guraya, Soledad Perez-Catán

Abstract:

Nanoporous g-Al₂O₃ samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al₂O₃. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al₂O₃ samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al₂O₃, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al₂O₃ for all samples. Also BET specific area values (253-280 m²/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.

Keywords: Nanostructure alumina, boehmite, sol-gel technique, N2 adsorption/desorption isotherm, pore size distribution, BET area.

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Authors: S. S. Sravanthi, Swati Ghosh Acharyya

Abstract:

Automotive light weighting is of major prominence in the current times due to its contribution in improved fuel economy and reduced environmental pollution. Various arc welding technologies are being employed in the production of automobile components with reduced weight. The present study is of practical importance since it involves preferential substitution of Zinc coated mild steel with a light weight alloy such as 6061 Aluminium by means of Gas Metal Arc Welding (GMAW) – Brazing technique at different processing parameters. However, the fabricated joints have shown the generation of Al – Fe layer at the interfacial regions which was confirmed by the Scanning Electron Microscope and Energy Dispersion Spectroscopy. These Al-Fe compounds not only affect the mechanical strength, but also predominantly deteriorate the corrosion resistance of the joints. Hence, it is essential to understand the phases formed in this layer and their crystal structure. Micro area X - ray diffraction technique has been exclusively used for this study. Moreover, the crevice corrosion analysis at the joint interfaces was done by exposing the joints to 5 wt.% FeCl₃ solution at regular time intervals as per ASTM G 48-03. The joints have shown a decreased crevice corrosion resistance with increased heat intensity. Inner surfaces of welds have shown severe oxide cracking and a remarkable weight loss when exposed to concentrated FeCl₃. The weight loss was enhanced with decreased filler wire feed rate and increased heat intensity. 

Keywords: Automobiles, welding, corrosion, lap joints, Micro XRD.

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Authors: M. Ferguson, T. Konkova, I. Violatos

Abstract:

Microstructure analysis of additively manufactured (AM) materials is an important step in understanding the interrelationship between mechanical properties and materials performance. Literature on the effect of a laser-based AM process parameters on the microstructure in the substrate-deposit interface is limited. The interface region, the adjoining area of substrate and deposit, is characterized by the presence of the fusion zone (FZ) and heat affected zone (HAZ) experiencing rapid thermal gyrations resulting in thermal induced transformations. Inconel 718 was utilized as a work material for both the substrate and deposit. Three blocks of Inconel 718 material were deposited by Direct Energy Deposition (DED) using three different laser powers, 550W, 750W and 950W, respectively. A coupled thermo-mechanical transient approach was utilized to correlate temperature history to the evolution of microstructure. Thermal history of the deposition process was monitored with the thermocouples installed inside the substrate material. Interface region of the blocks were analysed with Optical Microscopy (OM) and Scanning Electron Microscopy (SEM) including electron back-scattered diffraction (EBSD) technique. Laser power was found to influence the dissolution of intermetallic precipitated phases in the substrate and grain growth in the interface region. Microstructure and thermal history data were utilized to draw conclusive comparisons between the investigated process parameters.

Keywords: Additive manufacturing, direct energy deposition, electron back-scatter diffraction, finite element analysis, Inconel 718, microstructure, optical microscopy, scanning electron microscopy, substrate-deposit interface region.

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Authors: M. M. Hasan, A. S. M. A. Haseeb, R. Saidur, H. H. Masjuki

Abstract:

In this investigation, anatase TiO2 thin films were grown by radio frequency magnetron sputtering on glass substrates at a high sputtering pressure and room temperature. The anatase films were then annealed at 300-600 °C in air for a period of 1 hour. To examine the structure and morphology of the films, X-ray diffraction (XRD) and atomic force microscopy (AFM) methods were used respectively. From X-ray diffraction patterns of the TiO2 films, it was found that the as-deposited film showed some differences compared with the annealed films and the intensities of the peaks of the crystalline phase increased with the increase of annealing temperature. From AFM images, the distinct variations in the morphology of the thin films were also observed. The optical constants were characterized using the transmission spectra of the films obtained by UV-VIS-IR spectrophotometer. Besides, optical thickness of the film deposited at room temperature was calculated and cross-checked by taking a cross-sectional image through SEM. The optical band gaps were evaluated through Tauc model. It was observed that TiO2 films produced at room temperatures exhibited high visible transmittance and transmittance decreased slightly with the increase of annealing temperatures. The films were found to be crystalline having anatase phase. The refractive index of the films was found from 2.31-2.35 in the visible range. The extinction coefficient was nearly zero in the visible range and was found to increase with annealing temperature. The allowed indirect optical band gap of the films was estimated to be in the range from 3.39 to 3.42 eV which showed a small variation. The allowed direct band gap was found to increase from 3.67 to 3.72 eV. The porosity was also found to decrease at a higher annealing temperature making the film compact and dense.

Keywords: Titanium dioxide, RF reactive sputtering, Structuralproperties, Surface morphology, Optical properties.

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