Search results for: Bragg diffraction

Authors: Mohsen Sanayei, Jerzy Szpunar

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The present study investigates the effects of deformation strain and annealing temperature on the formation of twin boundaries, deformation and recrystallization texture evolution and grain boundary networks and connectivity. The resulting microstructures were characterized using Electron Backscatter Diffraction (EBSD) and X-Ray Diffraction (XRD) both immediately following small amount of deformation and after short time annealing at high temperature to correlate the micro and macro texture evolution of these alloys. Furthermore, this study showed that the process of grain boundary engineering, consisting cycles of deformation and annealing, is found to substantially reduce the mass and size of random boundaries and increase the proportion of low Coincidence Site Lattice (CSL) grain boundaries.

Keywords: coincidence site lattice, grain boundary engineering, electron backscatter diffraction, texture, x-ray diffraction

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Authors: Maurizio Dapor, Isabel Abril, Pablo de Vera, Rafael Garcia-Molina

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The ionization yield of ion tracks in polymers and bio-molecular systems reaches a maximum, known as the Bragg peak, close to the end of the ion trajectories. Along the path of the ions through the materials, many electrons are generated, which produce a cascade of further ionizations and, consequently, a shower of secondary electrons. Among these, very low energy secondary electrons can produce damage in the biomolecules by dissociative electron attachment. This work deals with the calculation of the energy distribution of electrons produced by protons in a sample of polymethylmethacrylate (PMMA), a material that is used as a phantom for living tissues in hadron therapy. PMMA is also of relevance for microelectronics in CMOS technologies and as a photoresist mask in electron beam lithography. We present a Monte Carlo code that, starting from a realistic description of the energy distribution of the electrons ejected by protons moving through PMMA, simulates the entire cascade of generated secondary electrons. By following in detail the motion of all these electrons, we find the radial distribution of the energy that they deposit in PMMA for several initial proton energies characteristic of the Bragg peak.

Keywords: Monte Carlo method, secondary electrons, energetic ions, ion-beam cancer therapy, ionization cross section, polymethylmethacrylate, proton beams, secondary electrons, radial energy distribution

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Authors: B. Atli-Veltin, A. Vosteen, D. Megan, A. Jedynska, L. K. Cheng

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Composite materials combine the advantages of being lightweight and possessing high strength. This is in particular of interest for the development of large constructions, e.g., aircraft, space applications, wind turbines, etc. One of the shortcomings of using composite materials is the complex nature of the failure mechanisms which makes it difficult to predict the remaining lifetime. Therefore, condition and health monitoring are essential for using composite material for critical parts of a construction. Different types of sensors are used/developed to monitor composite structures. These include ultrasonic, thermography, shearography and fiber optic. The first 3 technologies are complex and mostly used for measurement in laboratory or during maintenance of the construction. Optical fiber sensor can be surface mounted or embedded in the composite construction to provide the unique advantage of in-operation measurement of mechanical strain and other parameters of interest. This is identified to be a promising technology for Structural Health Monitoring (SHM) or Prognostic Health Monitoring (PHM) of composite constructions. Among the different fiber optic sensing technologies, Fiber Bragg Grating (FBG) sensor is the most mature and widely used. FBG sensors can be realized in an array configuration with many FBGs in a single optical fiber. In the current project, different aspects of using embedded FBG for composite wind turbine monitoring are investigated. The activities are divided into two parts. Firstly, FBG embedded carbon composite laminate is subjected to tensile and bending loading to investigate the response of FBG which are placed in different orientations with respect to the fiber. Secondly, the demonstration of using FBG sensor array for temperature and strain sensing and monitoring of a 5 m long scale model of a glass fiber mono-pile is investigated. Two different FBG types are used; special in-house fibers and off-the-shelf ones. The results from the first part of the study are showing that the FBG sensors survive the conditions during the production of the laminate. The test results from the tensile and the bending experiments are indicating that the sensors successfully response to the change of strain. The measurements from the sensors will be correlated with the strain gauges that are placed on the surface of the laminates.

Keywords: Fiber Bragg Gratings, embedded sensors, health monitoring, wind turbine towers

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Authors: Karthika Chandran, Pulkit Prakash, Amitabh Das, Santhosh P. N.

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Rare earth orthoferrites (RFeO₃) exhibit interesting and useful magnetic properties like multiferroicity, magnetodielectric coupling, spin reorientation (SR) and exchange bias. B site doped RFeO₃ are attracting attention due to the complex and tuneable magnetic transitions. In this work, 45% Mn-doped HoFeO₃ polycrystalline sample (HoFe₀.₅₅Mn₀.₄₅O₃) was synthesized by a solid-state reaction method. The magnetic structure and transitions were studied by magnetization measurements and neutron powder diffraction methods. The neutron diffraction patterns were taken at 13 different temperatures from 7°K to 300°K (7°K and 25°K to 300°K in 25°K intervals). The Rietveld refinement was carried out by using a FULLPROF suite. The magnetic space groups and the irreducible representations were obtained by SARAh module. The room temperature neutron diffraction refinement results indicate that the sample crystallizes in an orthorhombic perovskite structure with Pnma space group with lattice parameters a = 5.6626(3) Ǻ, b = 7.5241(3) Ǻ and c = 5.2704(2) Ǻ. The temperature dependent magnetization (M-T) studies indicate the presence of two magnetic transitions in the system ( TN Fe/Mn~330°K and TSR Fe/Mn ~290°K). The inverse susceptibility vs. temperature curve shows a linear behavior above 330°K. The Curie-Weiss fit in this region gives negative Curie constant (-34.9°K) indicating the antiferromagnetic nature of the transition. The neutron diffraction refinement results indicate the presence of mixed magnetic phases Γ₄(AₓFᵧG

Keywords: neutron powder diffraction, rare earth orthoferrites, Rietveld analysis, spin reorientation

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Authors: Sonam Behl, Raju, Ginu Rajan, Paul Farrar, B. Gangadhara Prusty

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Reinforcing dental composites with micro-sized fibres can significantly improve the physio-mechanical properties of dental composites. The short fibres can be oriented randomly within dental composites, thus providing quasi-isotropic reinforcing efficiency unlike unidirectional/bidirectional fibre reinforced composites enhancing anisotropic properties. Thus, short fibres reinforced dental composites are getting popular among practitioners. However, despite their popularity, resin-based dental composites are prone to failure on account of shrinkage during photo polymerisation. The shrinkage in the structure may lead to marginal gap formation, causing secondary caries, thus ultimately inducing failure of the restoration. The traditional methods to evaluate polymerisation shrinkage using strain gauges, density-based measurements, dilatometer, or bonded-disk focuses on average value of volumetric shrinkage. Moreover, the results obtained from traditional methods are sensitive to the specimen geometry. The present research aims to evaluate the real-time shrinkage strain at selected locations in the material with the help of optical fibre Bragg grating (FBG) sensors. Due to the miniature size (diameter 250 µm) of FBG sensors, they can be easily embedded into small samples of dental composites. Furthermore, an FBG array into the system can map the real-time shrinkage strain at different regions of the composite. The evaluation of real-time monitoring of shrinkage values may help to optimise the physio-mechanical properties of composites. Previously, FBG sensors have been able to rightfully measure polymerisation strains of anisotropic (unidirectional or bidirectional) reinforced dental composites. However, very limited study exists to establish the validity of FBG based sensors to evaluate volumetric shrinkage for randomly oriented fibres reinforced composites. The present study aims to fill this research gap and is focussed on establishing the usage of FBG based sensors for evaluating the shrinkage of dental composites reinforced with randomly oriented fibres. Three groups of specimens were prepared by mixing the resin (80% UDMA/20% TEGDMA) with 55% of silane treated BaAlSiO₂ particulate fillers or by adding 5% of micro-sized fibres of diameter 5 µm, and length 250/350 µm along with 50% of silane treated BaAlSiO₂ particulate fillers into the resin. For measurement of polymerisation shrinkage strain, an array of three fibre Bragg grating sensors was embedded at a depth of 1 mm into a circular Teflon mould of diameter 15 mm and depth 2 mm. The results obtained are compared with the traditional method for evaluation of the volumetric shrinkage using density-based measurements. Degree of conversion was measured using FTIR spectroscopy (Spotlight 400 FT-IR from PerkinElmer). It is expected that the average polymerisation shrinkage strain values for dental composites reinforced with micro-sized fibres can directly correlate with the measured degree of conversion values, implying that more C=C double bond conversion to C-C single bond values also leads to higher shrinkage strain within the composite. Moreover, it could be established the photonics approach could help assess the shrinkage at any point of interest in the material, suggesting that fibre-Bragg grating sensors are a suitable means for measuring real-time polymerisation shrinkage strain for randomly fibre reinforced dental composites as well.

Keywords: dental composite, glass fibre, polymerisation shrinkage strain, fibre-Bragg grating sensors

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Authors: Shahriar Ghammamy, Mehrnoosh Saboony

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Purpose: To evaluate the spectral specification (IR-XRD and SEM) of nano-ciprofloxacin that prepared by up-down method (satellite mill). Methods: the ciprofloxacin was minimized to nano-scale with satellite mill and its characterization evaluated by Infrared spectroscopy, XRD diffraction and semi electron microscope (SEM). Expectation enhances the antibacterial property of nano-ciprofloxacin in comparison to ciprofloxacin. IR spectrum of nano-ciprofloxacin compared with spectrum of ciprofloxacin, and both of them were almost agreement with a difference: the peaks in spectrum of nano-ciprofloxacin were sharper than peaks in spectrum of ciprofloxacin. X-Ray powder diffraction analysis of nano-ciprofloxacin shows the diameter of particles equal to 90.9nm. (on the basis of Scherer Equation). SEM image shows the global shape for nano-ciprofloxacin.

Keywords: antibiotic, ciprofloxacin, nano, IR, XRD, SEM

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Authors: Shahriar Ghammamy, Mehrnoosh Saboony

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Purpose: to evaluate the spectral specification(IR-XRD and SEM) of nano ciprofloxacin that prepared by up-down method (satellite mill). Methods: the ciprofloxacin was minimized to nano-scale with satellite mill and it,s characterization evaluated by Infrared spectroscopy, XRD diffraction and semi electron microscope (SEM). Expectation: to enhance the antibacterial property of nano ciprofloxacin in comparison to ciprofloxacin.IR spectrum of nano ciprofloxacin compared with spectrum of ciprofloxacin, and both of them were almost agreement with a difference: the peaks in spectrum of nano ciprofloxacin was sharper than peaks in spectrum of ciprofloxacin. X-Ray powder diffraction analysis of nano ciprofloxacin showes the diameter of particles equal to 90.9 nm (on the basis of scherrer equation). SEM image showes the global shape for nano ciprofloxacin.

Keywords: antibiotic, ciprofloxacin, nano, IR, XRD, SEM

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Authors: Jaroslav Fiala, Jaroslav Kaiser, Pavel Zlabek, Vaclav Mentl

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The X-ray diffraction technique was recognized as a useful tool for the assessment of material degradation degree after a long-time service. In many industrial applications materials are subjected to degradation of mechanical properties as a result of real service conditions. The assessment of the remnant lifetime of components and structures is commonly based on correlated procedures including numerous destructive, non-destructive and mathematical techniques that should guarantee reasonable precise assessment of the current damage extent of materials in question and the remnant lifetime assessment. This paper summarizes results of an experimental programme concentrated on mechanical properties degradation of welded components. Steel an Al-alloy test specimens of base metal, containing welds and simple weldments were fatigue loaded at room temperature to obtain Woehler S-N curve. X-ray diffraction technique was applied to assess the degradation degree of material as a result of cyclic loading.

Keywords: fatigue loading, material degradation, steels, AL-alloys, X-ray diffraction

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Authors: G. Farkas, K. Mathis, J. Pilch, P. Minarik

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Deformation mechanisms in an Mg-Al-Ca alloy reinforced with short alumina fibres were studied by acoustic emission and in-situ neutron diffraction method. The fibres plane orientation with respect to the loading axis was found to be a key parameter, which influences the acting deformation processes, such as twinning or dislocation slip. In-situ neutron diffraction tests were measured at different temperatures from room temperature (RT) to 200°C. The measurement shows the lattice strain changes in the matrix and also in the reinforcement phase depending on macroscopic compressive deformation and stress. In case of parallel fibre plane orientation, the increment of compressive lattice strain is lower in the matrix and higher in the fibres in comparison to perpendicular fibre orientation. Furthermore, acoustic emission results indicate a larger twinning activity and more frequent fibre cracking in sample with perpendicular fibre plane orientation. Both types of mechanisms are more dominant at elevated temperatures.

Keywords: neutron diffraction, acoustic emission, magnesium based composite, deformation mechanisms

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Authors: Shaila Bahl, S. P. Lochab, Pratik Kumar

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Nanotechnology and nanomaterials have attracted researchers from different fields, especially from the field of luminescence. Recent studies on various luminescent nanomaterials have shown their relevance in dosimetry of ionizing radiations for the measurements of high doses using the Thermoluminescence (TL) technique, where the conventional microcrystalline phosphors saturate. Ion beams have been used for diagnostic and therapeutic purposes due to their favorable profile of dose deposition at the end of the range known as the Bragg peak. While dealing with human beings, doses from these beams need to be measured with great precision and accuracy. Henceforth detailed investigations of suitable thermoluminescent dosimeters (TLD) for dose verification in ion beam irradiation are required. This paper investigates the TL response of nanocrystalline BaSO4 doped with Eu to 85 MeV carbon beam. The synthesis was done using Co-precipitation technique by mixing Barium chloride and ammonium sulphate solutions. To investigate the crystallinity and particle size, analytical techniques such as X-ray diffraction (XRD) and Transmission electron microscopy (TEM) were used which revealed the average particle sizes to 45 nm with orthorhombic structure. Samples in pellet form were irradiated by 85 MeV carbon beam in the fluence range of 1X1010-5X1013. TL glow curves of the irradiated samples show two prominent glow peaks at around 460 K and 495 K. The TL response is linear up to 1X1013 fluence after which saturation was observed. The wider linear TL response of nanocrystalline BaSO4: Eu and low fading make it a superior candidate as a dosimeter to be used for detecting the doses of carbon beam.

Keywords: radiation, dosimetry, carbon ions, thermoluminescence

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Authors: Hanan Alenezi

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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: Joel Ballesteros, Harriet Jane Caleja, Florian Del Mundo, Cherrie Pascual

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Diffraction-based sensing was utilized in the quantification of human ferritin in blood serum to provide an alternative to label-based immunoassays currently used in clinical diagnostics and researches. The diffraction intensity was measured by the diffractive optics technology or dotLab™ system. Two methods were evaluated in this study: direct immunoassay and direct sandwich immunoassay. In the direct immunoassay, human ferritin was captured by human ferritin antibodies immobilized on an avidin-coated sensor while the direct sandwich immunoassay had an additional step for the binding of a detector human ferritin antibody on the analyte complex. Both methods were repeatable with coefficient of variation values below 15%. The direct sandwich immunoassay had a linear response from 10 to 500 ng/mL which is wider than the 100-500 ng/mL of the direct immunoassay. The direct sandwich immunoassay also has a higher calibration sensitivity with value 0.002 Diffractive Intensity (ng mL-1)-1) compared to the 0.004 Diffractive Intensity (ng mL-1)-1 of the direct immunoassay. The limit of detection and limit of quantification values of the direct immunoassay were found to be 29 ng/mL and 98 ng/mL, respectively, while the direct sandwich immunoassay has a limit of detection (LOD) of 2.5 ng/mL and a limit of quantification (LOQ) of 8.2 ng/mL. In terms of accuracy, the direct immunoassay had a percent recovery of 88.8-93.0% in PBS while the direct sandwich immunoassay had 94.1 to 97.2%. Based on the results, the direct sandwich immunoassay is a better diffraction-based immunoassay in terms of accuracy, LOD, LOQ, linear range, and sensitivity. The direct sandwich immunoassay was utilized in the determination of human ferritin in blood serum and the results are validated by Chemiluminescent Magnetic Immunoassay (CMIA). The calculated Pearson correlation coefficient was 0.995 and the p-values of the paired-sample t-test were less than 0.5 which show that the results of the direct sandwich immunoassay was comparable to that of CMIA and could be utilized as an alternative analytical method.

Keywords: biosensor, diffraction, ferritin, immunoassay

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Authors: Nassima Hamzaoui, Mostefa Ghamnia

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Nanoscale thin films of pure and Mn-doped Nickel oxide (NiO) were prepared by dissolving nickel chloride hexahydrate (NiCl2, 6H2O) and manganese chloride tetrahydrate (MnCl2,4H2O) under experimental conditions. The resulting solution was stirred at room temperature for 30 OC minutes in order to obtain homogeneity. The solution was sprayed onto heated glass substrates. The films obtained were characterized by X-ray diffraction to verify crystallinity. Atomic force microscopy (AFM) reveals surface topographical structure. UV-visible spectroscopy shows good transparency of the NiO layers.

Keywords: films, NiO, AFM, X-ray diffraction

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Authors: Ahmed Nouainia, Mohamed Hajji, Taoufik Aguili

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In this paper, an electromagnetic analysis is presented for describing the influence of shielding in a rectangular waveguide. A hybridization based on the method of moments combined to the generalized equivalent circuit MoM-GEC is used to model the problem. This is validated by applying the MoM-GEC hybridization to investigate a diffraction structure. It consists of electromagnetic diffraction by an iris in a rectangular waveguide. Numerical results are shown and discussed and a comparison with FEM and Marcuvitz methods is achieved.

Keywords: method MoM-GEC, waveguide, shielding, equivalent circuit

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Authors: Yih-Chien Chen, Tse-Lung Lin

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The microwave characteristics of NdTi₍₀.₅₋ₓ₎GeₓMo₀.₅O₄ are studied to determine the feasibility of their use in the liquid sensor. The microwave characteristics of NdTi₍₀.₅₋ₓ₎GeₓMo₀.₅O₄ are determined using X-ray diffraction (XRD) patterns. The permittivity (𝜀r) of NdTi₍₀.₄₉₎Ge₀.₀₁Mo₀.₅O₄ that is sintered at 1425 ℃ for 4 h is 17.6, the unloaded quality factor (Qu×f) is 33,400 GHz, and it has a temperature coefficient at the resonance frequency (TCF) of -30.7 ppm/℃. The proposed liquid sensor is at the 5G FR1 bands.

Keywords: NdTi₍₀.₅₋ₓ₎GeₓMo₀.₅O₄, X-ray diffraction pattern, permittivity, Unloaded quality factor

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Authors: G. Vinitha, A. Ramalingam

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In view of a possible application in optical data storage devices, diffraction grating efficiency of an organic dye, Acid Fuchsin doped in PMMA matrix was studied under excitation with CW diode pumped Nd: YAG laser at 532 nm. The open aperture Z-scan of dye doped polymer displayed saturable absorption and the closed aperture Z-scan of the samples exhibited negative nonlinearity. The diffraction efficiency of the grating is the ratio of the intensity of the first order diffracted power to the incident read beam power. The dye doped polymer films were found to be good media for recording. It is observed that the formation of gratings strongly depend on the concentration of dye in the polymer film, the intensity ratios of the writing beams and the angle between the writing beams. It has been found that efficient writing can be made at an angle of 20° and when the intensity ratio of the writing beams is unity.

Keywords: diffraction efficiency, nonlinear optical material, saturable absorption, surface-relief-gratings

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Authors: Fatai O. Oladoyinbo, Felix O. Sanni, Akinwunmi Fatai, Kamoli A. Amusa, Saheed A. Ganiyu, Wasiu B. Ayinde, Tajudeen A. Afolabi, Enock O. Dare

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Silver (Ag) and silica (SiO2) nanoparticles were synthesized using the chemical reduction method from silver nitrate and sodium silicate, respectively. X-ray Diffraction (XRD), High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), Uv-Visible spectroscopy, Energy Dispersive X-ray (EDX) spectroscopy and N2 adsorption-desorption techniques were utilized to characterize the composition and structure of the samples. The crystallinity pattern of Ag nanoparticles was indexed as (111), (200), (220) and (311), which allowed reflections from face-centered cubic silver. XRD of SiO2 showed good porosity with a broad-spectrum band at Bragg’s angle 2θ of 22° while that of Ag-SiO2 showed distinct peaks at 2θ values of 39°, 43°, 66° and 79°. The XRD result agreed perfectly with the SEM and HRTEM images which showed Ag-SiO2 isotropic and anisotropic under the varying concentration of reactants. The elemental composition of Ag-SiO2, as displayed by EDX, confirmed Ag enrichment in the Ag-SiO2 heterostructure. The Uv-Visible peak at 421 nm confirmed the Surface Plasmon Resonance absorption peak of silver nanoparticles. N2 adsorption-desorption result showed a broad band of Ag-SiO2 from 3 to 8 nm, which indicated relatively narrow pore size distributions. Humidity sensing measurements performed in a controlled humidity chamber showed very high sensitivity with a sensitivity factor (SF) of 4.63 and high linearity with a steady decrease in resistance to humidity from 880 Ω at 10% RH to 190 Ω at 100% RH, indicating that Ag-SiO2 nanocomposite is a good sensing material with high sensitivity and linearity.

Keywords: silver, silica, nanocomposite, synthesis, heterostructure, core shell

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Authors: M. R. Akbari , H. Yousefnia, E. Mirrezaei

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Range uncertainties of protons are currently a topic of interest in proton therapy. Two of the parameters that are often used to specify proton range are water equivalent thickness (WET) and water equivalent ratio (WER). Since WER values for a specific material is nearly constant at different proton energies, it is a more useful parameter to compare. In this study, WER values were calculated for different proton energies in polymethyl methacrylate (PMMA), polystyrene (PS) and aluminum (Al) using FLUKA and TRIM codes. The results were compared with analytical, experimental and simulated SEICS code data obtained from the literature. In FLUKA simulation, a cylindrical phantom, 1000 mm in height and 300 mm in diameter, filled with the studied materials was simulated. A typical mono-energetic proton pencil beam in a wide range of incident energies usually applied in proton therapy (50 MeV to 225 MeV) impinges normally on the phantom. In order to obtain the WER values for the considered materials, cylindrical detectors, 1 mm in height and 20 mm in diameter, were also simulated along the beam trajectory in the phantom. In TRIM calculations, type of projectile, energy and angle of incidence, type of target material and thickness should be defined. The mode of 'detailed calculation with full damage cascades' was selected for proton transport in the target material. The biggest difference in WER values between the codes was 3.19%, 1.9% and 0.67% for Al, PMMA and PS, respectively. In Al and PMMA, the biggest difference between each code and experimental data was 1.08%, 1.26%, 2.55%, 0.94%, 0.77% and 0.95% for SEICS, FLUKA and SRIM, respectively. FLUKA and SEICS had the greatest agreement (≤0.77% difference in PMMA and ≤1.08% difference in Al, respectively) with the available experimental data in this study. It is concluded that, FLUKA and TRIM codes have capability for Bragg curves simulation and WER values calculation in the studied materials. They can also predict Bragg peak location and range of proton beams with acceptable accuracy.

Keywords: water equivalent ratio, dosimetric materials, proton therapy, Monte Carlo simulations

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Authors: Suresh Palla, Kalpna Sharma, Gaurav Bhatnagar, S. K. Chaturvedi, B. N. Mohapatra

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Determining the content of free lime is especially important to judge reactivity of the raw materials and clinker quality. The free lime limit isn’t the same for all cements; it depends on several factors, especially the temperature reached during the cooking and the grain size distribution in cement after grinding. Estimation of free lime by conventional method is influenced by the presence of portlandite and misleads the actual free lime content in the clinker for quality check up conditions. To ensure the product quality according to the standard specifications in terms of within the quality limits or not, a reliable, precise, and very reproducible method to quantify the relative phase abundances in the Portland Cement clinker and Portland Cements is to use X-ray diffraction (XRD) in combination with the Rietveld method. In the present study, a methodology was proposed using XRD to validate the obtained results of free lime by conventional method. The XRD and TG/DTA results confirm the presence of portlandite in the clinker to take the decision on the obtained free lime results through conventional method.

Keywords: free lime, quantitative phase analysis, conventional method, x ray diffraction

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Authors: Gülşah Çelik Gül, Figen Kurtuluş

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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: Raphaelle Guillou, Matthieu Le Saux, Jean-Christophe Brachet, Thomas Guilbert, Elodie Rouesne, Denis Menut, Caroline Toffolon-Masclet, Dominique Thiaudiere

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In some hypothetical accidental situations, such as during a Loss Of Coolant Accident (LOCA) in pressurized water reactors, fuel cladding tubes made of zirconium alloys can be exposed for a few minutes to steam at High Temperature (HT up to 1200°C) before being cooled and then quenched in water. Under LOCA-like conditions, the cladding undergoes a number of metallurgical changes (phase transformations, oxygen diffusion and growth of an oxide layer...) and is consequently submitted to internal stresses whose state evolves during the transient. These stresses can have an effect on the oxide structure and the oxidation kinetics of the material. They evolve during cooling, owing to differences between the thermal expansion coefficients of the various phases and phase transformations of the metal and the oxide. These stresses may result in the failure of the cladding during quenching, once the material is embrittled by oxidation. In order to progress in the evaluation of these internal stresses, X-ray diffraction experiments were performed in-situ under synchrotron radiation during HT oxidation and subsequent cooling on Zircaloy-4 sheet samples. First, structural evolutions, such as phase transformations, have been studied as a function of temperature for both the oxide layer and the metallic substrate. Then, internal stresses generated within the material oxidized at temperatures between 700 and 900°C have been evaluated thanks to the 2θ diffraction peak position shift measured during the in-situ experiments. Electron backscatter diffraction (EBSD) analysis was performed on the samples after cooling in order to characterize their crystallographic texture. Furthermore, macroscopic strains induced by oxidation in the conditions investigated during the in-situ X-ray diffraction experiments were measured in-situ in a dilatometer.

Keywords: APRP, stains measurements, synchrotron diffraction, zirconium allows

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Authors: Sheo K. Mishra, Rajneesh K. Srivastava, R. K. Shukla

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In the present work, we report on the optical properties including UV-vis absorption and photoluminescence (PL) of ZnO nanostructures synthesized by sol-gel method. Structural and morphological investigations have been performed by X-ray diffraction method (XRD) and scanning electron microscopy (SEM). The XRD result confirms the formation of hexagonal wurtzite phase of ZnO nanostructures. The presence of various diffraction peaks suggests polycrystalline nature. The XRD pattern exhibits no additional peak due to by-products such as Zn(OH)2. The average crystallite size of prepared ZnO sample corresponding to the maximum intensity peaks is to be ~38.22 nm. The SEM micrograph shows different nanostructures of pure ZnO. Photoluminescence (PL) spectrum shows several emission peaks around 353 nm, 382 nm, 419 nm, 441 nm, 483 nm and 522 nm. The obtained results suggest that the prepared phosphors are quite suitable for optoelectronic applications.

Keywords: ZnO, sol-gel, XRD, PL

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Authors: Shahriar Ghammamy, Maryam Gholipoor

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Metronidazole nano -powders with the average mean particle size around 90 nm were synthesized by high-energy milling using a planetary ball mill is provided. The Scattering factors, milling of time,the ball size and ball to powder ratio on the material properties powder by the Ray diffraction (XRD) study, scanning electron microscopy (SEM), IR. It has been observed that the density of nano-sized grinding balls as ball to powder ratio depends. Using the dispersion factor, the density Can be reduced below the initial particle size was achieved.

Keywords: metronidazole, ball-milling, nanoparticles, characterization, XRD diffraction

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Authors: D. Gazdič, I. Hájková, M. Fridrichová

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This paper involved the performance of a high-temperature X-Ray powder diffraction analysis (XRD) of a sample of chemical gypsum generated in the production of titanium white; this gypsum originates by neutralizing highly acidic water with limestone suspension. Specifically, it was gypsum formed in the first stage of neutralization when the resulting material contains, apart from gypsum, a number of waste products resulting from the decomposition of ilmenite by sulphuric acid. So it can be described as red titanogypsum. By conducting the experiment using XRD apparatus Bruker D8 Advance with a Cu anode (λkα=1.54184 Å) equipped with high-temperature chamber Anton Paar HTK 16, it was possible to identify clearly in the sample each phase transition in the system of CaSO4•xH2O.

Keywords: anhydrite, gypsum, bassanite, hematite, XRD, powder, high-temperature

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Authors: Mohsen Sanayei, Jerzy Szpunar, Sami Penttilä

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Exposure of Nickel-based superalloys to high temperature and harsh environment such as Super-Critical Water (SCW) environment leads to the formation of oxide scales composed of multiple and complex phases that are difficult to differentiate with conventional analysis techniques. In this study, we used simultaneous Electron Backscatter Diffraction (EBSD) and Energy Dispersive X-ray Spectroscopy (EDS) to analyze the complex oxide scales formed on several Nickel-based Superalloys exposed to high temperature SCW. Multi-layered structures of Iron, Nickel, Chromium and Molybdenum oxides and spinels were clearly identified using the simultaneous EBSD-EDS analysis technique. Furthermore, the orientation relationship between the oxide scales and the substrate has been investigated.

Keywords: electron backscatter diffraction, energy dispersive x-ray spectroscopy, superalloy, super-critical water

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Authors: Flóra Pomázi, Sándor Baranya, Zoltán Szalai

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A harmonized monitoring of the suspended sediment transport along such a large river as the world’s most international river, the Danube River, is a rather challenging task. The traditional monitoring method in Hungary is obsolete but using indirect measurement devices and techniques like optical backscatter sensors (OBS), laser diffraction or acoustic backscatter sensors (ABS) could provide a fast and efficient alternative option of direct methods. However, these methods are strongly sensitive to the particle characteristics (i.e. particle shape, particle size and mineral composition). The current method does not provide sufficient information about particle size distribution, mineral analysis is rarely done, and the shape of the suspended sediment particles have not been examined yet. The aims of the study are (1) to determine the particle characterisation of suspended sediment in the Danube River using advanced particle characterisation methods as laser diffraction and automated imaging, and (2) to perform a sensitivity analysis of the indirect methods in order to determine the impact of suspended particle characteristics. The particle size distribution is determined by laser diffraction. The particle shape and mineral composition analysis is done by the Morphologi G3ID image analyser. The investigated indirect measurement devices are the LISST-Portable|XR, the LISST-ABS (Sequoia Inc.) and the Rio Grande 1200 kHz ADCP (Teledyne Marine). The major findings of this study are (1) the statistical shape of the suspended sediment particle - this is the first research in this context, (2) the actualised particle size distribution – that can be compared to historical information, so that the morphological changes can be tracked, (3) the actual mineral composition of the suspended sediment in the Danube River, and (4) the reliability of the tested indirect methods has been increased – based on the results of the sensitivity analysis and the previous findings.

Keywords: advanced particle characterisation, automated imaging, indirect methods, laser diffraction, mineral composition, suspended sediment

Procedia PDF Downloads 111

Authors: I. Bouhaf Kharkhachi, A. Attaf

Abstract:

Tin sulfide thin films on glass substrate were prepared by spray ultrasonic technique, at different experimental conditions. The influence of deposition time (2, 4, 6, 8 and 10 min) on different properties of thin films, such us, (XRD) and (UV) spectroscopy visible spectrum was investigated. X-ray diffraction showing that thin films crystallized in SnS, SnS2, and Sn2S3 phases. The results of (UV) spectroscopy visible spectrum show that films deposited at 4 min are large transmittance 60% in the visible region.

Keywords: SnS, thin films, ultrasonic spray, X-ray diffraction, UV spectroscopy visible

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Authors: Chandni Rani, S. D. Tiwari

Abstract:

Ferrihydrite is one of the distinct minerals in the family of oxides, hydroxides and oxyhydroxides of iron. It is a nanocrystalline material. It occurs naturally in different sediments, soil systems and also found in the core of ferritin, an iron storage protien. This material can also be synthesized by suitable chemical methods in laboratories. This is known as less crystalline Iron (III) Oxyhydroxide. Due to its poor crystallinity, there are very broad peaks in x-ray diffraction. Depending on the number of peaks in x-ray diffraction pattern, it is classified as two lines and six lines ferrihydrite. The average crystallite size for these two forms is found to be about 2nm to 5nm. The exact crystal structure of this system is still under debate. Out of these two forms, the six lines ferrihydrite is more ordered in comparison to two lines ferrihydrite. The magnetic behavior of two lines ferrihydrite nanoparticles is somewhat well studied. But the magnetic behavior of six lines ferrihydrite nanoparticles could not attract the attention of researchers much. This motivated us to work on the magnetic properties of six lines ferrihydrite nanoparticles. In this work, we present synthesis, structural characterization and magnetic behavior of 5 nm six lines ferrihydrite nanoparticles. X-ray diffraction and transmission electron microscope are used for structural characterization of this system. Magnetization measurements are performed to fit the data at different temperatures. Then the effect of magnetic moment distribution is also found. All these observations are discussed in detail.

Keywords: nanoparticles, magnetism, superparamagnetism, magnetic anisotropy

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Authors: Gülşah Çelik Gül, Figen 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 modified-microwave 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/differantial thermal analysis (TG/DTA).

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

Procedia PDF Downloads 569

Authors: Maria V. Morozova, Zoya A. Mikhaylovskaya, Elena S. Buyanova, Sofia A. Petrova, Ksenia V. Arishina, Robert G. Zaharov

Abstract:

The present work is devoted to the investigation of two series of doped bismuth molybdates: Bi₂₆-₂ₓMn₂ₓMo₁₀O₆₉-d and Bi₂₆Mo₁₀-₂yMn₂yO₆₉-d. Complex oxides were synthesized by conventional solid state technology and by co-precipitation method. The products were identified by powder diffraction. The powders and ceramic samples were examined by means of densitometry, laser diffraction, and electron microscopic methods. Porosity of the ceramic materials was estimated using the hydrostatic method. The electrical conductivity measurements were carried out using impedance spectroscopy method.

Keywords: bismuth molybdate, columnar structures, impedance spectroscopy, oxygen ionic conductors

Procedia PDF Downloads 402