Search results for: synchrotron diffraction

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) and Fourier Transform Infrared Spectroscopy (FT-IR). 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: Masoume Ehsani, Ning Zhu, Huu Doan, Ali Lohi, Amira Abdelrasoul

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Membrane fouling poses severe challenges in membrane-based wastewater treatment applications. Ultrasound (US) has been considered an effective fouling remediation technique in filtration processes. Bubble cavitation in the liquid medium results from the alternating rarefaction and compression cycles during the US irradiation at sufficiently high acoustic pressure. Cavitation microbubbles generated under US irradiation can cause eddy current and turbulent flow within the medium by either oscillating or discharging energy to the system through microbubble explosion. Turbulent flow regime and shear forces created close to the membrane surface cause disturbing the cake layer and dislodging the foulants, which in turn improve the cleaning efficiency and filtration performance. Therefore, the number, size, velocity, and oscillation pattern of the microbubbles created in the liquid medium play a crucial role in foulant detachment and permeate flux recovery. The goal of the current study is to gain in depth understanding of the influence of the US power intensity and frequency on the microbubble dynamics and its characteristics generated under US irradiation. In comparison with other imaging techniques, the synchrotron in-line Phase Contrast Imaging technique at the Canadian Light Source (CLS) allows in-situ observation and real-time visualization of microbubble dynamics. At CLS biomedical imaging and therapy (BMIT) polychromatic beamline, the effective parameters were optimized to enhance the contrast gas/liquid interface for the accuracy of the qualitative and quantitative analysis of bubble cavitation within the system. With the high flux of photons and the high-speed camera, a typical high projection speed was achieved; and each projection of microbubbles in water was captured in 0.5 ms. ImageJ software was used for post-processing the raw images for the detailed quantitative analyses of microbubbles. The imaging has been performed under the US power intensity levels of 50 W, 60 W, and 100 W, in addition to the US frequency levels of 20 kHz, 28 kHz, and 40 kHz. For the duration of 2 seconds of imaging, the effect of the US power and frequency on the average number, size, and fraction of the area occupied by bubbles were analyzed. Microbubbles’ dynamics in terms of their velocity in water was also investigated. For the US power increase of 50 W to 100 W, the average bubble number and the average bubble diameter were increased from 746 to 880 and from 36.7 µm to 48.4 µm, respectively. In terms of the influence of US frequency, a fewer number of bubbles were created at 20 kHz (average of 176 bubbles rather than 808 bubbles at 40 kHz), while the average bubble size was significantly larger than that of 40 kHz (almost seven times). The majority of bubbles were captured close to the membrane surface in the filtration unit. According to the study observations, membrane cleaning efficiency is expected to be improved at higher US power and lower US frequency due to the higher energy release to the system by increasing the number of bubbles or growing their size during oscillation (optimum condition is expected to be at 20 kHz and 100 W).

Keywords: bubble dynamics, cavitational bubbles, membrane fouling, ultrasonic cleaning

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Authors: Raymond Dominic Uzoh

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Starch fillers were extracted from three plant sources namely amora tuber (a wild variety of Irish potato), sweet potato and yam starch and their particle size, pH, amylose, and amylopectin percentage decomposition determined accordingly by high performance liquid chromatography (HPLC). The starch was introduced into natural rubber in liquid phase (through gelatinization) by the latex compounding method and compounded according to standard method. The prepared starch/natural rubber composites was characterized by Instron Universal testing machine (UTM) for tensile mechanical properties. The composites was further characterized by x-ray diffraction and crosslink density analysis. The particle size determination showed that amora starch granules have the highest particle size (156 × 47 μm) followed by yam starch (155× 40 μm) and then the sweet potato starch (153 × 46 μm). The pH test also revealed that amora starch has a near neutral pH of 6.9, yam 6.8, and sweet potato 5.2 respectively. Amylose and amylopectin determination showed that yam starch has a higher percentage of amylose (29.68), followed by potato (22.34) and then amora starch with the lowest value (14.86) respectively. The tensile mechanical properties testing revealed that yam starch produced the best tensile mechanical properties followed by amora starch and then sweet potato starch. The structure, crystallinity/amorphous nature of the product composite was confirmed by x-ray diffraction, while the nature of crosslinking was confirmed by swelling test in toluene solvent using the Flory-Rehner approach. This research study has rendered a workable strategy for enhancing interfacial interaction between a hydrophilic filler (starch) and hydrophobic polymeric matrix (natural rubber) yielding moderately good tensile mechanical properties for further exploitation development and application in the rubber processing industry.

Keywords: natural rubber, fillers, starch, amylose, amylopectin, crosslink density

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Authors: Fatima Melit, Nedjemeddine Bounar

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Polycrystalline samples of Ce1-xMxO2-δ (x=0.1, 0.15, 0.2)(M=Gd, Y) were prepared by solid-state chemical reaction from mixtures of pre-dried oxides powders of CeO2, Gd2O3 and Y2O3 in the appropriate stoichiometric ratio to explore their use as solid electrolytes for intermediate temperature solid oxide fuel cells (IT-SOFCs). Their crystal structures and ionic conductivities were characterised by X-ray powder diffraction (XRD) and AC complex impedance spectroscopy (EIS). The XRD analyses confirm that all the resulting synthesised co-doped cerium oxide powders are single-phase and crystallise in the cubic structure system with the space group Fm3m. On the one hand, the lattice parameter (a ) of the phases increases with increasing Gd content; on the other hand, with increasing Y-substitution rate, the latter decreases. The results of complex impedance conductivity measurements have shown that doping has a remarkable effect on conductivity. The co-doped cerium phases showed significant ionic conductivity values, making these materials excellent candidates for solid oxide electrolytes at intermediate temperatures.

Keywords: electrolyte, Ceria, X-ray diffraction, EIS, SEM, SOFC

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Authors: Kalimi Trinadh, Corinne Nouveau, A. S. Khanna, Karanveer S. Aneja, K. Ram Mohan Rao

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This study concerns improving the corrosion resistance of low alloy steel after plasma nitriding performed at variable time and temperature. Nitriding carried out in the temperature range of 450-550ᵒC for a various time period of 1-8 hrs. at 500Pa in a glow discharge plasma of H₂ and N₂ (80:20). The substrate was kept biased negatively at 250V. Following nitriding the X-ray diffraction studies shown that the phases formed were mainly γ′ (Fe₄N) and ε (Fe₂₋₃N). The ε (Fe₂₋₃N) phase found to be the dominating phase. Cross sections of the samples under scanning electron microscope point analyses revealed the presence of nitrogen in the surface region. For the assessment of corrosion resistance property, potentiodynamic polarization tests were performed in 3.5% NaCl solution. It has been shown that the plasma nitriding significantly improved the corrosion resistance when compared to the as-received steel. Furthermore, it has also been found that nitriding for 6h has more corrosion resistance than nitriding for the 8h duration. The hardness of the nitrided samples was measured by Vicker’s microhardness tester. The hardness of the nitrided steel was found to be improved much above the hardness of the steel in the as-received condition. It was found to be around two-fold of the initial hardness.

Keywords: corrosion, steel, plasma nitriding, X-ray diffraction

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Authors: Meltem Nur Erdöl, Feyzanur Bayrak, Elif Emanetçi, Faik Nüzhet Oktar, Cevriye Kalkandelen, Oğuzhan Gündüz

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Nowadays, the bioceramic graft applications are very important due to the fact that especially European population is getting much older. Consequently, healing approaches for some health problems become more important in the near future. For instance, osteoporosis is one of the reasons for serious hip fractures. Beside these, the traffic accidents playing role increasing of various hip fractures and other bone fractures. Naturally all these are leading the importance developing new bioceramic graft materials. Hydroxyapatite (HA) is one of the leading bioceramics on the market. Beside the high biocompatibility HA bioceramics unfortunately are weak materials for loaded areas. For improvement mechanical properties of HA material, some oxides and metallic powders can be added. In this study, some rare earth oxides like hafnium (IV) oxide (HfO₂) and samarium (III) oxide (Sm₂O₃) are added to HA for improvement of their material characteristics. Thus, compression, microhardness and theoretical density tests are performed. X-ray diffraction patterns are also investigated corresponding x-ray diffraction equipment. At the end, studies of scanning electron microscope (SEM) and energy-dispersive x-ray spectroscopy (EDX) are completed. All values were compared with past BHA and various composites.

Keywords: biocomposite, hafnium oxide, hydroxyapatite, nanotechnology, samarium oxide

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Authors: Rafiuddin

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Solid polymer electrolytes have emerged as an area of interest in the field of solid state chemistry owing to their facile and cost-effective synthesis and number of applications in different areas of chemistry, extending over a wide range of temperatures. In the present work, polymer composite solid electrolyte comprising of Polyaniline (PANI) as polymer and potassium silver iodide (KAg4I5) using alumina (Al2O3) of different compositions having the formula (1-x) PANI- KAg4I5. x Al2O3 with x ranging from 0.0 to 0.5 was prepared by solid state reaction method. The structural elucidation and characterization was done by X- Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric- Differential Thermal Analysis (TG-DTA) and Impedance Spectroscopy. The thermal analysis shows a phase transition at 147°C attributed to β-α phase transition of AgI due to the disproportionation of KAg4I5 to AgI and KAg2I3 at temperatures higher than 36°C. The X Ray diffraction analysis also confirms the presence of both AgI and KAg2I3 in the samples. The conductivities recorded over a temperature range of 40-250° C lie in the range of 10-1 to 10-3 S cm-1. Maximum conductivity was seen in the compositon x = 0.4 i.e. 1.84 × 10-2 Scm-1 at 313 K and 1.38 × 10-1 Scm-1 at 513 K, with a minimum activation energy of 0.14 eV.

Keywords: polymer solid electrolytes, XRD, DTA, electrical conductivity, impedance spectroscopy

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Authors: Osama Saber

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Cyanate is one such anion which is produced during protein poisoning in the body and has been studied extensively in the field of biochemistry because of its toxicity. The present work aims at confinement and storage of cyanate in the nano scale. It was achieved through the intercalation of cyanate anions into nanolayerd structures of Ni-Al LDH. In addition, the effect of aging time on the intercalation of cyanate was clarified using X-ray diffraction and scanning electron microscopy. Furthermore, the effect of cations on the affinity towards the intercalation of cyanate anions inside LDH structure was studied by replacement of tetra-valent cations Ti4+ instead of the tri-vallent cations Al3+ during the preparation of LDH structure. X-ray diffraction patterns of the Ni-Ti LDH showed that the interlayer spacing was 0.73 nm. This spacing was smaller than that of Ni-Al LDH suggesting that the interlayered anions into Ni-Ti LDH are different from those into Ni-Al LDH. Thermal analyses (TG, DTG, and DTA) and Infra-red spectra revealed the presence of only cyanate anions into Ni-Ti LDH while, in the case of Ni-Al LDH, both cyanate and carbonate anions were observed. SEM images showed plate-like morphology for both Ni-Ti and Ni-Al LDHs although the shapes of their plates are not similar. Our results suggested that the LDH structures containing titanium cations have higher affinity for cyanate anions than those containing aluminum cations. Therefore, this choice for cyanate in the interlayered spacing widens the applicability to study the effect of the confinement on the toxicity of cyanate by bio researchers.

Keywords: nanolayered structures, Ni-Al LDH, Ni-Ti LDH, intercalation of cyanate anions, urea hydrolysis

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Authors: Gabriel K. Nzulu, Hans Högberg, Per Eklund, Lars Hultman, Martin Magnuson

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X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX) are applied to investigate the properties of rock samples from a drill hole from the Kubi Gold Project of the Asante Gold Corporation near Dunwka-on-Offin in the Central Region of Ghana. The distribution of these minerals in the rocks were observed in the drill hole sections. X-ray diffraction indicates that the samples contain garnet, pyrite, periclase, and quartz as the main indicator minerals. SEM revealed morphologies of these minerals. From EDX and XPS, Fe, Mg, Al, S, O, Hg, Ti, Mn, Na, Ag, Au, Cu, Si, and K are identified as the pathfinder elements in the area that either form alloys with gold or inherent elements in the sediments. This finding can be ascribed to primary geochemical distribution, which developed from crystallization of magma and hydrothermal liquids as well as the movement of metasomatic elements and the precipitous rate of chemical weathering of lateralization in secondary processes. The results indicate that Au mineralization in the Kubi Mine area is controlled by garnet, pyrite, goethite, and kaolinite that grades up to the surface (oxides) with hematite and limonite alterations.

Keywords: gold, minerals, pathfinder element, spectroscopy, X-ray

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Authors: Anil Kumar, Rajnish Kaur, Mateusz Czyzycki, Alessandro Migilori, Andreas Germanos Karydas, Sanjiv Puri

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The radiative decay of Li(i=1-3) sub-shell vacancies produced through photoionization results in production of the characteristic emission spectrum comprising several X-ray lines, whereas non-radiative vacancy decay results in Auger electron spectrum. Accurate reliable data on the Li(i=1-3) sub-shell X-ray production (XRP) cross sections is of considerable importance for investigation of atomic inner-shell ionization processes as well as for quantitative elemental analysis of different types of samples employing the energy dispersive X-ray fluorescence (EDXRF) analysis technique. At incident photon energies in vicinity of the absorption edge energies of an element, the many body effects including the electron correlation, core relaxation, inter-channel coupling and post-collision interactions become significant in the photoionization of atomic inner-shells. Further, in case of compounds, the characteristic emission spectrum of the specific element is expected to get influenced by the chemical environment (coordination number, oxidation state, nature of ligand/functional groups attached to central atom, etc.). These chemical effects on L X-ray fluorescence parameters have been investigated by performing the measurements at incident photon energies much higher than the Li(i=1-3) sub-shell absorption edge energies using EDXRF spectrometers. In the present work, the cross sections for production of the Lk(k= γ2,3, γ4) X-rays have been measured for some compounds of 66Dy, namely, Dy2O3, Dy2(CO3)3, Dy2(SO4)3.8H2O, DyI2 and Dy metal by tuning the incident photon energies few eV above the L1 absorption-edge energy in order to investigate the influence of chemical effects on these cross sections in presence of the many body effects which become significant at photon energies close to the absorption-edge energies. The present measurements have been performed under vacuum at the IAEA end-station of the X-ray fluorescence beam line (10.1L) of ELETTRA synchrotron radiation facility (Trieste, Italy) using self-supporting pressed pellet targets (1.3 cm diameter, nominal thicknesses ~ 176 mg/cm2) of 66Dy compounds (procured from Sigma Aldrich) and a metallic foil of 66Dy (nominal thickness ~ 3.9 mg/cm2, procured from Good Fellow, UK). The present measured cross sections have been compared with theoretical values calculated using the Dirac-Hartree-Slater(DHS) model based fluorescence and Coster-Kronig yields, Dirac-Fock(DF) model based X-ray emission rates and two sets of L1 sub-shell photoionization cross sections based on the non-relativistic Hartree-Fock-Slater(HFS) model and those deduced from the self-consistent Dirac-Hartree-Fock(DHF) model based total photoionization cross sections. The present measured XRP cross sections for 66Dy as well as for its compounds for the L2,3 and L4 X-rays, are found to be higher by ~14-36% than the two calculated set values. It is worth to be mentioned that L2,3 and L4 X-ray lines are originated by filling up of the L1 sub-shell vacancies by the outer sub-shell (N2,3 and O2,3) electrons which are much more sensitive to the chemical environment around the central atom. The present observed differences between measured and theoretical values are expected due to combined influence of the many-body effects and the chemical effects.

Keywords: chemical effects, L X-ray production cross sections, Many body effects, Synchrotron radiation

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Authors: P. M. Fonseca Alfonso, E. A. Murillo Ruiz, M. Diaz Lagos

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Understanding the physicochemical properties and mineralogy of fly ash from a particular source is essential for to protect the environment and considering its possible applications, specifically, in the production of geopolymeric materials that solidify/stabilize heavy metals ions. The results of the characterization of three fly ash samples are shown in this paper. The samples were produced in the TERMOPAIPA IV thermal power plant in the State of Boyaca, Colombia. The particle size distribution, chemical composition, mineralogy, and molecular structure of three samples were analyzed using laser diffraction, X-ray fluorescence, inductively coupled plasma mass spectrometry, X-ray diffraction, and infrared spectroscopy respectively. The particle size distribution of the three samples probably ranges from 0.128 to 211 μm. Approximately 59 elements have been identified in the three samples. It is noticeable that the ashes are made up of aluminum and silicon compounds. Besides, the iron phase in low content was also found. According to the results found in this study, the fly ash samples type F has a great potential to be used as raw material for the manufacture of geopolymers with potential use in the stabilization/solidification of heavy metals; mainly due to the presence of amorphous aluminosilicates typical of this type of ash, which react effectively with alkali-activator.

Keywords: fly ash, geopolymers, molecular structure, physicochemical properties.

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

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The 1:1 co-crystal 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, 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 co-crystal 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 R22(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 co-crystal I. Theoretical calculations are in good agreement with the experimental results. Solvent-free formation of this co-crystal I is confirmed by powder X-ray diffraction analysis.

Keywords: supramolecular co-crystal, 2-amino-4-chloro-6-methylpyrimidine, Harthree-Fock and DFT studies, spectroscopic analysis

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Authors: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: F. Laatar, S. Ktifa, H. Ezzaouia

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Plasma Enhanced Chemical Vapor Deposition (PECVD) method is used to deposit hydrogenated nanocrystalline silicon films (nc-Si: H) on Porous Anodic Alumina Films (PAF) on glass substrate at different deposition duration. Influence of the deposition time on the physical properties of nc-Si: H grown on PAF was investigated through an extensive correlation between micro-structural and optical properties of these films. In this paper, we present an extensive study of the morphological, structural and optical properties of these films by Atomic Force Microscopy (AFM), X-Ray Diffraction (XRD) techniques and a UV-Vis-NIR spectrometer. It was found that the changes in DT can modify the films thickness, the surface roughness and eventually improve the optical properties of the composite. Optical properties (optical thicknesses, refractive indexes (n), absorption coefficients (α), extinction coefficients (k), and the values of the optical transitions EG) of this kind of samples were obtained using the data of the transmittance T and reflectance R spectra’s recorded by the UV–Vis–NIR spectrometer. We used Cauchy and Wemple–DiDomenico models for the analysis of the dispersion of the refractive index and the determination of the optical properties of these films.

Keywords: hydragenated nanocrystalline silicon, plasma processing chemical vapor deposition, X-ray diffraction, optical properties

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Authors: Demet Tatar, Bahattin Düzgün

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In this study, we have newly developed titanium-tin oxide (TiSnO) thin films as the transparent conducting oxides materials by the spray pyrolysis technique. Tin oxide thin films doped with different Ti content were successfully grown by spray pyrolysis and they were characterized as a function of Ti content. The effect of Ti contents on the crystalline structure and optical properties of the as-deposited SnO2:Ti films was systematically investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), atomic force microscopy (AFM), UV-vis spectrometer and photoluminecenc spectrophotometer. The X-ray diffraction patterns taken at room temperature showed that the films are polycrystalline. The preferred directions of crystal growth appeared in the difractogram of SnO2: Ti (TiTO) films were correspond to the reflections from the (110), (200), (211) and (301) planes. The grain size varies from 21.8 to 27.8 nm for (110) preferred plane. SEM and AFM study reveals the surface of TiTO to be made of nanocrystalline particles. The highest visible transmittance (570 nm) of the deposited films is 80 % for 20 wt % titanium doped tin oxide films. The obtained results revealed that the structures and optical properties of the films were greatly affected by doping levels. These films are useful as conducting layers in electro chromic and photovoltaic devices.

Keywords: transparent conducting oxide, gas sensors, SnO2, Ti, optoelectronic, spray pyrolysis

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Authors: Rayan B. M. Ameen, Ian P. Jones, Yu Lung Chiu

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Single alpha-beta colony micro-pillars have been manufactured from a polycrystalline commercial Ti-6Al-4V sample using Focused Ion Beam (FIB). Each pillar contained two alpha lamellae separated by a thin fillet of beta phase. A nano-indenter was then used to conduct uniaxial micro-compression tests on Ti alloy single crystals, using a diamond flat tip as a compression platen. By controlling the crystal orientation along the micro-pillar using Electron back scattering diffraction (EBSD) different slip systems have been selectively activated. The advantage of the micro-compression method over conventional mechanical testing techniques is the ability to localize a single crystal volume which is characterizable after deformation. By matching the stress-strain relations resulting from micro-compression experiments to TEM (Transmission Electron Microscopy) studies of slip transmission mechanisms through the α-β interfaces, some proper constitutive material parameters such as the role of these interfaces in determining yield, strain-hardening behaviour, initial dislocation density and the critical resolved shear stress are suggested.

Keywords: α/β-Ti alloy, focused ion beam, micro-mechanical test, nano-indentation, transmission electron diffraction, plastic flow

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Authors: A. Srion, W. Thepsuwan, N. Monmaturapoj

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Two Lithium disilicate (LD) glass ceramics based on SiO2-Li2O-K2O-Al2O3 system were prepared through glass melting method and then fabricated into dental crowns via hot pressing at 850˚C and 900˚C in order to study the effect of the pressing temperatures on theirs phase formation and microstructure. The factor such as heat treatment temperature (as-cast glass, 600˚C and 700˚C) of the glass ceramics used to press was also investigated the effect of an initial microstructure before pressing. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to determine phase formation and microstructure of the samples, respectively. X-ray diffraction result shows that the main crystalline structure was Li2Si2O5 by having Li3PO4, Li0.6Al0.6Si2O6, Li2SiO3, Ca5 (PO4)3F, SiO2 as minor phases. Glass compositions with different heat treatment temperatures exhibited a difference phase formation but have less effect during pressing. Scanning electron microscopy analysis showed microstructure of lath-like of Li2Si2O5 in all glasses. With increasing the initial heat treatment temperature, the longer the lath-like crystals of lithium disilicate were increased especially when using glass heat treatment at 700˚C followed by pressing at 900˚C. This could be suggested that LD1 heat treatment at 700˚C which pressing at 900˚C presented the best formation by hot pressing and compiled microstructure.

Keywords: lithium disilicate, hot pressing, dental crown, microstructure

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Authors: I. Shuro

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The crystal structure of Tin Sulfide prepared by certain chemical methods is investigated using High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), and X-ray diffraction (XRD) methods. An anomalous HRTEM Fast Fourier Transform (FFT) exhibited a central scatter of diffraction spots, which is surrounded by secondary clusters of spots arranged in a hexagonal pattern around the central cluster was observed. FFT analysis has revealed a long lattice parameter and mostly viewed along a hexagonal axis where there many columns of atoms slightly displaced from one another. This FFT analysis has revealed that the metal sulfide has a long-range order interwoven chain of atoms in its crystal structure. The observed crystalline structure is inconsistent with commonly observed FFT patterns of chemically synthesized Tin Sulfide nanocrystals and thin films. SEM analysis showed the morphology of a myriad of multi-shaped crystals ranging from hexagonal, cubic, and spherical micro to nanostructured crystals. This study also investigates the presence of quasi-crystals as reflected by the presence of mixed local symmetries.

Keywords: fast fourier transform, high resolution transmission electron microscopy, tin sulfide, crystalline structure

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Authors: Babak Sadeghi, Parisa Ghayomipour

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ZnO/Ag nanocomposites coated with polyvinyl chloride (PVC) were prepared by chemical reduction method, for anti-infection biomaterial application. There is a growing interest in attempts in using biomolecular as the templates to grow inorganic nanocomposites in controlled morphology and structure. By optimizing the experiment conditions, we successfully fabricated high yield of ZnO/Ag nanocomposite with full coverage of high-density polyvinyl chloride (PVC) coating. More importantly, ZnO/Ag nanocomposites were shown to significantly inhibit the growth of S. aureus in solution. It was further shown that ZnO/Ag nanocomposites induced thiol depletion that caused death of S. aureus. The coatings were fully characterized using techniques such as scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). Most importantly, compared to uncoated metals, the coatings on PVC promoted healthy antibacterial activity. Importantly, compared to ZnO-Ag -uncoated PVC, the ZnO/Ag nanocomposites coated was approximately triplet more effective in preventing bacteria attachment. The result of Thermal Gravimetric Analysis (TGA) indicates that, the ZnO/Ag nanocomposites are chemically stable in the temperature range from 50 to 900 ºC. This result, for the first time, demonstrates the potential of using ZnO/Ag nanocomposites as a coating material for numerous anti-bacterial applications.

Keywords: nanocomposites, antibacterial activity, scanning electron microscopy (SEM), x-ray diffraction (XRD)

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Authors: SeyedMohammad Hosseini, Amirhossein Moghanian

Abstract:

The main purpose of this research was to design a biomimetic system by freeze-drying method for evaluating the effect of adding 5 and 10 mol. % of zinc (Zn)in 58S bioactive glass and gelatin (5ZnBG/G and 10ZnBG/G) in terms of structural and biological changes. The structural analyses of samples were performed by X-Ray Diffraction (XRD), scanning electron microscopy (SEM), and Fourier-transform infrared spectroscopy (FTIR). Also, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazoliumbromide(MTT) and alkaline phosphate (ALP) activity test were carried out for investigation of MC3T3-E1cell behaviors. The SEM results demonstrated the spherical shape of the formed hydroxyapatite (HA) phases, and also HA characteristic peaks were detected by X-ray diffraction spectroscopy (XRD)after 3 days of immersion in the simulated body fluid (SBF) solution. Meanwhile, FTIR spectra proved that the intensity of P–O peaks for 5ZnBG/G was more than 10ZnBG/G and control samples. Moreover, the results of alkaline phosphatase activity (ALP) test illustrated that the optimal amount of Zn (5ZnBG/G) caused a considerable enhancement in bone cell growth. Taken together, the scaffold with 5 mol.% Zn was introduced as an optimal sample because of its higher biocompatibility, in vitro bioactivity, and growth of MC3T3-E1cellsin in comparison with other samples in bone tissue engineering.

Keywords: scaffold, gelatin, modified bioactive glass, alp, bone tissue engineering

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Authors: Ismail Al-Yahmadi, Abbasher Gismelseed, Fatma Al-Mammari, Ahmed Al-Rawas, Ali Yousif, Imaddin Al-Omari, Hisham Widatallah, Mohamed Elzain

Abstract:

The influence of Fe-doping on the structural, magnetic and magnetocaloric properties of Nd₀.₆Sr₀.₄FeₓMn₁₋ₓO₃ (0≤ x ≤0.5) were investigated. The samples were synthesized by auto-combustion Sol-Gel method. The phase purity, crystallinity, and the structural properties for all prepared samples were examined by X-ray diffraction. XRD refinement indicates that the samples are crystallized in the orthorhombic single-phase with Pnma space group. Temperature dependence of magnetization measurements under a magnetic applied field of 0.02 T reveals that the samples with (x=0.0, 0.1, 0.2 and 0.3) exhibit a paramagnetic (PM) to ferromagnetic (FM) transition with decreasing temperature. The Curie temperature decreased with increasing Fe content from 256 K for x =0.0 to 80 K for x =0.3 due to increasing of antiferromagnetic superexchange (SE) interaction coupling. Moreover, the magnetization as a function of applied magnetic field (M-H) curves was measured at 2 K, and 300 K. the results of such measurements confirm the temperature dependence of magnetization measurements. The magnetic entropy change|∆SM | was evaluated using Maxwell's relation. The maximum values of the magnetic entropy change |-∆SMax |for x=0.0, 0.1, 0.2, 0.3 are found to be 15.35, 5.13, 3.36, 1.08 J/kg.K for an applied magnetic field of 9 T. Our result on magnetocaloric properties suggests that the parent sample Nd₀.₆Sr₀.₄MnO₃ could be a good refrigerant for low-temperature magnetic refrigeration.

Keywords: manganite perovskite, magnetocaloric effect, X-ray diffraction, relative cooling power

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Authors: Morteza Hadi

Abstract:

This research investigates the potential enhancement of the rollability of Cu-Ge-Ni alloy through the mitigation of microstructural and compositional inhomogeneities via two distinct heat treatment methods: homogenization and solution treatment. To achieve this objective, the alloy with the desired composition was fabricated using a vacuum arc remelting furnace (VAR), followed by sample preparation for microstructural, compositional, and heat treatment analyses at varying temperatures and durations. Characterization was conducted employing optical and scanning electron microscopy (SEM), X-ray diffraction (XRD), and Vickers hardness testing. The results obtained indicate that a minimum duration of 10 hours is necessary for adequate homogenization of the alloy at 750°C. This heat treatment effectively removes coarse dendrites from the casting microstructure and significantly reduces elemental separations. However, despite these improvements, the presence of a second phase with markedly different hardness from the matrix results in poor rolling ability for the alloy. The optimal time for solution treatment at various temperatures was determined, with the most effective cycle identified as 750°C for 2 hours, followed by rapid quenching in water. This process induces the formation of a single-phase microstructure and complete elimination of the second  phase, as confirmed by X-ray diffraction analysis. Results demonstrate a reduction in hardness by 30 Vickers, and the elimination of microstructural unevenness enables successful thickness reduction by up to 50% through rolling without encountering cracking.

Keywords: Cu-Ge-Ni alloy, homogenization. solution treatment, rollability

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Authors: Ayed S. Al-Shihri, Abul Kalam, Abdullah G. Al-Sehemi, Gaohui Du, Tokeer Ahmad, Ahmad Irfan

Abstract:

We report here the synthesis of nickel oxide (NiO) nanoparticles by microwave-assisted method, using a common precipitating agent followed by calcination in air at 400°C. The effect of the microwave and pH on the crystallite size, morphology, structure, energy band gap and surface area of NiO have been investigated by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), ultraviolet visible spectroscopy (UV-vis) and BET surface area studies. X-ray diffraction studies showed the formation of monophasic and highly crystalline cubic NiO. TEM analysis led to decrease the average grain size of NiO nanoparticles from 16.5 nm to 14 nm on increasing the amount of NaOH. FTIR studies also confirm the formation of NiO nanoparticles. It was observed that on increasing the volume of NaOH, the optical band gap energy (2.85 eV to 2.95 eV) and specific surface area (33.1 to 39.8 m2/g) increases, however the average particles size decreases (16.5 nm to 14 nm). This method may be extended to large scale synthesis of other metal oxides nanoparticles and the present study could be used for the potential applications in water treatment and many other fields.

Keywords: BET surface area analysis, electron microscopy, optical properties, X-ray techniques

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Authors: Christina Roman, Deepak Koirala, Joseph A. Piccirilli

Abstract:

Phage displaying synthetic Fab libraries have been used to obtain Fabs that bind to specific RNA targets with high affinity and specificity. These Fabs have been demonstrated to facilitate RNA crystallization. However, the antibody framework used in the construction of these phage display libraries contains numerous bulky, flexible, and charged residues, which facilitate solubility and hinder aggregation. These residues can interfere with crystallization due to the entropic cost associated with burying them within crystal contacts. To systematically reduce the surface entropy of the Fabs and improve their crystallization properties, a protein engineering strategy termed surface entropy reduction (SER) is being applied to the Fab framework. In this approach, high entropy residues are mutated to smaller ones such as alanine or serine. Focusing initially on Fab BL3-6, which binds an RNA AAACA pentaloop with 20nM affinity, the SER P server (http://services.mbi.ucla.edu/SER/) was used and analysis was performed on existing RNA-Fab BL3-6 co-crystal structures. From this analysis twelve surface entropy reduced mutants were designed. These SER mutants were expressed and are now being measured for their crystallization and diffraction performance with various RNA targets. So far, one mutant has generated 3.02 angstrom diffraction with the yjdF riboswitch RNA. Ultimately, the most productive mutations will be combined into a new Fab framework to be used in a optimized phage displayed Fab library.

Keywords: antibody fragment, crystallography, RNA, surface entropy reduction

Procedia PDF Downloads 153

Authors: Manel Bouloudenine, Karima Djeddou, Hadjer Ben Manser, Hana Soualah Alila, Mohmed Bououdina

Abstract:

This survey research involves the elaboration and characterization of silver nanoparticles for therapeutic and environmental applications. The silver nanoparticles "Ag NPs" were synthesized by reducing AgNO3 with microwaves. The characterization of nanoparticles was done by using Transmission Electron Microscopy " TEM ", Energy Dispersive Spectroscopy "EDS", Selected Area Electron Diffraction "SEAD", UV-Visible Spectroscopy and Dynamic Light Scattering "DLS". Transmission Electron Microscopy and Electron Diffraction have confirmed the nanoscale, the shape, and the crystalline quality of as synthesized silver nanoparticles. Elementary analysis has proved the purity of Ag NPs and the presence of the Surface Plasmon Resonance phenomenon "SPR". A strong absorption shift was observed in the visible range of the UV-visible spectrum of as synthesized Ag NPs, which indicates the presence of metallic silver. When the strong absorption in the ultraviolet range of the spectrum has revealed the presence of ionic Ag NPs ionic Ag aggregates species. The autocorrelation function measured by the Dynamic Light Scattering has shown a strong monodispersed character of Ag NPs, which is indicated by the presence of a single size population, with a minima and a maxima laying between 40 and 111 nm. Related to other research, our results confirm the performance properties of as synthesized Ag NPs, which allows them to be performing in many technological applications, including therapeutic and environmental ones.

Keywords: silvers nanoparticles, microwaves, EDS, TEM

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Authors: Andrey V. Malyshev, Anna B. Petrova, Anatoly P. Surzhikov

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The article presents the results of the influence of diamagnetic additives on the defects level of ferrite ceramics. For this purpose, we use a previously developed method based on the mathematical analysis of experimental temperature dependences of the initial permeability. A phenomenological expression for the description of such dependence was suggested and an interpretation of its main parameters was given. It was shown, that the main criterion of the integral defects level of ferrite ceramics is the relation of two parameters correlating with elastic stress value in a material. Model samples containing a controlled number of intergranular phase inclusions served to prove the validity of the proposed method, as well as to assess its sensitivity in comparison with the traditional XRD (X-ray diffraction) analysis. The broadening data of diffraction reflexes of model samples have served for such comparison. The defects level data obtained by the proposed method are in good agreement with the X-ray data. The method showed high sensitivity. Therefore, the legitimacy of the selection relationship β/α parameters of phenomenological expression as a characteristic of the elastic state of the ferrite ceramics confirmed. In addition, the obtained data can be used in the detection of non-magnetic phases and testing the optimal sintering production technology of soft magnetic ferrites.

Keywords: cure point, initial permeability, integral defects level, homogeneity

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Authors: Mohieldin Elmashad, Salwa Yassin

Abstract:

Expansive soils regarded as one of the most problematic unsaturated formations in the Egyptian arid zones and present a great challenge in civil engineering, in general, and geotechnical engineering, in particular. Severe geotechnical complications and consequent structural damages have been arising due to an excessive and differential volumetric change upon wetting and change in water content. Different studies have been carried out concerning the swelling performance of the expansive soils using different additives including phospho-gypsum as an industrial waste product. However, this paper describes the results of a comprehensive testing programme that was carried out to investigate the effect of phospho-gypsum (PG) and sodium chloride (NaCl), as an additive mixture, on the swelling performance of constituent samples of swelling soils. The constituent samples comprise commercial bentonite collected from a natural site, mixed with different percentages of PG-NaCl mixture. The testing programme had been scoped to cover the physical and chemical properties of the constituent samples. In addition, a mineralogical study using x-ray diffraction (XRD) was performed on the collected bentonite and the mixed bentonite with PG-NaCl mixture samples. The obtained results of this study showed significant improvement in the swelling performance of the tested samples with the increase of the proposed PG-NaCl mixture content.

Keywords: expansive soils, industrial waste, mineralogical study, swelling performance, X-ray diffraction

Procedia PDF Downloads 243

Authors: Evrim Colak, Andriy E. Serebryannikov, Thore Magath, Ekmel Ozbay

Abstract:

Single beam deflection and unidirectional transmission are examined for oblique incidence in a Photonic Crystal (PC) structure which employs defect layer instead of surface corrugations at the interfaces. In all of the studied cases, the defect layer is placed such that the symmetry is broken. Two types of deflection are observed depending on whether the zeroth order is coupled or not. These two scenarios can be distinguished from each other by considering the simulated field distribution in PC. In the first deflection type, Floquet-Bloch mode enables zeroth order coupling. The energy of the zeroth order is redistributed between the diffraction orders at the defect layer, providing deflection. In the second type, when zeroth order is not coupled, strong diffractions cause blazing and the evanescent waves deliver energy to higher order diffraction modes. Simulated isofrequency contours can be utilized to estimate the coupling behavior. The defect layer is placed at varying rows, preserving the asymmetry of PC while evancescent waves can still couple to higher order modes. Even for deeply buried defect layer, asymmetric transmission and beam deflection are still encountered when the zeroth order is not coupled. We assume ε=11.4 (refractive index close to that of GaAs and Si) for the PC rods. A possible operation wavelength can be within microwave and infrared range. Since the suggested material is low loss, the structure can be scaled down to operate higher frequencies. Thus, a sample operation wavelength is selected as 1.5μm. Although the structure employs no surface corrugations transmission value T≈0.97 can be achieved by means of diffraction order m=-1. Moreover, utilizing an extra line defect, T value can be increased upto 0.99, under oblique incidence even if the line defect layer is deeply embedded in the photonic crystal. The latter configuration can be used to obtain deflection in one frequency range and can also be utilized for the realization of another functionality like defect-mode wave guiding in another frequency range but still using the same structure.

Keywords: asymmetric transmission, beam deflection, blazing, bi-directional splitting, defect layer, dual beam splitting, Floquet-Bloch modes, isofrequency contours, line defect, oblique incidence, photonic crystal, unidirectionality

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Authors: Srutirekha Giri, Manoranjan Sahoo, Anuradha Das, Pravanjan Mallick, Biswajit Mallick

Abstract:

Ion Beam (IB) technique is a very powerful experimental technique for both material synthesis and material modifications. In this work, 3MeV proton beam was generated using the 3MV Tandem machine of the Institute of Physics, Bhubaneswar and extracted into air for the irradiation-induced modification purpose[1]. The polymeric material can be modeled for a three-phase system viz. crystalline(I), amorphous(II) and mesomorphic(III). So far, our knowledge is concerned. There are only few techniques reported for the synthesis of this third-phase(III) of polymer. The IB induced technique is one of them and has been reported very recently [2-4]. It was observed that by irradiating polyethylene terephthalate (PET) fiber at very low proton fluence, 10¹⁰ - 10¹² p/s, possess 2D mesophase structure. This was confirmed using X-ray diffraction technique. A low-intensity broad peak was observed at small angle of about 2θ =6º, when the fiber axis was mounted parallel to the X-ray direction. Such peak vanished in the diffraction spectrum when the fiber axis was mounted perpendicular to the beam direction. The appearance of this extra peak in a particular orientation confirms that the phase is 2-dimensionally oriented (mesophase). It is well known that the mesophase is a 2-dimensionally ordered structure but 3-dimensionally disordered. Again, the crystallite of the mesophase peak particle was measured about 3nm. The MeV proton-induced 2D mesophase patterning of nanocrystallites (3nm) of PET due to irradiation was observed within the above low fluence range and failed in high proton fluence. This is mainly due to the breaking of crystallites, radiation-induced thermal degradation, etc.

Keywords: Ion irradiation, mesophase, nanocrystallites, polymer

Procedia PDF Downloads 170