Search results for: X-ray diffraction technique

Authors: Kanta Maan Sangwan, Neetu Ahlawat, Rajender Singh Kundu

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BaZrTiO3 ceramics having high dielectric constant and low dielectric loss are interesting material for being used as commercial capacitor applications. BZT (BaZrTiO3) has attracted attentions for their many applications for the microwave technology as the doping of Zr4+ on Ti4+ has advantage to the stability of the system. In the present work, co-doping of Zr and V with BaTiO3 ceramics was synthesized by the conventional solid state reaction technique and sintered at 1200 K for 6 hours, and their structural and ferroelectric properties were studied. The XRD (x-ray diffraction) pattern of BZT (BaZrTiO3) ceramics shows that the crystalline sample is single phase tetragonal structure with P4mm space group. The result revealed that Zr ion enters the unit cell maintaining the perovskite structure of BZT ceramics and the impedance spectroscopy of the sample performed in selected frequency and temperature range.

Keywords: ferroelectric, impedance spectroscopy, space group, tetragonal

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Authors: G. Çelik Gül, F. Kurtuluş

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

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

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Authors: Mohammad Arifin, Huda Abdullah, Norshafadzila Mohammad Naim

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The fabricated PANI-(SnO₂, ZnO)/rGO nanocomposite thin films for the E. coli bacteria sensor were investigated. The nanocomposite thin films were prepared by the sol-gel method and deposited on the glass substrate using the spin-coating technique. The internal structure and surface morphology of the thin films have been analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and atomic force microscopy (AFM). The optical properties of the films were investigated by UV-Vis spectroscopy, Raman spectroscopy, and Fourier transform infrared spectroscopy (FTIR). The sensitivity performance was identified by measuring the changing conductivity before and after the incubation of E. coli bacteria using current-voltage (I-V) and cyclic voltammetry (C-V) measurements.

Keywords: PANI-(SnO₂, ZnO)/rGO, nanocomposite, bacteria sensor, thin films

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Authors: Sanusi Abdullahi, Musa Momoh, Abubakar Umar Moreh, Aminu Muhammad Bayawa, Olubunmi Popoola

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Kesterite-type Cu₂ZnSnS₄ (CZTS) thin films were deposited on corning glass from a single quaternary target. In this study, we investigated the growth mechanism and the influence of thin film thickness on the structural and compositional properties of CZTS films. All the four samples (as-deposited inclusive) show peaks corresponding to kesterite-type structure. The diffraction peaks of (112) are sharp and the small characteristics peaks of the kesterite structure such as (220)/ (204) and (312)/ (116) are also clearly observed in X-ray diffraction pattern. These results indicate that the quaternary CZTS would be a potential candidate for solar cell applications.

Keywords: RF sputtering, Cu2ZnSnS4 thin film, annealing, growth mechanism, annealing, growth mechanism, renewable energy

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Authors: M. P. Joshi, F. Deganello, L. F. Liotta, V. La Parola, G. Pantaleo

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For the first time, commercial iron nitrate was replaced by rust wastes, as a source of Iron for the preparation of LaFeO₃ powders by solution combustion synthesis (SCS). A detailed comparison with a reference powder obtained by SCS, starting from a commercial iron nitrate, was also performed. Several techniques such as X-ray diffraction combined with Rietveld refinement, mass plasma atomic emission spectroscopy, nitrogen adsorption measurements, temperature programmed reduction, X-ray photoelectron spectroscopy, Fourier transform analysis and scanning electron microscopy were used for the characterization of the rust wastes as well as of the perovskite powders. The performance of this ecofriendly material was evaluated by testing the activity and selectivity in the propylene oxidation, in order to use it for the benefit of the environment. Characterization and performance results clearly evidenced limitations and peculiarities of this new approach.

Keywords: perovskite type catalysts, solution combustion synthesis, X-ray diffraction, rust wastes

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Authors: Ibrahim Dauda Muhammad, Mokhtar Awang

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To synthesize a specific phase of zirconia (ZrO₂) nanotubes, zirconium (Zr) foil was subjected to the anodization process in a fluorine-containing electrochemical bath for a fixed duration. The resulting zirconia nanotubes (ZNTs) were then characterized using various techniques, including UV-vis spectroscopy, Fourier-transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). The XRD diffraction pattern confirmed that the ZNTs were crystalline, with a predominant texture along the [111] direction, indicating that the majority of the phase was cubic. TEM images revealed that most of the nanotubes were vertically aligned and self-organized, with diameters ranging from 32.9 to 38.8 nm and wall thicknesses between 3.0 and 7.3 nm. Additionally, the synthesized ZNTs had a length-to-width ratio of 235, which closely matches the ratio of 240 observed in another study where anodization was not used. This study demonstrates that a specific phase of zirconia nanotube can be successfully synthesized, with promising potential applications in catalysis and other areas.

Keywords: zirconia nanotubes, anodization, characterization, cubic phase

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Authors: M. Sari Yilmaz, N. Karamahmut Mermer

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Coal fly ash is formed as a solid waste product from the combustion of coal in coal fired power stations. Huge amounts of fly ash are produced globally every year and are predicted to increase. Nowadays, less than half of the fly ash is used as a raw material for cement manufacturing, construction and the rest of it is disposed as a waste causing yet another environmental concern. For this reason, the recycling of this kind of slurries into useful materials is quite important in terms of economical and environmental aspects. The purpose of this study is to evaluate the Orhaneli and Tuncbilek coal fly ashes for utilization in some industrial applications. Therefore the mineralogical and chemical compositions of these fly ashes were analyzed by X-ray fluorescence (XRF) spectroscopy and X-ray diffraction (XRD). The silicon (Si) and aluminum (Al) in the fly ashes were activated by alkali fusion technique with sodium hydroxide. The obtained extracts were analyzed for Si and Al content by inductively coupled plasma optical emission spectrometry (ICP-OES).

Keywords: extraction, fly ash, fusion, XRD

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Authors: Sanghamitra Acharya, Suwarna Datar

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Extensive use of digital and smart communication createsprolong expose of unwanted electromagnetic (EM) radiations. This harmful radiation creates not only malfunctioning of nearby electronic gadgets but also severely affects a human being. So, a suitable microwave absorbing material (MAM) becomes a necessary urge in the field of stealth and radar technology. Initially, Aluminum based hexa ferrite was prepared by sol-gel technique and for carbon derived composite was prepared by the simple one port chemical reduction method. Finally, composite films of Poly (Vinylidene) Fluoride (PVDF) are prepared by simple gel casting technique. Present work demands that aluminum-based hexaferrite phase conjugated with graphene in PVDF matrix becomes a suitable candidate both in commercially important X and Ku band. The structural and morphological nature was characterized by X-Ray diffraction (XRD), Field emission-scanning electron microscope (FESEM) and Raman spectra which conforms that 30-40 nm particles are well decorated over graphene sheet. Magnetic force microscopy (MFM) and conducting force microscopy (CFM) study further conforms the magnetic and conducting nature of composite. Finally, shielding effectiveness (SE) of the composite film was studied by using Vector network analyzer (VNA) both in X band and Ku band frequency range and found to be more than 30 dB and 40 dB, respectively. As prepared composite films are excellent microwave absorbers.

Keywords: carbon nanocomposite, microwave absorbing material, electromagnetic shielding, hexaferrite

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Authors: Himanshu Pavagadhi, Maunik Jani, S. M. Vyas, Jaymin Ray, Vimal Patel, Piyush Patel, Jignesh P. Raval

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The preparation of pure and Sn-doped cadmium sulfide (CdS) pellets was carried out using a compression technique with a pelletizer. The energy dispersive X-ray (EDX) analysis is used to confirm the purity and stoichiometric ratio of Cd, S, and Sn in the prepared pellets. The surface morphology of the pellets was examined using a scanning electron microscope. Both XRD and Raman scattering spectrum analysis confirmed the doping effect in the CdS pellets. The X-ray diffraction (XRD) analysis confirmed the hexagonal structure and revealed that the grain size decreases with increasing Sn dopant concentration in the parent CdS pellet. The optical properties of the pellets were evaluated by measuring diffuse reflectance using a UV-vis spectrophotometer. The analysis indicated that as the Sn concentration increases in the parent CdS pellet, the optical band gap decreases. This implies that the optical properties of the CdS material are also affected by the Sn dopant.

Keywords: CdS, Sn dopant, UV-Spetrophotometer, XRD

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

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

Keywords: laser cladding, residual stress, neutron diffraction, HAZ

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Authors: Binyamien Ibrahim Rasoul

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Controlled burning of rice husk can produce amorphous rice husk ash (RHA) with high silica content which can significantly enhance the properties of concrete. This study has been undertaken to investigate the relationship between the incineration temperatures and time to produce RHA with ultimate reactivity. The rice husk samples were incinerated in an electrical muffle furnace at 350°C, 400°C, 425°C 450°C, 475°C, and 500°C for 60 and 90 minutes, respectively. The silica structure in the Rice Husk Ash (RHA) was determined using X-Ray diffraction analysis, while chemical properties obtained using X-Ray Fluorescence. The results show that RHA appeared to be the totally amorphous when the husk incineration up to 425°C for 60 and even at 90 minutes. However, with increased temperature to 450°C, 475°C and 500°C, traces of crystalline silica (quartz) were detected. However, cannot be taken into account as it does not affect on the ash structure. In conclusion, the result gives an idea of the temperature and the time required to produce ash from rice husk with totally amorphous form.

Keywords: rice husk ash, silica, compressive strength, tensile strength, X-Ray diffraction, X-R florescence, pozzolanic activity

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Authors: Tatiana S. Ogneva

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Aluminum and nickel-based intermetallic compounds have attracted the attention of scientific community as promising materials for heat-resistant and wear-resistant coatings in such manufacturing areas as microelectronics, aircraft and rocket building and chemical industries. Magnetron sputtering makes possible to coat materials without formation of liquid phase and improves the mechanical and functional properties of nickel aluminides due to the possibility of nanoscale structure formation. The purpose of the study is the investigation of structure and properties of intermetallic coatings produced by magnetron sputtering technique. The feature of this work is the using of composite targets for sputtering, which were consisted of two semicircular sectors of cp-Ni and cp-Al. Plates of alumina, silicon, titanium and steel alloys were used as substrates. To estimate sputtering conditions on structure of intermetallic coatings, a series of samples were produced and studied in detail using scanning and transition electron microcopy and X-Ray diffraction. Besides, nanohardness and scratching tests were carried out. The varying parameters were the distance from the substrate to the target, the duration and the power of the sputtering. The thickness of the obtained intermetallic coatings varied from 0.05 to 0.5 mm depending on the sputtering conditions. The X-ray diffraction data indicated that the formation of intermetallic compounds occurred after sputtering without additional heat treatment. Sputtering at a distance not closer than 120 mm led to the formation of NiAl phase. Increase in the power of magnetron from 300 to 900 W promoted the increase of heterogeneity of the phase composition and the appearance of intermetallic phases NiAl, Ni₂Al₃, NiAl₃, and Al under the aluminum side, and NiAl, Ni₃Al, and Ni under the nickel side of the target. A similar trend is observed with increasing the distance of sputtering from 100 to 60 mm. The change in the phase composition correlates with the changing of the atomic composition of the coatings. Scanning electron microscopy revealed that the coatings have a nanoscale grain structure. In this case, the substrate material and the distance from the substrate to the magnetron have a significant effect on the structure formation process. The size of nanograins differs from 10 to 83 nm and depends not only on the sputtering modes but also on material of a substrate. Nanostructure of the material influences the level of mechanical properties. The highest level of nanohardness of the coatings deposited during 30 minutes on metallic substrates at a distance of 100 mm reached 12 GPa. It was shown that nanohardness depends on the grain size of the intermetallic compound. Scratching tests of the coatings showed a high level of adhesion of the coating to substrate without any delamination and cracking. The results of the study showed that magnetron sputtering of composite targets consisting of nickel and aluminum semicircles makes it possible to form intermetallic coatings with good mechanical properties directly in the process of sputtering without additional heat treatment.

Keywords: intermetallic coatings, magnetron sputtering, mechanical properties, structure

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy (FTIR), micro-Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence Spectroscopy (PL) and Field Effect Scanning electron microscopy (FESEM)

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Authors: María Magdalena Méndez-González, Miguel García Rocha, Carlos Manuel Yermo De la Cruz

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Calcium phosphate (Ca5(PO4)3(X)) is widely used in orthopedic applications and is widely used as powder and granules. However, their presence in bone is in the form of nanometric needles 60 nm in length with a non-stoichiometric phase of apatite contains CO3-2, Na+, OH-, F-, and other ions in a matrix of collagen fibers. The crystal size, morphology control and interaction with cells are essential for the development of nanotechnology. The structural results of calcium phosphate, synthesized by chemical precipitation with crystal size of 22.85 nm are presented in this paper. The calcium phosphate powders were analyzed by X-ray diffraction, energy dispersive spectroscopy (EDS), infrared spectroscopy and FT-IR transmission electron microscopy. Network parameters, atomic positions, the indexing of the planes and the calculation of FWHM (full width at half maximum) were obtained. The crystal size was also calculated using the Scherer equation d (hkl) = cλ/βcosѲ. Where c is a constant related to the shape of the crystal, the wavelength of the radiation used for a copper anode is 1.54060Å, Ѳ is the Bragg diffraction angle, and β is the width average peak height of greater intensity. Diffraction pattern corresponding to the calcium phosphate called hydroxyapatite phase of a hexagonal crystal system was obtained. It belongs to the space group P63m with lattice parameters a = 9.4394 Å and c = 6.8861 Å. The most intense peak is obtained 2Ѳ = 31.55 (FWHM = 0.4798), with a preferred orientation in 121. The intensity difference between the experimental data and the calculated values is attributable to the temperature at which the sintering was performed. The intensity of the highest peak is at angle 2Ѳ = 32.11. The structure of calcium phosphate obtained was a hexagonal configuration. The intensity changes in the peaks of the diffraction pattern, in the lattice parameters at the corners, indicating the possible presence of a dopant. That each calcium atom is surrounded by a tetrahedron of oxygen and hydrogen was observed by infrared spectra. The unit cell pattern corresponds to hydroxyapatite and transmission electron microscopic crystal morphology corresponding to the hexagonal phase with a preferential growth along the c-plane was obtained.

Keywords: structure, nanoparticles, calcium phosphate, metallurgical and materials engineering

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Authors: Askar Kilmametov, Julia Ivanisenko, Boris Straumal, Horst Hahn

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The high-pressure α- to ω-phase transition was discovered in elemental Ti and Zr fifty years ago using static high pressure and then observed to appear between 2 and 12 GPa at room temperature, depending on the experimental technique, the pressure environment, and the sample purity. The fact that ω-phase is retained in a metastable state in ambient condition after the removal of the pressure has been used to check the changes in magnetic and superconductive behavior, electron band structure and mechanical properties. However, the fundamental knowledge on a combination of both mechanical treatment and high applied pressure treatments for ω-phase formation in Ti alloys is currently lacking and has to be studied in relation to improved mechanical properties of bulk nanostructured states. In the present study, nanostructured (α+β) Ti alloys containing β-stabilizing elements such as Co, Fe, Cr, Nb were performed by severe plastic deformation, namely high pressure torsion (HPT) technique. HPT-induced α- to ω-phase transformation was revealed in dependence on applied pressure and shear strains by means of X-ray diffraction, transmission electron microscopy, and differential scanning calorimetry. The transformation kinetics was compared with the kinetics of pressure-induced transition. Orientation relationship between α-, β- and ω-phases was taken into consideration and analyzed according to theoretical calculation proposed earlier. The influence of initial state before HPT appeared to be considerable for subsequent α- to ω-phase transition. Thermal stability of the HPT-induced ω-phase was discussed as well in the frame of mechanical behavior of Ti and Ti-based alloys produced by shear deformation under high applied pressure.

Keywords: bulk nanostructured materials, high pressure phase transitions, severe plastic deformation, titanium alloys

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Authors: Ravi Prakash

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The effects of Zr addition on kinetics and hydrogen absorption characteristics of BCC alloy 52Ti-12V-36Cr doped with x wt% of Zr (x = 0, 4, 8 & 12) was investigated. The samples have been characterized by X-ray diffraction, and activation study were made at four different temperatures- 100 oC, 200 oC, 300 oC and 400 oC. First hydrogenation kinetics of alloys were studied at 20 bar of hydrogen pressure and room temperature after giving heat treatment at different temperatures for 6 hours. Among the various Zr doped alloys studied, the composition 52Ti-12V-36Cr + 4wt% Zr shows maximum hydrogen storage capacity of 3.6wt%. Small amount of Zr shows advantageous effects on kinetics of alloy. It was also found out that alloys with the higher Zr concentration can be activated by giving heat treatment at lower temperatures. There is reduction in hydrogen storage capacity with increasing Zr content in the alloy primarily due to increasing abundance of secondary phase as established by X-Ray Diffraction and Scanning Electron Microscope results.

Keywords: hydrogen storage, metal hydrides, bcc alloy, heat treatment

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Authors: Siva Prasad Peddi

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Silver nanoparticles were successfully synthesized from silver nitrate through a rapid green synthesis method using Eclipta prostrata leaf extract as a reducing cum stabilizing agent. The experimental procedure was readily conducted at room temperature and pressure, and could be easily scaled up. The silver nanoparticles thus obtained were characterized using UV-Visible Spectroscopy (UV-VIS) which yielded an absorption peak at 416 nm. The biomolecules responsible for capping of the bio-reduced silver nanoparticles synthesized using plant extract were successfully identified through FTIR analysis. It was evinced through Scanning Electron Microscope (SEM), and X-ray diffraction (XRD) analysis that the silver nanoparticles were crystalline in nature and spherical in shape. The average size of the particles obtained using Scherrer’s formula was 27.4 nm. The adopted technique for silver nanoparticle synthesis is suitable for large-scale production.

Keywords: silver nanoparticles, green synthesis, characterization, Eclipta prostrata

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Authors: Shreyash Hadke, Manendra Singh Parihar, Rajesh Khatirkar

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In the present investigation, the variation in the microstructure with the changes in the heat treatment conditions i.e. temperature and time was observed. Ti-6Al-4V alloy was subject to solution annealing treatments in β (1066C) and α+β phase (930C and 850C) followed by quenching, air cooling and furnace cooling to room temperature respectively. The effect of solution annealing and cooling on the microstructure was studied by using optical microscopy (OM), scanning electron microscopy (SEM), electron backscattered diffraction (EBSD) and x-ray diffraction (XRD). The chemical composition of the β phase for different conditions was determined with the help of energy dispersive spectrometer (EDS) attached to SEM. Furnace cooling resulted in the development of coarser structure (α+β), while air cooling resulted in much finer structure with widmanstatten morphology of α at the grain boundaries. Quenching from solution annealing temperature formed α’ martensite, their proportion being dependent on the temperature in β phase field. It is well known that the transformation of β to α follows Burger orientation relationship (OR). In order to reconstruct the microstructure of parent β phase, a MATLAB code was written using neighbor-to-neighbor, triplet method and Tari’s method. The code was tested on the annealed samples (1066C solution annealing temperature followed by furnace cooling to room temperature). The parent phase data thus generated was then plotted using the TSL-OIM software. The reconstruction results of the above methods were compared and analyzed. The Tari’s approach (clustering approach) gave better results compared to neighbor-to-neighbor and triplet method but the time taken by the triplet method was least compared to the other two methods.

Keywords: Ti-6Al-4V alloy, microstructure, electron backscattered diffraction, parent phase reconstruction

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Authors: Gurpreet Singh, Hazoor Singh, Buta Singh Sidhu

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In the current investigation plasma spray technique was used for depositing hydroxyapatite (HA) and HA – silicon oxide (SiO2) coatings on 316L SS substrate. In HA-SiO2 coating, 20 wt% SiO2 was mixed with HA. The feedstock and coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM)/energy-dispersive X-ray spectroscopy (EDX) analyses. The corrosion resistance of the uncoated, HA coated and HA + 20 wt% SiO2 coated 316L SS was investigated by electrochemical corrosion testing in simulated human body fluid (Ringer’s solution). The influence of SiO2 (20 wt%) on corrosion resistance was determined. After the corrosion testing, the samples were analyzed by XRD and SEM/EDX analyses. The addition of SiO2 reduces the crystallinity of the coating. The corrosion resistance of the 316L SS was found to increase after the deposition of the HA + 20 wt% SiO2 and HA coatings.

Keywords: HA, SiO2, corrosion, Ringer’s solution, 316L SS

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Authors: Victor A. Okenyi, Kehinde A. Alawode

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Corrosion of reinforcement in concrete structures remains a durability issue in structural engineering with the increasing cost of repair and maintenance. The mechanism and factors influencing reinforcement corrosion in concrete with various electrochemical monitoring techniques including non-destructive, destructive techniques and the roles of sensors have been reviewed with the aim of determining the monitoring technique that proved most effective in determining corrosion parameters and more practicable for the assessment of concrete durability. Electrochemical impedance spectroscopy (EIS) and linear polarization resistance (LPR) techniques showed great performance in evaluating corrosion kinetics and corrosion rate, respectively, while the gravimetric weight loss (GWL) technique provided accurate measurements. However, no single monitoring technique showed to be the ultimate technique, and this calls for more research work in the development of more dynamic monitoring tools capable of considering all possible corrosion factors in the corrosion monitoring process.

Keywords: corrosion, concrete structures, durability, non-destructive technique, sensor

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Authors: Bounar Nedjemeddine

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Materials with the pyrochlore lattice structure have attracted much recent attention due to their wide applications in ceramic thermal barrier coatings, high-permittivity dielectrics, and potential solid electrolytes in solid-oxide fuel cells. The work described in this paper is devoted to the synthesis and characterization of a pyrochlore structure based on lanthanum (La₂O₃) and tin (SnO₂) oxides of general formula La₂Sn₂O₇, substituted by Sr at the site La. Their structures were determined from X-ray powder diffraction using CELFER analysis. All the compositions present the space group Fd-3m. The substitution of La by Sr in the La₂Sn₂O₇ compound causes a variation of the cell parameters. The difference in charge between La³⁺ and Sr²⁺ and the difference in size cause the cell parameters to decrease from a=10.7165 A° to a=10.6848 A° for the substitution rates (x = 0.05, 0.1, 0.15 ...), which leads to a decrease in the volume of the mesh. For a substitution rate x = 0.25, there is an increase in the cell parameters (a=10.7035A°), which can be explained by a competitiveness of the size effect and the presence of a gap in the structure which go in the opposite direction.

Keywords: solid-oxide fuel cells, structure, pyrochlore, X-ray diffraction

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Authors: C. L. Popa, S. L. Iconaru, A. Costescu, C. S. Ciobanu, M. Motelica Heino, R. Guegan, D. Predoi

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Surface functionalization of ceramic composites with a special focus on tetraethyl orthosilicate (TEOS) and hydroxyapatite (HAp) is discoursed. Mesoporous ceramic HAp-TEOS composites were prepared by the incorporation of hydroxyapatite into tetraethyl orthosilicate by sol-gel method. The resulting samples were analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and Raman spectroscopy and nitrogen physisorption. The removal of Pb2+ ions from aqueous solutions was evaluated using Atomic Absorbtion Spectroscopy (AAS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled Pb2+ at pH ~ 3 and pH ~ 5. After removal experiment of Pb2+ at pH 3 and pH 5, porous hydroxyapatite nanoparticles is transformed into PbHAp_3 and PbHAp_5 via the adsorption of Pb2+ ions followed by the cation exchange reaction. The diffraction patterns show that THAp nanoparticles were successfully coated with teos without any structural changes. On the other, the AAS analysis showed that THAp can be useful in the removal Pb2+ from water contaminated.

Keywords: teos, hydroxyapatite, environment applications, biosystems engineering

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Authors: Neha Thakur, Pravin S. More

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The interaction of CO, H2 and LPG with Cu-dosed SnO2 catalysts was studied by means of Fourier transform infrared spectroscopy (FTIR). With increasing Cu loading, pronounced and progressive red shifts of the C–O stretching frequency associated with molecular CO adsorbed on the Cu/SnO2 component were observed. This decrease in n(CO) correlates with enhancement of CO dissociation at higher temperatures on Cu promoted SnO2 catalysts under conditions, where clean Cu is almost ineffective. In the conclusion, the capability of our technique is discussed, and a technique for enhancing the sensitivity in our technique is proposed.

Keywords: FTIR, spectroscopic, dissociation, n(CO)

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Authors: Anjan Sil, Rajni Sharma, Subrata Ray

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The effect of carbon nanofibers (CNFs) on the electrical properties of Poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP)) based gel polymer electrolytes has been investigated in the present work. The length and diameter ranges of CNFs used in the present work are 5-50 µm and 200-600 nm, respectively. The nanocomposite gel polymer electrolytes have been synthesized by solution casting technique with varying CNFs content in terms of weight percentage. Electrochemical impedance analysis demonstrates that the reinforcement of carbon nanofibers significantly enhances the ionic conductivity of the polymer electrolyte. The decrease of crystallinity of P(VdF-HFP) due the addition of CNFs has been confirmed by X-ray diffraction (XRD). The interaction of CNFs with various constituents of nanocomposite gel polymer electrolytes has been assessed by Fourier Transform Infrared (FTIR) spectroscopy. Moreover, CNFs added gel polymer electrolytes offer superior thermal stability as compared to that of CNFs free electrolytes as confirmed by Thermogravimetric analysis (TGA).

Keywords: polymer electrolytes, CNFs, ionic conductivity, TGA

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Authors: Aji Budi Rinekso

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There are some common problems that are often faced by students in writing. The problems are related to macro and micro skills of writing, such as incorrect spellings, inappropriate diction, grammatical errors, random ideas, and irrelevant supporting sentences. Therefore, it is needed a teaching technique that can solve those problems. Dictogloss technique is a teaching technique that involves listening practices. So, it is a suitable teaching technique for students with auditory learning style. Dictogloss technique comprises of four basic steps; (1) warm up, (2) dictation, (3) reconstruction and (4) analysis and correction. Warm up is when students find out about topics and do some preparatory vocabulary works. Then, dictation is when the students listen to texts read at normal speed by a teacher. The text is read by the teacher twice where at the first reading the students only listen to the teacher and at the second reading the students listen to the teacher again and take notes. Next, reconstruction is when the students discuss the information from the text read by the teacher and start to write a text. Lastly, analysis and correction are when the students check their writings and revise them. Dictogloss offers some advantages in relation to the efforts of improving writing skills. Through the use of dictogloss technique, students can solve their problems both on macro skills and micro skills. Easier to generate ideas and better writing mechanics are the benefits of dictogloss.

Keywords: auditory learners, writing skills, dictogloss technique, second language learning

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Authors: Mingmei Zhang, Xinyong Li

Abstract:

Novel AgInS2/SnS2/RGO (AISR) heterojunctions photocatalysts were synthesized by simple hydrothermal method. The morphology and composition of the fabricated AISR nanocomposites were investigated by field-emission scanning electron microscopy (SEM), X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). Moreover, the as-prepared AISR photocatalysts exhibited excellent photocatalytic activities for the degradation of Norfloxacin (NOR), mainly due to its high optical absorption and separation efficiency of photogenerated electron-hole pairs, as evidenced by UV–vis diffusion reflection spectra (DRS) and Surface photovoltage (SPV) spectra. Furthermore, laser flash photolysis technique was conducted to test the lifetime of charge carriers of the fabricated nanocomposites. The interfacial charges transfer mechanism was also discussed.

Keywords: AISR heterojunctions, electron-hole pairs, SPV spectra, charges transfer mechanism

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Authors: M. Belhadj Lachachi, Tayeb Benabdallah, M. Hadj Youcef, Jason M. Lynama

Abstract:

The application of inorganic chemistry to catalysis and environmental chemistry is a rapidly developing field, and novel catalytic metal complexes are now having an impact on the industrial development practice. Advances in organometallic chemistry are crucial for improving the design of compounds to reduce toxic side effects and understand their mechanisms of action. The reaction of platinum(II) organometallic complexes with bidentate Schiff bases derived from 2-Hydroxynaphtalydeneaniline have been carried out. It concerns N,N’-naphtalidene para-nitroaniline (1-a), the, the N,N’-naphtalidene para-ethoxyaniline (1-b), the N,N’-naphtalideneaniline (1-c), the N,N’-naphtalidene para-chloroaniline (1-d) and the N,N’-naphtalidene para-methoxyaniline (1-e). The ligands were fully characterized by I.R., elemental analysis, 1H-NMR, 13C-NMR, ESI Mass Spectrometry and X-Ray Diffraction. The resulting metal complexes were obtained as a cationic species, through a simple substitution reaction, leading to two geometric isomers [1, 2], and characterized by IR, 1H-NMR, 13C-NMR, LIFDI Mass Spectrometry and supported by Elemental Analysis and X-Ray diffraction. Furthermore, a bimetallic platinum complex was prepared from the same ligands and dichloro(1,5-cyclooctadiene)platinum and characterized by X-Ray diffraction [3]The catalytic properties of the prepared platinum complexes in the hydrogenative and dehydrogenative silylation of styrene were investigated, and reaction kinetics conversion to products was determined by 1H-NMR and confirmed by GC-MS. This presentation will detail a comparison of the catalytic activity of five platinum organometallic complexes bearing different Schiff base ligands in the hydrosilylation of styrene, varying the experimental conditions of temperature, nature of the complex and the loading of the catalyst.

Keywords: catalysis, hydrosilylation, organometallic, schiff base

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Authors: Yuhao Jin, Zhou Zhou, Katsumi Yoshida, Zhengcao Li, Tadashi Maruyama, Toyohiko Yano

Abstract:

Four kinds of nuclear graphite, IG-110U, ETP-10, CX-2002U and IG-430U were neutron-irradiated at different fluences and temperatures, ranged from 1.38 x 1024 to 7.4 x 1025 n/m2 (E > 1.0 MeV) at 473K, 573K and 673K. To take into account the disorder in the microstructure, such as stacking faults and anisotropic coherent lengths, the X-ray diffraction patterns were interpreted using a comprehensive structural model and a refinement program CARBONXS. The deduced structural parameters show the changes of lattice parameters, coherent lengths along the c-axis and the basal plane, and the degree of turbostratic disorder as a function of the irradiation dose. Our results reveal neutron irradiation effects on the microstructure and macroscopic dimension, which are consistent with previous work. The methodology used in this work enables the quantification of the damage on the microstructure of nuclear graphite induced by neutron irradiation.

Keywords: nuclear graphite, neutron irradiation, thermal annealing, recovery behavior, dimensional change, CARBONX, XRD analysis

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Authors: Ayla Roberta Galaco, Juliana Fonseca De Lima, Osvaldo Antonio Serra

Abstract:

Coordination polymers, also known as metal-organic frameworks (MOFs) or lanthanoide organic frameworks (LOFs) have been reported due of their promising applications in gas storage, separation, catalysis, luminescence, magnetism, drug delivery, and so on. As a type of organic–inorganic hybrid materials, the properties of coordination polymers could be chosen by deliberately selecting the organic and inorganic components. LOFs have received considerable attention because of their properties such as porosity, luminescence, and magnetism. Methods such as solvothermal synthesis are important as a strategy to control the structural and morphological properties as well as the composition of the target compounds. In this work the first solvothermal synthesis was employed to obtain the compound [Y0.4,Yb0.4,Er0.2(dmf)(for)(H2O)(tft)], by using terephthalic acid (tft) and oxalic acid, decomposed in formate (for), as ligands; Yttrium, Ytterbium and, Erbium as metal centers, in DMF and water for 4 days under 160 °C. The semi-rigid terephthalic acid (dicarboxylic) coordinates with Ln3+ ions and also is possible to form a polyfunctional bridge. On the other hand, oxalate anion has no high-energy vibrational groups, which benefits the excitation of Yb3+ in upconversion process. It was observed that the compounds with water molecules in the coordination sphere of the lanthanoide ions cause lower crystalline properties and change the structure of the LOF (1D, 2D, 3D). In the FTIR, the bands at 1589 and 1500 cm-1 correspond to the asymmetric stretching vibration of –COO. The band at 1383 cm-1 is assigned to the symmetric stretching vibration of –COO. Single crystal X-ray diffraction study reveals an infinite 3D coordination framework that crystalizes in space group P21/c. The other three products, [TR(chel)(ofd)0,5(H2O)2], where TR= Eu3+, Y3, and Yb3+/Er3+ were obtained by using 1, 2-phenylenedioxydiacetic acid (ofd) and chelidonic acid (chel) as organic ligands. Thermal analysis shows that the lanthanoide organic frameworks do not collapse at temperatures below 250 °C. By the polycrystalline X-ray diffraction patterns (PXRD) it was observed that the compounds with Eu3+, Y3+, and Yb3+/Er3+ ions are isostructural. From PXRD patterns, high crystallinity can be noticed for the complexes. The final products were characterized by single X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), energy dispersive spectroscopy (EDS) and thermogravimetric analysis (TGA). The X-ray diffraction (XRD) is an effective method to investigate crystalline properties of synthesized materials. The solid crystal obtained in the synthesis show peaks at 2θ < 10°, indicating the MOF formation. The chemical composition of LOFs was also confirmed by EDS.

Keywords: isostructural, lanthanoids, lanthanoids organic frameworks (LOFs), metal organic frameworks (MOFs), thermogravimetry, X-Ray diffraction

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Authors: Khalid H. Abass

Abstract:

Al-Ni-Cr alloy contains different ratios of Ni and Cr was prepared by mixing Al, Ni and Cr at 800oC under an argon atmosphere. The prepared alloys were heated for 1300 hr to 560oC, and then cooled rapidly by water at the ambient temperature. Surface morphology for alloys is studied by scanning electron microscope (SEM). The resultant homogeneous surface is a result of heat treatment. The X-ray diffraction patterns showed (111), (200), and (220) diffraction lines from cubic Al crystal structure, and suggested that the intensity of peak (111) orientation is predominant. Three binary phases were observed and grown in alloys: Al3Ni (Orthorhombic, a = 6.598Ǻ, b = 7.352 Ǻ, c = 4.802 Ǻ), Cr9Al17 (Rhombohedra, a = 12.910 Ǻ, c = 15.677), and Ni2Cr3 (Tetragonal, a = 8.82 Ǻ, c = 4.58 Ǻ). The average crystallite sizes of the prepared samples were found to be from 3000 to 3094 nm by SEM, which is much smaller than that estimated from XRD data. Corrosion resistance increases with increasing Ni-Cr content in Al alloys. The electrical volume resistivity decreased with increasing Ni-Cr content at low frequency. This behavior can be seen generally at 50Hz, where the electrical volume resistivity reached the value of 3.98×10-8Ω.cm for the ratio Al-1.8 at.%Ni-0.18at.%Cr.

Keywords: Al-Ni-Cr alloy, corrosion current, electrical volume resistivity, binary phase, homogeneous surface

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