Search results for: Energy Dispersive X-Ray Spectroscopy (EDS)

Authors: Hanan Alenezi

Abstract:

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

Keywords: Energy Dispersive X-Ray Spectroscopy (EDS), Membrane, Polyetherimide PEI, Scanning electron microscope (SEM), Solvent, X-Ray Diffraction (XRD)

Procedia PDF Downloads 143

Authors: Mohsen Sanayei, Jerzy Szpunar, Sami Penttilä

Abstract:

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

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

Procedia PDF Downloads 290

Authors: Ghada Ben Hamad, Zohir Younsi, Fabien Salaun, Hassane Naji, Noureddine Lebaz

Abstract:

The graphene oxide (GO) material has attracted much attention for solar energy applications. This paper reports the synthesis and characterization of partially oxidized graphite oxide (GTO). GTO was obtained by modified Hummers method, which is based on the chemical oxidation of natural graphite. Several samples were prepared with different oxidation degree by an adjustment of the oxidizing agent’s amount. The effect of the oxidation degree on the chemical structure and on the morphology of GTO was determined by using Fourier transform infrared (FT-IR) spectroscopy, Energy Dispersive X-ray Spectroscopy (EDS), and scanning electronic microscope (SEM). The thermal stability of GTO was evaluated by using thermogravimetric analyzer (TGA) in Nitrogen atmosphere. The results indicate high degree oxidation of graphite oxide for each sample, proving that the process is efficient. The GTO synthesized by modified Hummers method shows promising characteristics. Graphene oxide (GO) obtained by exfoliation of GTO are recognized as a good candidate for thermal energy storage, and it will be used as solid shell material in the encapsulation of phase change materials (PCM).

Keywords: modified hummers method, graphite oxide, oxidation degree, solar energy storage

Procedia PDF Downloads 90

Authors: Darlington Ashiegbu, Herman Johannes Potgieter

Abstract:

The increasing utilization of Zinc Oxide (ZnO) as a better alternative to TiO₂ has been attributed to its wide bandgap (3.37eV), lower production cost, ability to absorb over a larger range of the UV-spectrum and higher efficiency in some cases. ZnO nanoparticles were synthesized via sol-gel process and calcined at 400ᵒC, 500ᵒC, and 650ᵒC. The as-synthesized nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and Brunauer–Emmett–Teller (BET) surface area measurement. Scanning electron micrograph revealed pseudo-spherical and rod-like morphologies and a high rate of agglomeration for the sample calcined at 650ᵒC, Brunnauer Emmett Teller (BET) surface area measurement was highest in the sample calcined at 500ᵒC, energy dispersive X-ray spectroscopy (EDS) results confirmed the purity of the samples as only Zn and O₂ were detected and X-ray diffraction (XRD) results revealed crystalline hexagonal wurtzite structure of the ZnO nanoparticles. All three samples were utilized in the degradation of ethylbenzene, and a UV-Vis spectrophotometer was utilized in monitoring degradation of ethylbenzene. The sample calcined at 500ᵒC had the highest surface area for reaction, lowest agglomeration and the highest photocatalytic activity in the degradation of ethylbenzene. This revealed temperature as a very important factor in improved and higher photocatalytic activity.

Keywords: ethylbenzene, pseudo-spherical, sol-gel, zinc oxide

Procedia PDF Downloads 130

Authors: S. Zhuiykov, E. Kats

Abstract:

Electrical properties and morphology of orthorhombic β–WO3 nano-flakes with thickness of ~7-9 nm were investigated at the nano scale using energy dispersive X-ray diffraction (XRD), X-ray photo electron spectroscopy (XPS) and current sensing force spectroscopy atomic force microscopy (CSFS-AFM, or PeakForce TUNATM). CSFS-AFM analysis established good correlation between the topography of the developed nano-structures and various features of WO3 nano-flakes synthesized via a two-step sol-gel-exfoliation method. It was determined that β–WO3 nano-flakes annealed at 550ºC possess distinguished and exceptional thickness-dependent properties in comparison with the bulk, micro- and nano-structured WO3 synthesized at alternative temperatures.

Keywords: electrical properties, layered semiconductors, nano-flake, sol-gel, exfoliation WO3

Procedia PDF Downloads 213

Authors: Hakan Gungunes, Ismail A. Auwal, Abdulhadi Baykal, Sagar E. Shirsath

Abstract:

Barium hexaferrite, BaFe₁₂O₁₉, substituted by Bi³⁺ and La³⁺ (BaBiₓLaₓFe₁₂₋₂ₓO₁₉ where 0.0 ≤ x ≤ 0.5) were prepared by solid state synthesis route. The effect of substituted Bi³⁺ and La³⁺ ions on the structure, morphology, magnetic and cation distributions of barium hexaferrite were investigated by X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR) and Mössbauer spectroscopy. XRD powder patterns were refined by the Rietveld analysis method which confirmed the formation of single phase magneto-plumbite structure and the substitution of La³⁺ and Bi³⁺ ions into the lattice of barium ferrite. These results show that both La³⁺ and Bi³⁺ ions completely enter into barium hexaferrite lattice without disturbing the hexagonal ferrite structure. The EDX spectra confirmed the presence of all the constituents in expected elemental percentage. From 57Fe Mössbauer spectroscopy data, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values on Bi and La substitutions have been determined. Cation distribution in the presently investigated hexaferrite system was estimated using the relative area of Mössbauer spectroscopy.

Keywords: hexaferrite, mössbauer, cation distribution, solid state synthesis

Procedia PDF Downloads 335

Authors: C. L Popa, C.S. Ciobanu, S. L. Iconaru, P. Chapon, A. Costescu, P. Le Coustumer, D. Predoi

Abstract:

In this paper, the preparation and characterization of silver doped hydroxyapatite thin films and their antimicrobial activity characterized is reported. The resultant Ag: HAp films coated on commercially pure Si disks substrates were systematically characterized by Scanning Electron Microscopy (SEM) coupled with X-ray Energy Dispersive Spectroscopy detector (X-EDS), Glow Discharge Optical Emission Spectroscopy (GDOES) and Fourier Transform Infrared spectroscopy (FT-IR). GDOES measurements show that a substantial Ag content has been deposited in the films. The X-EDS and GDOES spectra revealed the presence of a material composed mainly of phosphate, calcium, oxygen, hydrogen and silver. The antimicrobial efficiency of Ag:HAp thin films against Escherichia coli and Staphylococcus aureus bacteria was demonstrated. Ag:HAp thin films could lead to a decrease of infections especially in the case of bone and dental implants by surface modification of implantable medical devices.

Keywords: silver, hydroxyapatite, thin films, GDOES, SEM, FTIR, antimicrobial effect

Procedia PDF Downloads 396

Authors: Charles Klein O. Gorit, Mark Tristan J. Quimque Jr., M. Cecilia V. Almeda, Concepcion M. Salvana

Abstract:

Chitosan is a promising biopolymer commonly found in crustacean shells that has plausible effects in water purification and wastewater treatment. It is a primary derivative of chitin and considered second of the most abundant biopolymer prior to cellulose. Morphological analysis had been done using Scanning Electron Microscopy with Energy Dispersive Microscopy (SEM/EDS), and due to its porous nature, it showcases a certain degree of porosity, hence, larger adsorption site of heavy metal. The Energy Dispersive Spectroscopy of the chitosan and ‘lead-bound’ chitosan, shows a relative increase of percent abundance of lead cation from 1.44% to 2.08% hence, adsorption occurs. Chitosan, as a nitrogenous polysaccharide, subjected to Fourier transform infrared spectroscopy (FTIR) analysis shows amide bands ranging from 1635.36 cm⁻¹ for amide 1 band and 1558.40 cm-1 for amide 2 band with NH stretching. For ‘lead-bound’ chitosan, the FT-IR analysis shows a change in peaks upon adsorption of Pb(II) cation. The spectrum shows broadening of OH and NH stretching band. Such observation can be attributed to the probability that the attachment of Pb(II) ions is in these functional groups. A column filter was devised with lead-bound chitosan to determine the zero point charge (pHzpc) of the biopolymer. The results show that at pH 8.34, below than the zpc level of literatures cited for lead which ranges from pH 4 to 7, favors the adsorption site of chitosan and its capability to adsorb traces amount of aqueous lead.

Keywords: chitosan, biopolymer, FT-IR, SEM, zero-point charge, heavy metal, lead ions

Procedia PDF Downloads 115

Authors: Gabriel K. Nzulu, Lina Rostorm, Hans Högberg, Jun Liu, per Eklund, Lars Hultman, Martin Magnuson

Abstract:

Altered and gangue quartz in hydrothermal veins from the Kubi Gold deposit in Dunkwa on Offin in the central region of Ghana are investigated for possible Au associated pathfinder minerals and to provide understanding and increase the knowledge of the mineral hosting and alteration processes in quartz. X-ray diffraction, air annealing furnace, differential scanning calorimetry, energy dispersive X-ray spectroscopy, and transmission electron microscopy have been applied on different quartz types outcropping from surface and bed rocks at the Kubi Gold Mining to reveal the material properties at different temperatures. From the diffraction results of the fresh and annealed quartz samples, we find that the samples contain pathfinder and the impurity minerals FeS₂, biotite, TiO₂, and magnetite. These minerals, under oxidation process between 574-1400 °C temperatures experienced hematite alterations and a transformation from α-quartz to β-quartz and further to cristobalite as observed from the calorimetry scans for hydrothermally exposed materials. The energy dispersive spectroscopy revealed elemental species of Fe, S, Mg, K, Al, Ti, Na, Si, O, and Ca contained in the samples and these are attributed to the impurity phase minerals observed in the diffraction. The findings also suggest that during the hydrothermal flow regime, impurity minerals and metals can be trapped by voids and faults. Under favorable temperature conditions the trapped minerals can be altered to change color at different depositional stages by oxidation and reduction processes leading to hematite alteration which is a useful pathfinder in mineral exploration.

Keywords: quartz, hydrothermal, minerals, hematite, x-ray diffraction, crystal-structure, defects

Procedia PDF Downloads 61

Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda

Abstract:

In this report, the impact of Gd³⁺ substitution in ZnFe₂O₄ spinel ferrite nanoparticles on structural, optical and magnetic properties was investigated. ZnFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) nanoparticles were synthesized by honey-mediated sol-gel combustion method. X-ray diffraction, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy confirmed the formation of cubic spinel ferrite crystal structure. The morphology and elemental analysis were studied using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. UV-Visible reflectance spectroscopy revealed band gap variation with concentration of Gd³⁺ substitution in ZnFe₂O₄ nanoparticles. Magnetic property was studied using vibrating sample magnetometer at room temperature. The synthesized spinel ferrite nanoparticles showed ferromagnetic behaviour. The evaluated magnetic parameters such as saturation magnetization, coercivity and remanence showed variation with Gd³⁺ substitution in spinel ferrite nanoparticles. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: sol-gel combustion method, nanoparticles, magnetic property, optical property

Procedia PDF Downloads 264

Authors: Jan Luxa, Vlastimil Mazanek, Petr Malinsky, Alexander Romanenko, Mariapompea Cutroneo, Vladimir Havranek, Josef Novak, Eva Stepanovska, Anna Mackova, Zdenek Sofer

Abstract:

Using accelerated energetic ions is an interesting method for the introduction of structural changes in various carbon-based materials. This way, the properties can be altered in two ways: a) the ions lead to the formation of conductive pathways in graphene oxide structures due to the elimination of oxygen functionalities and b) doping with selected ions to form metal nanoclusters, thus increasing the conductivity. In this work, energetic beams were employed in two ways to prepare capacitor structures in graphene oxide (GO), reduced graphene oxide (rGO) and polyimide (PI) on a micro-scale. The first method revolved around using ion beam writing with a focused ion beam, and the method involved ion implantation via a polymeric mask. To prepare the polymeric mask, a direct spin-coating of PMMA on top of the foils was used. Subsequently, proton beam writing and development in isopropyl alcohol were employed. Finally, the mask was removed using acetone solvent. All three materials were exposed to ion beams with an energy of 2.5-5 MeV and an ion fluence of 3.75x10¹⁴ cm-² (1800 nC.mm-²). Thus, prepared microstructures were thoroughly characterized by various analytical methods, including Scanning electron microscopy (SEM) with Energy-Dispersive X-ray spectroscopy (EDS), X-ray Photoelectron spectroscopy (XPS), micro-Raman spectroscopy, Rutherford Back-scattering Spectroscopy (RBS) and Elastic Recoil Detection Analysis (ERDA) spectroscopy. Finally, these materials were employed and tested as sensors for humidity using electrical conductivity measurements. The results clearly demonstrate that the type of ions, their energy and fluence all have a significant influence on the sensory properties of thus prepared sensors.

Keywords: graphene, graphene oxide, polyimide, ion implantation, sensors

Procedia PDF Downloads 43

Authors: N. Boudinar, A. Djekoun, A. Otmani, B. Bouzabata, J. M. Greneche

Abstract:

High-energy ball milling is a solid-state powder processing technique that allows synthesizing a variety of equilibrium and non-equilibrium alloy phases starting from elemental powders. The advantage of this process technology is that the powder can be produced in large quantities and the processing parameters can be easily controlled, thus it is a suitable method for commercial applications. It can also be used to produce amorphous and nanocrystalline materials in commercially relevant amounts and is also amenable to the production of a variety of alloy compositions. Mechanical alloying (high-energy ball milling) provides an inter-dispersion of elements through a repeated cold welding and fracture of free powder particles; the grain size decreases to nano metric scale and the element mix together. Progressively, the concentration gradients disappear and eventually the elements are mixed at the atomic scale. The end products depend on many parameters such as the milling conditions and the thermodynamic properties of the milled system. Here, the mechanical alloying technique has been used to prepare nano crystalline Fe_50 and Fe_64 wt.% Ni alloys from powder mixtures. Scanning electron microscopy (SEM) with energy-dispersive, X-ray analyses and Mössbauer spectroscopy were used to study the mixing at nanometric scale. The Mössbauer Spectroscopy confirmed the ferromagnetic ordering and was use to calculate the distribution of hyperfin field. The Mössbauer spectrum for both alloys shows the existence of a ferromagnetic phase attributed to γ-Fe-Ni solid solution.

Keywords: nanocrystalline, mechanical alloying, X-ray diffraction, Mössbauer spectroscopy, phase transformations

Procedia PDF Downloads 407

Authors: T. V. Dinh, I. Y. Choi, J. W. Ahn, Y. H. Oh, G. Bo, J. Y. Lee, J. C. Kim

Abstract:

A Non-Dispersive Infrared (NDIR) multi-gas analyzer has been developed to monitor the emission of carbon monoxide (CO) and sulfur dioxide (SO2) from various industries. The NDIR technique for gas measurement is based on the wavelength absorption in the infrared spectrum as a way to detect particular gasses. NDIR analyzers have popularly applied in the Tele-Monitoring System (TMS). The advantage of the NDIR analyzer is low energy consumption and cost compared with other spectroscopy methods. However, zero/span drift and interference are its urgent issues to be solved. Multi-pathway technique based on optical White cell was employed to improve the sensitivity of the analyzer in this work. A pyroelectric detector was used to detect the Infrared radiation. The analytical range of the analyzer was 0 ~ 200 ppm. The instrument response time was < 2 min. The detection limits of CO and SO2 were < 4 ppm and < 6 ppm, respectively. The zero and span drift of 24 h was less than 3%. The linearity of the analyzer was less than 2.5% of reference values. The precision and accuracy of both CO and SO2 channels were < 2.5% of relative standard deviation. In general, the analyzer performed well. However, the detection limit and 24h drift should be improved to be a more competitive instrument.

Keywords: analyzer, CEMS, monitoring, NDIR, TMS

Procedia PDF Downloads 224

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

Abstract:

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

Keywords: bacteria, biosynthesis, silver-phosphate, Sporosarcina pasteurii, nanoparticle

Procedia PDF Downloads 419

Authors: Swati Sharma, R. P. Sharma

Abstract:

We intend to study the nonlinear evolution of the parallel propagating finite frequency Alfvén wave (also called Dispersive Alfvén wave/Hall MHD wave) propagating in the solar wind regime of the solar region when a perpendicularly propagating magnetosonic wave is present in the background. The finite frequency Alfvén wave behaves differently from the usual non-dispersive behavior of the Alfvén wave. To study the nonlinear processes (such as filamentation) taking place in the solar regions such as solar wind, the dynamical equation of both the waves are derived. Numerical simulation involving finite difference method for the time domain and pseudo spectral method for the spatial domain is then performed to analyze the transient evolution of these waves. The power spectra of the Dispersive Alfvén wave is also investigated. The power spectra shows the distribution of the magnetic field intensity of the Dispersive Alfvén wave over different wave numbers. For DAW the spectra shows a steepening for scales larger than the proton inertial length. This means that the wave energy gets transferred to the solar wind particles as the wave reaches higher wave numbers. This steepening of the power spectra can be explained on account of the finite frequency of the Alfvén wave. The obtained results are consistent with the observations made by CLUSTER spacecraft.

Keywords: solar wind, turbulence, dispersive alfven wave

Procedia PDF Downloads 573

Authors: Afshin Zohdi, Selçuk Özdemir, Mustafa Aksoy

Abstract:

Tungsten carbide-cobalt (WC-Co) is a widely utilized material for cold forming dies, including those employed in fastener production. In this study, we investigated the effectiveness of the pack boriding method in improving the surface properties of WC-Co cold forging dies. The boriding process involved embedding WC-Co samples, along with a steel control sample, within a chamber made of H13 tool steel. A boriding powder mixture was introduced into the chamber, which was then sealed using a paste. Subsequently, the samples were subjected to a temperature of 700°C for 5 hours in a furnace. Microstructural analysis, including cross-sectional examination and scanning electron microscopy (SEM), confirmed successful boron diffusion and its presence on the surface of the borided samples. The microhardness of the borided layer was significantly increased (3980 HV1) compared to the unborided sample (1320 HV3), indicating enhanced hardness. The borided layer exhibited an acceptable thickness of 45 microns, with a diffusion coefficient of 1.125 × 10-7 mm²/s, signifying a moderate diffusion rate. Energy-dispersive X-ray spectroscopy (EDS) mapping revealed an increase in boron content, desirable for the intended purpose, while an undesired increase in oxygen content was observed. Furthermore, the pin-on-disk wear test demonstrated a reduction in friction coefficient, indicating improved mechanical and tribological properties of the surface. The successful implementation of the pack boriding process highlights its potential for enhancing the performance of WC-Co cold forging dies.

Keywords: WC-Co, cold forging dies, pack boriding, surface hardness, wear resistance, microhardness, diffusion coefficient, scanning electron microscopy, energy-dispersive X-ray spectroscopy

Procedia PDF Downloads 45

Authors: Jiyaul Haque, Vandana Srivastava, M. A. Quraishi

Abstract:

The amino acids based corrosion inhibitors 2-(3-(carboxymethyl)-1H-imidazol-3-ium-1-yl) acetate (Z-1),2-(3-(1-carboxyethyl)-1H-imidazol-3-ium-1-yl) propanoate (Z-2) and 2-(3-(1-carboxy-2-phenylethyl)-1H-imidazol-3-ium-1-yl)-3- phenylpropanoate (Z-3) were synthesized by the reaction of amino acids, glyoxal and formaldehyde, and characterized by the FTIR and NMR spectroscopy. The corrosion inhibition performance of synthesized inhibitors was studied by electrochemical (EIS and PDP), surface and DFT methods. The results show, the studied Z-1, Z-2 and Z-3 are effective inhibitors, showed the maximum inhibition efficiency of 88.52 %, 89.48 and 96.08% at concentration 200ppm, respectively. The results of potentiodynamic polarization (PDP) study showed that Z-1 act as a cathodic inhibitor, while Z-2 and Z-3 act as mixed type inhibitors. The results of electrochemical impedance spectroscopy (EIS) studies showed that zwitterions inhibit the corrosion through adsorption mechanism. The adsorption of synthesized zwitterions on the mild steel surface was followed the Langmuir adsorption isotherm. The formation of zwitterions film on mild steel surface was confirmed by the scanning electron microscope (SEM) and energy-dispersive X-ray spectroscopy (EDX). The quantum chemical parameters were used to study the reactivity of inhibitors and supported the experimental results. An inhibitor adsorption model is proposed.

Keywords: electrochemical impedance spectroscopy, green corrosion inhibitors, mild steel, SEM, quantum chemical calculation, zwitterions

Procedia PDF Downloads 150

Authors: Temitope Olumide Olugbade

Abstract:

Low resistance and delayed fracture to corrosion, especially in harsh environmental conditions, often limit the wide application of high-manganese (high-Mn) steels. To address this issue, the present work investigates the influence of microalloying on the corrosion properties of high-Mn steels. Microalloyed and base high-Mn steels were synthesized through an arc melting process under an argon atmosphere. To generate different microstructures, the temperature and duration were varied via thermal homogenization treatments. The electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to determine the corrosion properties in 0.6 M NaCl aqueous solution at room temperature. The relationship between the microstructures and corrosion properties was investigated via Scanning Kelvin Probe Microscopy (SKPFM), energy dispersive X-ray spectroscopy (EDX), and Scanning electron microscopy (SEM) techniques. The local corrosion properties were investigated via in situ atomic force spectroscopy (AFM), considering the homogenization treatments. The results indicate that microalloying is a successful technique for enhancing the corrosion behavior of high-Mn steels. Compared to other alloying elements, Vanadium has shown improvement in corrosion properties for both general and local corrosion in chloride environments.

Keywords: corrosion, high-manganese steel, homogenization, microalloying, vanadium

Procedia PDF Downloads 40

Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

Abstract:

Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

Procedia PDF Downloads 41

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

Abstract:

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

Procedia PDF Downloads 84

Authors: H. Boucheloukh, N. Aoun, S. Rouissa, T. Sehili, F. Parrino, V. Loddo

Abstract:

Photocatalysis has made a revolution in wastewater treatment and the elimination of persistent organic pollutants. This process is based on the use of semiconductors as photocatalysts. In this study, nickel ferrite spinel (NiFe2O4) nanoparticles were successfully synthesized by the sol-gel route. The structural, morphological, elemental composition, chemical state, particle size, optical and electrochemical characterizations using powder X-ray diffraction (P-XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy(SEM), energy-dispersive X-ray spectroscopy (EDAX ). We tested the prepared NiFe2O4(NPS)by monitoring the degradation of Rose Bengal (RB) dye in an aqueous solution under direct sunlight irradiation. The effects of catalyst dosage and dye concentration were also considered for the effective degradation of RB dye. The optimum catalyst dosage and concentration of dye were found to be 1 g/L and 10 μM, respectively. A maximum of 80% photocatalytic degradation efficiency (DE%) was achieved at 120 min of direct sunlight irradiation.

Keywords: Rose Bengal, Nickelate, photocatalysis, irradiation

Procedia PDF Downloads 183

Authors: Sabir Hussain, Mujtaba Hassan, Kashif Rasool, Asif Shahzad

Abstract:

Fine particulate matter with an aerodynamic diameter of less than 2.5 μm (PM2.5) was collected in Islamabad from November 2022 to January 2023, at urban sites. The average mass concentrations of PM2.5 varied, ranging from 90.5 to 133 μg m−3 in urban areas. Environmental scanning electron microscopy (ESEM) analysis revealed that Islamabad's PM2.5 comprised soot aggregates, ashes, minerals, bio-particles, and unidentified particles. Results from inductively coupled plasma atomic emission spectroscopy (ICP-OES) indicated a gradual increase in total elemental concentrations in Islamabad PM2.5 in winter, with relatively high levels in December. Significantly different elemental compositions were observed in urban PM2.5. Enrichment factor (EF) analysis suggested that elements such as K, Na, Ca, Mg, Al, Fe, Ba, and Sr were of natural origin, while As, Cu, Zn, Pb, Cd, Mn, Ni, and Se originated from anthropogenic sources. Plasmid DNA assays demonstrated varying levels of potential toxicity in Islamabad PM2.5 collected from urban sites, as well as across different seasons. Notably, the urban winter PM2.5 sample exhibited much stronger toxicity compared to other samples. The presence of heavy metals in Islamabad PM2.5, including Cu, Zn, Pb, Cd, Cr, Mn, and Ni, may have synergistic effects on human health.

Keywords: islamabad particulate matter pm2.5, scanning electron microscopy with energy-dispersive x-ray spectroscopy(sem-eds), fourier transform infrared spectroscopy(ftir), inductively coupled plasma optical emission spectroscopy(icp-oes)

Procedia PDF Downloads 31

Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Jaromir Havlica, Lukas Kalina, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

Abstract:

In this work, CoFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) spinel ferrite nanoparticles are synthesized by sonochemical method. The structural properties and cation distribution are investigated using X-ray Diffraction (XRD), Raman Spectroscopy, Fourier Transform Infrared Spectroscopy and X-ray photoelectron spectroscopy. The morphology and elemental analysis are screened using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. The particle size measured by FE-SEM and XRD analysis confirm the formation of nanoparticles in the range of 7-10 nm. The electrical properties show that the Gd³⁺ doped cobalt ferrite (CoFe₂₋ₓGdₓO₄; x= 0.20) exhibit enhanced dielectric constant (277 at 100 Hz) and ac conductivity (20.17 x 10⁻⁹ S/cm at 100 Hz). The complex impedance measurement study reveals that as Gd³⁺ doping concentration increases, the impedance Z’ and Z’ ’ decreases. The influence of Gd³⁺ doping in cobalt ferrite nanoparticles on the magnetic property is examined by using vibrating sample magnetometer. Magnetic property measurement reveal that the coercivity decreases with Gd³⁺ substitution from 234.32 Oe (x=0.00) to 12.60 Oe (x=0.05) and further increases from 12.60 Oe (x=0.05) to 68.62 Oe (x=0.20). The saturation magnetization decreases with Gd³⁺ substitution from 40.19 emu/g (x=0.00) to 21.58 emu/g (x=0.20). This decrease follows the three-sublattice model suggested by Yafet-Kittel (Y-K). The Y-K angle increases with the increase of Gd³⁺ doping in cobalt ferrite nanoparticles.

Keywords: sonochemical method, nanoparticles, magnetic property, dielectric property, electrical property

Procedia PDF Downloads 325

Authors: Keri̇m Emre Öksüz, Şaduman Şen, Uğur Şen

Abstract:

0.5 wt. % B2O3–doped Ba (Ti1-xZrx) O3, (x=0-0.4) lead-free nanoceramics were synthesized using the solid-state reaction method by adopting the ball milling technique. The influence of the substitution content on crystallographic structure, phase transition, microstructure and sintering behaviour of BT and BZT ceramics were investigated. XRD analysis at room temperature revealed a structural transformation from tetragonal to rhombohedral with enhancement of ZrO2 content in the barium titanate matrix. The scanning electron microscope (SEM) and energy-dispersive X-ray spectroscopy (EDS) were used to investigate microstructure and surface morphology of the sintered samples. The evolution of the Raman spectra was studied for various compositions, and the spectroscopic signature of the corresponding phase was determined. Scanning Electron Microscope (SEM) observations revealed enhanced microstructural uniformity and retarded grain growth with increasing Zr content.

Keywords: BaTiO3, barium-titanate-zirconate, nanoceramics, raman spectroscopy

Procedia PDF Downloads 312

Authors: Hatem I. Mokhtar, Randa A. Abd-El-Salam, Ghada M. Hadad

Abstract:

An improved nano-composite of self-doped polyaniline nanofibers and silica-coated magnetite nanoparticles were prepared and evaluated for suitability to magnetic dispersive micro solid-phase extraction. The work focused on optimization of the composite capacity to extract four fluoroquinolones (FQs) antibiotics, ciprofloxacin, enrofloxacin, danofloxacin, and difloxacin from water and improvement of composite stability towards acid and atmospheric degradation. Self-doped polyaniline nanofibers were prepared by oxidative co-polymerization of aniline with anthranilic acid. Magnetite nanopariticles were prepared by alkaline co-precipitation and coated with silica by silicate hydrolysis on magnetite nanoparticles surface at pH 6.5. The composite was formed by self-assembly by mixing self-doped polyaniline nanofibers with silica-coated magnetite nanoparticles dispersions in ethanol. The composite structure was confirmed by transmission electron microscopy (TEM). Self-doped polyaniline nanofibers and magnetite chemical structures were confirmed by FT-IR while silica coating of the magnetite was confirmed by Energy Dispersion X-ray Spectroscopy (EDS). Improved stability of the composite magnetic component was evidenced by resistance to degrade in 2N HCl solution. The adsorption capacity of self-doped polyaniline nanofibers based composite was higher than previously reported corresponding composite prepared from polyaniline nanofibers instead of self-doped polyaniline nanofibers. Adsorption-pH profile for the studied FQs on the prepared composite revealed that the best pH for adsorption was in range of 6.5 to 7. Best extraction recovery values were obtained at pH 7 using phosphate buffer. The best solvent for FQs desorption was found to be 0.1N HCl in methanol:water (8:2; v/v) mixture. 20 mL of Spiked water sample with studied FQs were preconcentrated using 4.8 mg of composite and resulting extracts were analysed by HPLC-UV method. The prepared composite represented a suitable adsorbent phase for magnetic dispersive micro-solid phase application.

Keywords: fluoroquinolones, magnetic dispersive micro extraction, nano-composite, self-doped polyaniline nanofibers

Procedia PDF Downloads 97

Authors: Lila A. Alkhattaby, Norah A. Alsayegh, Mohammad S. Ansari, Mohammad O. Ansari

Abstract:

In this work, we doped zinc oxide ZnO with potassium K we have synthesized using the sol-gel method. Structural properties were depicted by X-ray diffractometer (XRD) and energy distribution spectroscopy, X-ray diffraction studies confirm the nanosized of the particles and favored orientations along the (100), (002), (101), (102), (110), (103), (200), and (112) planes confirm the hexagonal wurtzite structure of ZnO NPs. The optical properties study using the UV-Vis spectroscopy. The band gap decreases from 4.05 eV to 3.88 eV, the lowest band gap at 10% doped concentration. The photoluminescence (PL) spectroscopy results show two main peaks, a sharp peak at ≈ 384 nm in the UV region and a broad peak around 479 nm in the visible region. The highest intensity of the band-edge luminescence was for 2% doped concentration because of the combined effect of the decreased probability of nonradiative recombination and has better crystallinity.

Keywords: K doped ZnO, photoluminescence spectroscopy, UV-Vis spectroscopy, x-ray spectroscopy

Procedia PDF Downloads 205

Authors: Richard, Iyan Subiyanto, Chairul Hudaya

Abstract:

Activated carbon has been playing a significant role for many applications, especially in energy storage devices. However, commercially activated carbons generally require complicated processes and high production costs. Therefore, in this study, an activated carbon originating from green coke waste, that is economically affordable will be used as a carbon source. To synthesize activated carbon, KOH as an activator was employed with variation of C:KOH in ratio of 1:2, 1:3, 1:4, and 1:5, respectively, with an activation temperature of 700°C. The characterizations of activated carbon are obtained from Scanning Electron Microscopy, Energy Dispersive X-Ray, Raman Spectroscopy, and Brunauer-Emmett-Teller. The optimal activated carbon sample with specific surface area of 2,024 m²/g with high carbon content ( > 80%) supported by the high porosity carbon image obtained by SEM was prepared at C:KOH ratio of 1:4. The result shows that the synthesized activated carbon would be an ideal choice for energy storage device applications. Therefore, this study is expected to reduce the costs of activated carbon production by expanding the utilization of petroleum waste.

Keywords: activated carbon, energy storage material, green coke, specific surface area

Procedia PDF Downloads 132

Authors: Arifa Batool, Ghulam Hussain Bhatti, Syed Mujtaba Shah

Abstract:

Inorganic n-type (TiO2, CdO) and p-type (NiO, CuO) metal oxide nanoparticles were synthesized by a facile wet chemical method at room temperature. The morphological, compositional, structural and optical properties were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, FT-IR, XRD analysis, UV/Visible and fluorescence spectroscopy. All semiconducting nanoparticles were photosensitized with Ru (II) based Z907 dye in ethanol solvent by grafting. Grafting of dye on the surface of nanoparticles was confirmed by UV/Visible and FT-IR spectroscopy. The synthesized photo-active nanohybrid was thoroughly blended with P3HT, a solid electrolyte and I-V measurements under solar stimulated radiations 1000 W/m2 (AM 1.5) were recorded. Maximum incident photon to current conversion efficiency (IPCE) of 0.9% was achieved with dye functionalized Z907-TiO2 hybrid, IPCE of 0.72% was achieved with bulk-heterojunction of TiO2-Z907-CuO and IPCE of 0.68% was attained with nanocomposite of TiO2-CdO. TiO2 based Solar cells have maximum Jscvalue i.e.4.63 mA/cm2. Dye-functionalized TiO2-based photovoltaic devices were found more efficient than the reference device but the morphology of the device was a major check in progress.

Keywords: solar cell, bulk heterojunction, nanocomposites, photosensitization, dye sensitized solar cell

Procedia PDF Downloads 253

Authors: Mai M. Khalaf, Hany M. Abd El-Lateef

Abstract:

A new good application for the sol gel method is to improve the corrosion inhibition properties of carbon steel by the dip coating method of Nano TiO2 films and its modification with Poly Ethylene Glycol (PEG). The prepared coating samples were investigated by different techniques, X-ray diffraction, Scanning Electron Microscopy (SEM), transmission electron microscopy and Energy Dispersive X-ray Spectroscopy (EDAX). The corrosion inhibition performance of the blank carbon steel and prepared coatings samples were evaluated in 0.5 M H2SO4 by using Electrochemical Impedance Spectroscopy (EIS) and potentiodynamic polarization measurements. The results showed that corrosion resistance of carbon steel increases with increasing the number of coated layers of both nano–TiO2 films and its modification of PEG. SEM-EDAX analyses confirmed that the percentage atomic content of iron for the carbon steel in 0.5 M H2SO4 is 83% and after the deposition of the steel in nano TiO2 sol and that with PEG are 94.3% and 93.7% respectively.

Keywords: dip-coatings, corrosion protection, sol gel, TiO2 films, PEG

Procedia PDF Downloads 398

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

Abstract:

One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy

Procedia PDF Downloads 217