Search results for: Scanning Electron Microscopy-Energy Dispersive Spectroscopy

Authors: Abhishek Sraw, Amit Sobti, Yamini Pandey, R. K. Wanchoo, Amrit Pal Toor

Abstract:

Monocrotophos (MCP) is a widely used pesticide in India, which belong to an extremely toxic organophosphorus family, is persistent in nature and its toxicity is widely reported in all environmental segments in the country. Advanced Oxidation Process (AOP) is a promising solution to the problem of water pollution. TiO₂ is being widely used as a photocatalyst because of its many advantages, but it has a large band gap, due to which it is modified using metal and nonmetal dopant to make it active under sunlight and visible light. The use of nanosized powdered catalysts makes the recovery process extremely complicated. Hence the aim is to use low cost, easily available, eco-friendly clay material in form of bead as the support for the immobilization of catalyst, to solve the problem of post-separation of suspended catalyst from treated water. A recirculation type photocatalytic reactor (RTPR), using ultraviolet light emitting source (blue black lamp) was designed which work effectively for both suspended catalysts and catalyst coated clay beads. The bare, TiO₂ and W-TiO₂ coated clay beads were characterized by scanning electron microscopy (SEM), electron dispersive spectroscopy (EDS) and N₂ adsorption–desorption measurements techniques (BET) for their structural, textural and electronic properties. The study involved variation of different parameters like light conditions, recirculation rate, light intensity and initial MCP concentration under UV and sunlight for the degradation of MCP. The degradation and mineralization studies of the insecticide solution were performed using UV-Visible spectrophotometer, and COD vario-photometer and GC-MS analysis respectively. The main focus of the work lies in checking the recyclability of the immobilized TiO₂ over clay beads in the developed RTPR up to 30 continuous cycles without reactivation of catalyst. The results demonstrated the economic feasibility of the utilization of developed RTPR for the efficient purification of pesticide polluted water. The prepared TiO₂ clay beads delivered 75.78% degradation of MCP under UV light with negligible catalyst loss. Application of W-TiO₂ coated clay beads filled RTPR for the degradation of MCP under sunlight, however, shows 32% higher degradation of MCP than the same system based on undoped TiO₂. The COD measurements of TiO₂ coated beads led to 73.75% COD reduction while W-TiO₂ resulted in 87.89% COD reduction. The GC-MS analysis confirms the efficient breakdown of complex MCP molecules into simpler hydrocarbons. This supports the promising application of clay beads as a support for the photocatalyst and proves its eco-friendly nature, excellent recyclability, catalyst holding capacity, and economic viability.

Keywords: immobilized clay beads, monocrotophos, recirculation type photocatalytic reactor, TiO₂

Procedia PDF Downloads 182

Authors: Lukas Munster, Pavel Bazant, Ivo Kuritka

Abstract:

Zinc oxide sub-micro particles and metallic silver nano particles (Ag/ZnO) were deposited on micro crystalline cellulose surface by a fast, simple and environmentally friendly one-pot microwave assisted solvo thermal synthesis in an open vessel system equipped with an external reflux cooler. In order to increase the interaction between the surface of cellulose and the precipitated Ag/ZnO particles, oxidized form of cellulose (cellulose dialdehyde, DAC) prepared by periodate oxidation of micro crystalline cellulose was added to the reaction mixture of Ag/ZnO particle precursors and untreated micro crystalline cellulose. The structure and morphology of prepared hybrid powder materials were analysed by X-ray diffraction (XRD), energy dispersive analysis (EDX), scanning electron microscopy (SEM) and nitrogen absorption method (BET). Microscopic analysis of the prepared materials treated by ultra-sonication showed that Ag/ZnO particles deposited on the cellulose/DAC sample exhibit increased adhesion to the surface of the cellulose substrate which can be explained by the DAC adhesive effect in comparison with the material prepared without DAC addition.

Keywords: microcrystalline cellulose, microwave synthesis, silver nanoparticles, zinc oxide sub-microparticles, cellulose dialdehyde

Procedia PDF Downloads 478

Authors: Opeyemi Atiba-Oyewo, Maurice S. Onya, Christian Wolkersdorfer

Abstract:

Nanostructure formation and characterization of eco-friendly banana peels nanosorbent are thoroughly described in this paper. The transformation of material during mechanical milling to enhance certain properties such as changes in microstructure and surface area to solve the current problems involving water pollution and water quality were studied. The mechanical milling was employed using planetary continuous milling machine and ethanol as process control agent, the sample were taken at time interval between 10 h to 30 h to examine the structural changes. The samples were characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infra-red (FTIR), Transmission electron microscopy (TEM) and Brunauer Emmett and teller (BET). Results revealed that the three typical structures with different grain-size, lattice strain and shapes were observed, and the deformation mechanisms in these structures were found to be different, further particles fracturing results to surface area increment which was confirmed by Brunauer Emmett and teller (BET) analysis. X-ray diffraction (XRD) shows high densities of dislocations in large crystallites, implying that dislocation slip is the dominant deformation mechanism. Scanning electron microscopy revealed the morphological properties of the materials at different milling time, nanostructure of the particles and fibres were confirmed by Transmission electron microscopy and FT-IR identified the functional groups responsible for its capacity to coordinate and remove metal ions, such as the carboxylic and amine groups at absorption bands of 1730 and 889 cm-1, respectively. However, the choice of this sorbent material for the sorption of any contaminants will depend on the composition of the effluent to be treated.

Keywords: banana peels, eco-friendly, mechanical milling, nanosorbent, nanostructure water quality

Procedia PDF Downloads 256

Authors: Shrikaant Kulkarni, Akshata Naik Nimbalkar

Abstract:

In this worki a method protocol has been developed for the synthesis of innovative Co3O4 material by using a method of chemical synthesis followed by calcination. The effect of calcination temperature on the morphology, structure and catalytic performance on material in question is investigated by using characterization tools like scanning electron microscopy (SEM), X-ray diffraction (XRD) spectroscopy and electrochemical techniques. The SEM images reveal that the morphology of the Co3O4 material undergoes a change from the rod to a beadlike shape on calcination at temperature of 700 °C. The XRD image shows that although the morphology of synthesized Co3O4 material exhibits a cubic phase but it differs in crystallinity depending upon morphology. Similarly spherical beadlike Co3O4 material has exhibited better activity than its rodlike counterpart which is reflected from electrochemical findings. Further, its performance in terms of bifunctional nature and hlods a lot much of promise as a excellent electrode material in the next generation batteries and fuel cells.

Keywords: bifunctional, next generation material, Co3O4, XRD

Procedia PDF Downloads 380

Authors: Tooba Aslam, Efthalia Chatzisymeon

Abstract:

UV-assisted irradiation technologies are well-established for water and wastewater treatment. UVC treatments are widely used at large-scale, while UVA irradiation has more often been applied in combination with a catalyst (e.g. TiO₂ or FeSO₄) in smaller-scale systems. A technical issue of these systems is the formation of fouling on the quartz sleeves that houses the lamps. This fouling can prevent complete irradiation, therefore reducing the efficiency of the process. This paper investigates the effects of operational parameters, such as the type of wastewater, irradiation source, H₂O₂ addition, and water pH on fouling formation and, ultimately, the treatment of municipal wastewater. Batch experiments have been performed at lab-scale while monitoring water quality parameters including: COD, TS, TSS, TDS, temperature, pH, hardness, alkalinity, turbidity, TOC, UV transmission, UV₂₅₄ absorbance, and metal concentrations. The residence time of the wastewater in the reactor was 5 days in order to observe any fouling formation on the quartz surface. Over this period, it was observed that chemical oxygen demand (COD) decreased by 30% and 59% during photolysis (Ultraviolet A) and photo-catalysis (UVA/Fe/H₂O₂), respectively. Higher fouling formation was observed with iron-rich and phosphorous-rich wastewater. The highest rate of fouling was developed with phosphorous-rich wastewater, followed by the iron-rich wastewater. Photo-catalysis (UVA/Fe/H₂O₂) had better removal efficiency than photolysis (UVA). This was attributed to the Photo-Fenton reaction, which was initiated under these operational conditions. Scanning electron microscope (SEM) measurements of fouling formed on the quartz sleeves showed that particles vary in size, shape, and structure; some have more distinct structures and are generally larger and have less compact structure than the others. Energy-dispersive X-ray spectroscopy (EDX) results showed that the major metals present in the fouling cake were iron, phosphorous, and calcium. In conclusion, iron-rich wastewaters are more suitable for UV-assisted treatment since fouling formation on quartz sleeves can be minimized by the formation of oxidizing agents during treatment, such as hydroxyl radicals.

Keywords: advanced oxidation processes, photo-fenton treatment, photo-catalysis, wastewater treatment

Procedia PDF Downloads 77

Authors: Matthew Ferguson, Tatyana Konkova, Ioannis Violatos

Abstract:

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

Keywords: additive manufacturing, direct energy deposition, electron back-scattered diffraction, finite element analysis, inconel 718, microstructure, optical microscopy, scanning electron microscopy, substrate-deposit interface region

Procedia PDF Downloads 204

Authors: Zohreh Derikvand

Abstract:

One new 2D metal-organic coordination polymer of Ni(II) namely [Ni2(ndc)2(DMSO)4(H2O)]n, where ndc = naphthalene-1,4-dicarboxylic acid and DMSO= dimethyl sulfoxide has been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. Compound 1 possesses a 2D layer structure constructed from dinuclear nickel(II) building blocks in which two crystallographically independent Ni2+ ions are bridged by ndc2– ligands and water molecule. The ndc2– ligands adopt μ3 bridging modes, linking the metal centers into a two-dimensional coordination framework. The two independent NiII cations are surrounded by dimethyl sulfoxide and naphthalene-1,4-dicarboxylate molecules in distorted octahedron geometry. In the crystal structures of 1 there are non-classical hydrogen bonding arrangements and C-H–π stacking interactions. Electrochemical behavior of [Ni2(ndc)2(DMSO)4(H2O)]n, (Ni-NDA) on the surface of carbon nanotube (CNTs) glassy carbon electrode (GCE) was described. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). Oxidation of fructose on the surface of modified electrode was investigated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) and the results showed that the Ni-NDA/CNTs film displays excellent electrochemical catalytic activities towards fructose oxidation.

Keywords: naphthalene-1, 4-dicarboxylic acid, crystal structure, coordination polymer, electrocatalysis, impedance spectroscopy

Procedia PDF Downloads 332

Authors: Mehran Bakhshi, Mohammad Raouf Hosseini, Mohammadhosein Rahimi

Abstract:

The cadmium sulfide nanoparticles were synthesized from the nickel-cadmium cake of a hydrometallurgical zinc producing plant and sodium sulfide as Cd²⁺ and S^-2 sources, respectively. Also, the synthesis process was performed by using the secretions of Bacillus licheniformis as bio-surfactant. Initially, in order to obtain a cadmium rich solution, two following steps were carried out: 1) Alkaline leaching for the removal of zinc oxide from the cake, and 2) acidic leaching to dissolve cadmium from the remained solid residue. Afterward, the obtained CdSO₄ solution was used for the nanoparticle biosynthesis. Nanoparticles were characterized by the energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) to confirm the formation of CdS crystals with cubic structure. Also, transmission electron microscopy (TEM) was applied to determine the particle sizes which were in 2-10 nm range. Moreover, the presence of the protein containing bio-surfactants was approved by using infrared analysis (FTIR). In addition, the absorbance below 400 nm confirms quantum particles’ size. Finally, it was shown that valuable CdS quantum dots could be obtained from the industrial waste products via environment-friendly biological approaches.

Keywords: biosynthesis, cadmium cake, cadmium sulfide, nanoparticle, zinc smelter

Procedia PDF Downloads 304

Authors: Irlana C. do Mar, Thayna A. Ferreira, Dayane S. Rezende, Bruno A. M. Figueira, José M. R. Mercury

Abstract:

This work presents a low-cost Mn starting material to synthesis manganese oxide octahedral molecular sieve with Mg²⁺ in the tunnel (Mg-OMS-1), based on the Mn residues from Carajás Mineral Province (Amazon, Brazil). After hydrothermal and cation exchange procedures, the Mn residues transformed to a single phase, Mg-OMS-1. The raw material and the synthesis processes were analyzed by means of X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Infrared spectroscopy (FTIR). The tunnel structure was synthesized hydrothermally at 180 °C for three days without impurities. According to the XRD analysis, the formation of crystalline Mg-OMS-1 was identified through reflections at 9.8º, 12º and 18º (2θ), as well as a thermal stability around 300 ºC. The SEM analysis indicated that the final product presents good crystallinity with a homogeneous size. In addition, an intense and diagnostic FTIR band was identified at 515 cm⁻¹ related to the MnO₆ octahedral stretching vibrations.

Keywords: Mn residues , Octahedral Molecular Sieve, Synthesis, Characterization

Procedia PDF Downloads 194

Authors: Ali Akbar Kazemi Asl, Mansour Rahsepar

Abstract:

Mesoporous carbon nanospheres (MCNs) with uniform particle size distribution having an average of 290 nm and large specific surface area (274.4 m²/g) were synthesized by a one-step hydrothermal method followed by the calcination process and then utilized as an enzyme-free glucose biosensor. Morphology, crystal structure, and porous nature of the synthesized nanospheres were characterized by scanning electron microscopy (SEM), X-Ray diffraction (XRD), and Brunauer–Emmett–Teller (BET) analysis, respectively. Also, the electrochemical performance of the MCNs@GCE electrode for the measurement of glucose concentration in alkaline media was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and chronoamperometry (CA). MCNs@GCE electrode shows good sensing performance, including a rapid glucose oxidation response within 3.1 s, a wide linear range of 0.026-12 mM, a sensitivity of 212.34 μA.mM⁻¹.cm⁻², and a detection limit of 25.7 μM with excellent selectivity.

Keywords: biosensor, electrochemical, glucose, mesoporous carbon, non-enzymatic

Procedia PDF Downloads 190

Authors: Ambrish Singh

Abstract:

The corrosion inhibition performance of pyran (AP) and benzimidazole (BI) derivatives on J55 steel in 3.5% NaCl solution saturated with CO₂ was investigated by electrochemical, weight loss, surface characterization, and theoretical studies. The electrochemical studies included electrochemical impedance spectroscopy (EIS), potentiodynamic polarization (PDP), electrochemical frequency modulation (EFM), and electrochemical frequency modulation trend (EFMT). Surface characterization was done using contact angle, scanning electron microscopy (SEM), and atomic force microscopy (AFM) techniques. DFT and molecular dynamics (MD) studies were done using Gaussian and Materials Studio softwares. All the studies suggested the good inhibition by the synthesized inhibitors on J55 steel in 3.5% NaCl solution saturated with CO₂ due to the formation of a protective film on the surface. Molecular dynamic simulation was applied to search for the most stable configuration and adsorption energies for the interaction of the inhibitors with Fe (110) surface.

Keywords: corrosion, inhibitor, EFM, AFM, DFT, MD

Procedia PDF Downloads 105

Authors: M. Mujahid, Omar A. Al-Hartomy

Abstract:

Ag-doped ZnO2 loaded on the Pt-carbon spheres have been synthesized and characterized by standard analytical techniques. i.e., UV-Vis spectroscopy, X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). In order to find the effect of loading of Ag doping on ZnO2, the concentration of Ag was varied from 0-3.5%. The XRD analysis showed that the obtained particles are anatase phase. The SEM images showed Ag-doped ZnO2 are loaded on the surface of the Pt-carbon spheres. The photocatalytic activity of the synthesized particles was tested by studying the degradation of methyl orange dye and 4-chlorophenol as a function of time on irradiation in aqueous suspension. Ag-doped ZnO2@Pt-carbon sphere particle with platinum concentration of 3.0 % showed the highest photocatalytic activity as compared to the other Ag concentrations for the degradation of methyl orange and 4-chlorophenol.

Keywords: Ag-ZnO2, Pt-carbon spheres, degradation, methyl orange, 4-chlorophenol

Procedia PDF Downloads 370

Authors: Temesgen Geremew

Abstract:

ZnO is currently receiving a lot of attention in the semiconductor industry due to its unique characteristics. ZnO is widely used in solar cells, heat-reflecting glasses, optoelectronic bias, and detectors. In this composition, we provide an overview of the ZnO thin flicks' packages, methods of characterization, and implicit operations. They consist of Transmission spectroscopy, Raman spectroscopy, Field emigration surveying electron microscopy, and X-ray diffraction. This review content also demonstrates how ZnO thin flicks function in electrical components for piezoelectric bias, optoelectronics, detectors, and renewable energy sources. Zinc oxide (ZnO) thin films offer a captivating tapestry of possibilities due to their unique blend of electrical, optical, and mechanical properties. This review delves into the realm of their potential applications and future prospects, highlighting the pivotal contributions of research endeavors aimed at tailoring their functionalities.

Keywords: Zinc oxide, raman spectroscopy, thin films, piezoelectric devices

Procedia PDF Downloads 86

Authors: Khadijat O. Abdulwahab, Mohammad A. Malik, Paul O’Brien, Grigore A. Timco, Floriana Tuna

Abstract:

The synthesis of spinel ferrite nanoparticles with a narrow size distribution is very crucial in their numerous applications including information storage, hyperthermia treatment, drug delivery, contrast agent in magnetic resonance imaging, catalysis, sensors, and environmental remediation. Ferrites have the general formula MFe2O4 (M = Fe, Co, Mn, Ni, Zn etc.) and possess remarkable electrical and magnetic properties which depend on the cations, method of preparation, size and their site occupancies. To the best of our knowledge, there are no reports on the use of a single source precursor to synthesise quaternary ferrite nanoparticles. Herein, we demonstrated the use of trimetallic iron pivalate cluster [CrCoFeO(O2CtBu)6(HO2CtBu)3] as a single source precursor to synthesise monodisperse cobalt chromium ferrite (FeCoCrO4) nanoparticles by the hot injection thermolysis method. The precursor was thermolysed in oleylamine, oleic acid, with diphenyl ether as solvent at its boiling point (260°C). The effect of concentration on the stoichiometry, phases or morphology of the nanoparticles was studied. The p-XRD patterns of the nanoparticles obtained at both concentrations were matched with cubic iron cobalt chromium ferrite (FeCoCrO4). TEM showed that a more monodispersed spherical ferrite nanoparticles of average diameter 4.0 ± 0.4 nm were obtained at higher precursor concentration. Magnetic measurements revealed that all the ferrite particles are superparamagnetic at room temperature. The nanoparticles were characterised by Powder X-ray Diffraction (p-XRD), Transmission Electron Microscopy (TEM), Inductively Coupled Plasma (ICP), Electron Probe Microanalysis (EPMA), Energy Dispersive Spectroscopy (EDS) and Super Conducting Quantum Interference Device (SQUID).

Keywords: quaternary ferrite nanoparticles, single source precursor, monodisperse, cobalt chromium ferrite, colloidal, hot injection thermolysis

Procedia PDF Downloads 275

Authors: Selma Hamimed, Abdelwaheb Chatti

Abstract:

The current study deals with the biological treatment of saline wastewaters generated by various agro-food industries using Yarrowia lipolytica. The ability of this yeast was studied on the mixture of olive mill wastewater and tuna wash processing wastewater. Results showed that the high proportion of olive mill wastewater in the mixture about (75:25) is the suitable one for the highest Y. lipolytica biomass production, reaching 11.3 g L⁻¹ after seven days. In addition, results showed significant removal of chemical oxygen demand (COD) and phosphorous of 97.49 % and 98.90 %, respectively. On the other hand, Y. lipolytica was found to be effective to desalinate all mixtures reaching a removal of 92.21 %. Moreover, the analytical results using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM) confirmed the biosorption of NaCl on the surface of the yeast as nanocrystals form with a size of 47.3 nm.

Keywords: nanocrystallization of NaCl, desalination, wastewater treatment, yarrowia lipolytica

Procedia PDF Downloads 187

Authors: L. Rozumová, J. Seidlerová

Abstract:

The aim of this paper was to study the sorption properties of a blast furnace sludge used as the sorbent. The sorbent was utilized for reduction of content of lead and zinc ions. Sorbent utilized in this work was obtained from metallurgical industry from process of wet gas treatment in iron production. The blast furnace sludge was characterized by X-Ray diffraction, scanning electron microscopy, and XRFS spectroscopy. Sorption experiments were conducted in batch mode. The sorption of metal ions in the sludge was determined by correlation of adsorption isotherm models. The adsorption of lead and zinc ions was best fitted with Langmuir adsorption isotherms. The adsorption capacity of lead and zinc ions was 53.8 mg.g^-1 and 10.7 mg.g^-1, respectively. The results indicated that blast furnace sludge could be effectively used as secondary material and could be also employed as a low-cost alternative for the removal of heavy metals ions from wastewater.

Keywords: blast furnace sludge, lead, zinc, sorption

Procedia PDF Downloads 302

Authors: Siva Prasad Peddi

Abstract:

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

Procedia PDF Downloads 469

Authors: Javiera Poblete, Fernando Gajardo, Katherina Fernandez

Abstract:

Graphene, and its derivatives such as graphene oxide (GO), are emerging nanoscopic materials, with interesting physical and chemical properties. From them, it is possible to develop three-dimensional macrostructures, such as aerogels, which are characterized by a low density, high porosity, and large surface area, having a promising structure for the development of materials. The use of GO as a precursor of these structures provides a wide variety of materials, which can be developed as a result of the functionalization of their oxygenated groups, with specific compounds such as polyethylene glycol (PEG). The synthesis of aerogels of GO-PEG for non-covalent interactions has not yet been widely reported, being of interest due to its feasible escalation and economic viability. Thus, this work aims to develop a non-covalently functionalized GO-PEG aerogels and characterize them physicochemically. In order to get this, the GO was synthesized from the modified hummers method and it was functionalized with the PEG by polymer-assisted GO gelation (crosslinker). The gelation was obtained for GO solutions (10 mg/mL) with the incorporation of PEG in different proportions by weight. The hydrogel resulting from the reaction was subsequently lyophilized, to obtain the respective aerogel. The material obtained was chemically characterized by analysis of Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray diffraction (XRD), and its morphology by scanning electron microscopy (SEM) images; as well as water absorption tests. The results obtained showed the formation of a non-covalent aerogel (FTIR), whose structure was highly porous (SEM) and with a water absorption values greater than 50% g/g. Thus, a methodology of synthesis for GO-PEG was developed and validated.

Keywords: aerogel, graphene oxide, polyethylene glycol, synthesis

Procedia PDF Downloads 127

Authors: Magdalena Blachnio, Viktor Bogatyrov, Mariia Galaburda, Anna Derylo-Marczewska

Abstract:

Agricultural waste materials from traditional oil mill and after extraction of natural raw materials in supercritical conditions were used for the preparation of carbon nanomaterials (activated carbons) by two various methods. Chemical activation using acetic acid and physical activation with a gaseous agent (carbon dioxide) were chosen as mild and environmentally friendly ones. The effect of influential factors: type of raw material, temperature and activation agent on the porous structure characteristics of the materials was discussed by using N₂ adsorption/desorption isotherms at 77 K. Furthermore scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were employed to examine the physicochemical properties of the obtained sorbents. Selection of a raw material and an optimization of the conditions of the synthesis process, allowed to obtain the cheap sorbents with a targeted distribution of pores enabling effective adsorption of the model organic pollutants carried out in the multicomponent systems. Adsorption behavior (capacity and rate) of the chosen activated carbons was estimated by utilizing Crystal violet (CV), 4-chlorophenoxyacetic acid (4-CPA), 2.4-dichlorophenoxyacetic acid (2.4-D) as the adsorbates. Both rate and adsorption capacity of the organics on the sorbents evidenced that the activated carbons could be effectively used in sewage treatment plants. The mechanisms of organics adsorption were studied and correlated with activated carbons properties.

Keywords: activated carbon, adsorption equilibrium, adsorption kinetics, organics adsorption

Procedia PDF Downloads 179

Authors: Sarmistha Baruah, Akshai Kumar, Nageswara Rao Peela

Abstract:

The global energy crisis due to the dependence on fossil fuels and its limited reserves as well as environmental pollution are key concerns to the research communities. However, the implementation of alcohol-based fuel cells such as methanol is anticipated as a reliable source of future energy technology due to their high energy density, environment friendliness, ease of storage, transportation, etc. To drive the anodic methanol oxidation reaction (MOR) in direct methanol fuel cells (DMFCs), an active and long-lasting catalyst is necessary for efficient energy conversion from methanol. Recently, transition metal-zeolite-based materials have been considered versatile catalysts for a variety of industrial and lab-scale processes. Large specific surface area, well-organized micropores, and adjustable acidity/basicity are characteristics of zeolites that make them excellent supports for immobilizing small-sized and highly dispersed metal species. Significant advancement in the production and characterization of well-defined metal clusters encapsulated within zeolite matrix has substantially expanded the library of materials available, and consequently, their catalytic efficacy. In this context, we developed bimetallic Ni-Co catalysts encapsulated within LTA (also known as 4A) zeolite via a method combined with the in-situ encapsulation of metal species using hydrothermal treatment followed by a chemical reduction process. The prepared catalyst was characterized using advanced characterization techniques, such as X-ray diffraction (XRD), field emission transmission electron microscope (FETEM), field emission scanning electron microscope (FESEM), energy dispersive X-ray (EDX), and X-ray photoelectron spectroscopy (XPS). The electrocatalytic activity of the catalyst for MOR was carried out in an alkaline medium at room temperature using techniques such as cyclic voltammetry (CV), and chronoamperometry (CA). The resulting catalyst exhibited better catalytic activity of 12.1 mA cm-2 at 1.12 V vs Ag/AgCl and retained remarkable stability (~77%) even after 1000 cycles CV test for the electro-oxidation of methanol in alkaline media without any significant microstructural changes. The high surface area, better Ni-Co species integration in the zeolite, and the ample amount of surface hydroxyl groups contribute to highly dispersed active sites and quick analyte diffusion, which provide notable MOR kinetics. Thus, this study will open up new possibilities to develop a noble metal-free zeolite-based electrocatalyst due to its simple synthesis steps, large-scale fabrication, improved stability, and efficient activity for DMFC application.

Keywords: alkaline media, bimetallic, encapsulation, methanol oxidation reaction, LTA zeolite.

Procedia PDF Downloads 66

Authors: M. Adabi, A. Amadeh

Abstract:

Electrodeposition is known as a relatively economical and simple technique commonly used for preparation of metallic and composite coatings. Electrodeposited composite coatings produced by dispersion of particles into the metal matrix show better properties than pure metallic coatings. In recent years, many researches were carried out on Ni matrix coatings reinforced by ceramic particles such as Ni-SiC, Ni-Al2O3, Ni-WC, Ni-CeO2, Ni-ZrO2, Ni-TiO2 to improve their corrosion and wear resistance. However, little effort has been made on incorporation of metal particles into Ni matrix. Therefore, the aim of this work was to produce Ni–Al composite coating on 6061 aluminum alloy by pulse plating and to investigate the effects of electrodeposition parameters, e.g. concentration Al particles in the electrolyte and current density, on composition and corrosion resistance of the composite coatings. The morphology and corrosion behavior of the coated 6061 Al alloys were studied by means of scanning electron microscope (SEM) equipped with energy dispersive X-ray spectrometer (EDS) and potentiodynamic polarization method, respectively. The results indicated that the addition of Al particles up to 50 g L-1 increased the amount of co-deposited Al particles in nickel matrix. It is also observed that the incorporation of Al particles decreased with increasing current density. Meanwhile, the corrosion resistance of the coatings shows an increment by increasing the content of Al particles into nickel matrix.

Keywords: Ni-Al composite coating, current density, corrosion resistance

Procedia PDF Downloads 487

Authors: Folorunso Omoniyi, Peter Olubambi, Rotimi Sadiku

Abstract:

Thermal barrier coating (TBC) system is used in both aero engines and other gas turbines to offer oxidation protection to superalloy substrate component. In the present work, it shows the ability of a new fabrication technique to develop rapidly new coating composition and microstructure. The compact powders were prepared by Powder Metallurgy method involving powder mixing and the bond coat was synthesized through the application of Spark Plasma Sintering (SPS) at 10500C to produce a fully dense (97%) NiCrAl bulk samples. The influence of sintering temperature on the hardness of NiCrAl, done by Micro Vickers hardness tester, was investigated. And Oxidation test was carried out at 1100oC for 20h, 40h, and 100h. The resulting coat was characterized with optical microscopy, scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDAX) and x-ray diffraction (XRD). Micro XRD analysis after the oxidation test revealed the formation of protective oxides and non-protective oxides.

Keywords: high-temperature oxidation, powder metallurgy, spark plasma sintering, thermal barrier coating

Procedia PDF Downloads 508

Authors: Muhammad Arshad, Ghulam Hussain Bhatti, Abdul Qayyum

Abstract:

Zinc-doped silica oxide nanoparticles having size 7.93nm were synthesized by the deposition precipitation method by using different solvents (acetonitrile, n-hexane, isoamylalchol). Biological potential such as antibacterial activities against Bacillussubtilusand Escherichia coli, and antifungal activities against Candida parapsilosis and Aspergilusniger were also investigated by Disc diffusion method. Different characterizations techniques including Fournier Transmission Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Thermo-gravimeteric Analysis (TGA), Atomic forced microscopy (AFM), and Dynamic Light Scattering (DLS) were used. FT-IR characterization confirmed the presence of metal oxide bond (SiO2) while XRD showed the hexagonal structure. SEM and TEM characterization showed the morphology of nanoparticles. AFM study showed good particle size distribution as depicted by a histogram. DLS study showed the gradual decease in the size of nanoparticles from 24.86nm to 13.24 nm. Highest antibacterial activities revealed by acetonitrile solvents (6%and 4.5%) followed by isoamylalchol (3% and 2.4%) while n-hexane solvent showed the lowest activity (2%and 1%) respectively. Higher antifungal activities exhibited by n-hexane (0.34 % and 0.43%) followed by isoamylalchol (0.27% and 0.19%) solvent while acetonitrile (0.21% and 0.17%) showed least activity respectively. Statistical analysis by using one-way ANOVA also indicated the significant results of both biological activities.

Keywords: nanoparticles, precipitation methods, antibacterial, antifungal, characterizations

Procedia PDF Downloads 207

Authors: Fernando G. Torres, Donna M. Ebenstein, Monica Merino

Abstract:

Most fish are covered by a protective external armour. The characteristics of these armours depend on the individual elements that form them, such as scales, scutes or dermal plates. In this work, we assess the properties of two different types of protective elements: scales from A. gigas and dermal plates from P. pardalis. A. Gigas and P. Pardalis are two Amazonian fish with a rather prehistoric aspect. They have large scales and dermal plates that form two different types of protective body armours. Although both scales and dermal plates are formed by collagen and hydroxyapatite, their structures display remarkable differences. The structure and composition of the samples were assessed by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). Morphology studies were carried out using a Scanning Electron Microscopy (SEM). Nanoindentation tests were performed to measure the reduced moduli in A. gigas scales and P. pardalis plates. The similarities and differences between scales and dermal plates are discussed based on the experimental results. Both protective armours are designed to be lightweight, flexible and tough. A. Gigas scales are are light laminated composites, while P. pardalis dermal plates show a sandwich like structure with dense outer layers and a porous inner matrix. It seems that the armour of P. pardalis is more suited for a bottom-dwelling fish and allows for protection against predators. The scales from A. Gigas are more adapted to give protection to a swimming fish. The information obtained from these studies is also important for the development of bioinspired nanocomposites, with potential applications in the biomedical field.

Keywords: pterygoplichthys pardalis, dermal plates arapaima gigas, fish scales

Procedia PDF Downloads 392

Authors: Uttam Kumar Ghorai, Madhupriya Samanta, Subhajit Saha, Swati Das, Nilesh Mazumder, Kalyan Kumar Chattopadhyay

Abstract:

Organic semiconductors have gained potential interest in the last few decades for their significant contributions in the various fields such as solar cell, non-volatile memory devices, field effect transistors and light emitting diodes etc. The most important advantages of using organic materials are mechanically flexible, light weight and low temperature depositing techniques. Recently with the advancement of nanoscience and technology, one dimensional organic and inorganic nanostructures such as nanowires, nanorods, nanotubes have gained tremendous interests due to their very high aspect ratio and large surface area for electron transport etc. Among them, self-assembled organic nanostructures like Copper, Zinc Phthalocyanine have shown good transport property and thermal stability due to their π conjugated bonds and π-π stacking respectively. Field emission properties of inorganic and carbon based nanostructures are reported in literatures mostly. But there are few reports in case of cold cathode emission characteristics of organic semiconductor nanostructures. In this work, the authors report the field emission characteristics of chemically and physically synthesized Copper Phthalocyanine (CuPc) nanostructures such as nanowires, nanotubes and nanotips. The as prepared samples were characterized by X-Ray diffraction (XRD), Ultra Violet Visible Spectrometer (UV-Vis), Fourier Transform Infra-red Spectroscopy (FTIR), and Field Emission Scanning Electron Microscope (FESEM) and Transmission Electron Microscope (TEM). The field emission characteristics were measured in our home designed field emission set up. The registered turn-on field and local field enhancement factor are found to be less than 5 V/μm and greater than 1000 respectively. The field emission behaviour is also stable for 200 minute. The experimental results are further verified by theoretically using by a finite displacement method as implemented in ANSYS Maxwell simulation package. The obtained results strongly indicate CuPc nanostructures to be the potential candidate as an electron emitter for field emission based display device applications.

Keywords: organic semiconductor, phthalocyanine, nanowires, nanotubes, field emission

Procedia PDF Downloads 502

Authors: Djamil Guettiche, Ahmed Mekki, Tighilt Fatma-Zohra, Rachid Mahmoud

Abstract:

The aim of this study was to synthesize and characterize conducting polymer composites of polypyrrole and graphene, including pristine and surface-treated graphene (PPy/GO, PPy/rGO, and PPy/rGO-ArCOOH), for use as sensitive elements in a homemade chemiresistive module for on-line detection of nitrogen oxides vapors. The chemiresistive module was prepared, characterized, and evaluated for performance. Structural and morphological characterizations of the composite were carried out using FTIR, Raman spectroscopy, and XRD analyses. After exposure to NO and NO₂ gases in both static and dynamic modes, the sensitivity, selectivity, limit of detection, and response time of the sensor were determined at ambient temperature. The resulting sensor showed high sensitivity, selectivity, and reversibility, with a low limit of detection of 1 ppm. A composite of polypyrrole and graphene functionalized with aryl 4-carboxy benzene diazonium salt was synthesized and characterized using FTIR, scanning electron microscopy, transmission electron microscopy, UV-visible, and X-ray diffraction. The PPy-rGOArCOOH composite exhibited a good electrical resistance response to NO₂ at room temperature and showed enhanced NO₂-sensing properties compared to PPy-rGO thin films. The selectivity and stability of the NO₂ sensor based on the PPy/rGO-ArCOOH nanocomposite were also investigated.

Keywords: conducting polymers, surface treated graphene, diazonium salt, polypyrrole, Nitrogen oxide sensing

Procedia PDF Downloads 78

Authors: Amir Shafiee Kisomi, Mehrdad Mofidi

Abstract:

Nowadays, fuel cells as a promising alternative for power source have been widely studied owing to their security, high energy density, low operation temperatures, renewable capability and low environmental pollutant emission. The nanoparticles of core-shell type could be widely described in a combination of a shell (outer layer material) and a core (inner material), and their characteristics are greatly conditional on dimensions and composition of the core and shell. In addition, the change in the constituting materials or the ratio of core to the shell can create their special noble characteristics. In this study, a fast technique for the fabrication of a Pd-Co/G/GCE modified electrode is offered. Thermal decomposition reaction of cobalt (II) formate salt over the surface of graphene/glassy carbon electrode (G/GCE) is utilized for the synthesis of Co nanoparticles. The nanoparticles of Pd-Co decorated on the graphene are created based on the following method: (1) Thermal decomposition reaction of cobalt (II) formate salt and (2) the galvanic replacement process Co by Pd2+. The physical and electrochemical performances of the as-prepared Pd-Co/G electrocatalyst are studied by Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDS), Cyclic Voltammetry (CV), and Chronoamperometry (CHA). Galvanic replacement method is utilized as a facile and spontaneous approach for growth of Pd nanostructures. The Pd-Co/G is used as an anode catalyst for ethanol oxidation in alkaline media. The Pd-Co/G not only delivered much higher current density (262.3 mAcm-2) compared to the Pd/C (32.1 mAcm-2) catalyst, but also demonstrated a negative shift of the onset oxidation potential (-0.480 vs -0.460 mV) in the forward sweep. Moreover, the novel Pd-Co/G electrocatalyst represents large electrochemically active surface area (ECSA), lower apparent activation energy (Ea), higher levels of durability and poisoning tolerance compared to the Pd/C catalyst. The paper demonstrates that the catalytic activity and stability of Pd-Co/G electrocatalyst are higher than those of the Pd/C electrocatalyst toward ethanol oxidation in alkaline media.

Keywords: thermal decomposition, nanostructures, galvanic replacement, electrocatalyst, ethanol oxidation, alkaline media

Procedia PDF Downloads 153

Authors: Ubeyd Toçoğlu, Miraç Alaf, Hatem Akbulut

Abstract:

We present a work which was conducted in order to improve the cycle life of silicon based lithium ion battery anodes by utilizing novel composite structure. In this study, carbon coated nano sized (50-100 nm) silicon particles were embedded into Graphene/MWCNT silicon matrix to produce free standing silicon based electrodes. Also, conventional Si powder anodes were produced from Si powder slurry on copper current collectors in order to make comparison of composite and conventional anode structures. Free –standing composite anodes (binder-free) were produced via vacuum filtration from a well dispersion of Graphene, MWCNT and carbon coated silicon powders. Carbon coating process of silicon powders was carried out via microwave reaction system. The certain amount of silicon powder and glucose was mixed under ultrasonication and then coating was conducted at 200 °C for two hours in Teflon lined autoclave reaction chamber. Graphene which was used in this study was synthesized from well-known Hummers method and hydrazine reduction of graphene oxide. X-Ray diffraction analysis and RAMAN spectroscopy techniques were used for phase characterization of anodes. Scanning electron microscopy analyses were conducted for morphological characterization. The electrochemical performance tests were carried out by means of galvanostatic charge/discharge, cyclic voltammetry and electrochemical impedance spectroscopy.

Keywords: graphene, Li-Ion, MWCNT, silicon

Procedia PDF Downloads 258

Authors: Bourfaa Fouzia, Meryem Lamri Zeggar, Adjimi Amel, Mohammed Salah Aida, Nadir Attaf

Abstract:

Semiconductor photocatalysts such as ZnO has attracted much attention in recent years due to their various applications for the degradation of organic pollutants in water, air and in dye sensitized photovoltaic solar cell. In the present work, ZnO thin films were prepared by ultrasonic spray pyrolysis by using different precursors namely: Acetate, chloride and zinc nitrate in order to investigate their influence on ZnO photocatalytic activity. The films crystalline structure was studied by mean of X-ray diffraction measurements (XRD) and the films surface morphology by Scanning Electron Microscopy (SEM). The films optical properties were studied by mean of UV–visible spectroscopy. The prepared films were tested for the degradation of the red reactive dye largely used in textile industry. As a result, we found that the zinc nitrate is the best precursor to prepare ZnO thin films suitable for a good photocatalytic activity.

Keywords: precursor, thins films, spray pyrolysis, zinc oxide

Procedia PDF Downloads 328

Authors: Escada A. L. A., Pereira C. A., Jorge A. O. C., Alves Claro A. P. R.

Abstract:

In the present work, a susceptibility and efficacy of the Ti–7.5Mo alloy nanotube and Ti–7.5Mo alloy to bacterial biofilm formation after surface treatment was evaluated. The Ti–7.5Mo alloy was obtained in arc furnace under an argon atmosphere. Ingots were then homogenized under vacuum at 1100 ◦C for 86.4 ks to eliminate chemical segregation and after cold worked discs were cutting. Nanotubes were processed using anodic oxidation in 0.25% NH4F electrolyte solution. Biofilms were grown in discs immersed in sterile brain heart infusion broth (BHI) containing 5% sucrose, inoculated with microbial suspension (106 cells/ml) and incubated for 5 days. Next, the discs were placed in tubes with sterile physiological solution 0.9% sodium chloride (NaCl) and sonicated for to disperse the biofilms. Tenfold serial dilutions were carried and aliquots seeded in selective agar, which were then incubated for 48 h. Then, the numbers CFU/ml (log 10) were counted and analyzed statistically. Scanning electron microscopy (SEM) on discs with biofilms groupswas performed, atomic force microscope (AFM) and contact angle. The results show that there is no difference in bacterial adhesion between Ti–7.5Mo alloy nanotube pure titanium and Ti–7.5Mo alloy.

Keywords: biofilm, titanium alloy, brain heart infusion, scanning electron microscopy

Procedia PDF Downloads 318