Search results for: Coherent Anti-Stokes Raman Spectroscopy

Authors: Sara Khamseh, Kambiz Javanruee, Hamid Khorsand

Abstract:

Plenty of metallic materials are used for biomedical applications like hip joints and screws. Besides, it is reported that metal platforms such as stainless steel show significant deterioration because of wear and friction. The surface of metal substrates has been coated with a variety of multicomponent coatings to prevail these problems. The carbon-based multicomponent coatings such as metal-added amorphous carbon and diamond coatings are crucially important because of their remarkable tribological performance and chemical stability. In the current study, H-D contained Nb: (a-C) multicomponent coatings (H-D: hexagonal diamond, a-C: amorphous carbon) coated on A 304 steel substrates using an unbalanced magnetron (UBM) sputtering system. The effects of Nb and H-D content and ID/IG ratio on microstructure, mechanical and tribological characteristics of (Nb: H-D: a-C) composite coatings were investigated. The results of Raman spectroscopy represented that a-C phase with a Graphite-like structure (GLC with high value of sp2 carbon bonding) is formed, and its domain size increased with increasing Nb content of the coatings. Moreover, the Nb played a catalyst for the formation of the H-D phase. The nanoindentation hardness value of the coatings ranged between ~17 to ~35 GPa and (Nb: H-D: a-C) composite coatings with more H-D content represented higher hardness and plasticity index. It seems that the existence of extra-hard H-D particles straightly increased hardness. The tribological performance of the coatings was evaluated using the pin-on-disc method under the wet environment of SBF (Simulated Body Fluid). The COF value of the (Nb: H-D: a-C) coatings decreased with an increasing ID/IG ratio. The lower coefficient of friction is a result of the lamelliform array of graphitic domains. Also, the wear rate of the coatings decreased with increasing H-D content of the coatings. Based on the literature, a-C coatings with high hardness and H3/E2 ratio represent lower wear rates and better tribological performance. According to the nanoindentation analysis, hardness and H3/E2 ratio of (Nb: H-D: a-C) multicomponent coatings increased with increasing H-D content, which in turn decreased the wear rate of the coatings. The mechanical and tribological potency of (Nb: H-D: a-C) composite coatings on A 304 steel substrates paved the way for the development of innovative advanced coatings to ameliorate the performance of A 304 steel for biomedical applications.

Keywords: COF, mechanical properties, (Nb: H-D: a-C) coatings, wear rate

Procedia PDF Downloads 103

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

Abstract:

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

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

Procedia PDF Downloads 333

Authors: Hayder Raad Hafuze, Munqith Saleem Dawood, Jamal Abdul Jabbar

Abstract:

The effect of using both ultrasounds with laser in medical imaging of the biological tissue has been studied in this paper. Different wave lengths of incident laser light (405 nm, 532 nm, 650 nm, 808 nm and 1064 nm) were used with different ultrasound frequencies (1MHz and 3.3MHz). The results showed that, the change of acoustic intensity enhance the laser penetration of the tissue for different thickness. The existence of the ideal Raman-Nath diffraction pattern were investigated in terms of phase delay and incident angle.

Keywords: tissue, laser, ultrasound, effect, imaging

Procedia PDF Downloads 433

Authors: Peter Thissen

Abstract:

In this work, we report about the influence of the chemical potential of water on the carbonation reaction of wollastonite (CaSiO3) as model surface of cement and concrete. Total energy calculations based on density functional theory (DFT) combined with kinetic barrier predictions based on nudge elastic band (NEB) method show that the exposure of the water-free wollastonite surface to CO2 results in a barrier-less carbonation. CO2 reacts with the surface oxygen and forms carbonate (CO32-) complexes together with a major reconstruction of the surface. The reaction comes to a standstill after one carbonate monolayer has been formed. In case one water monolayer is covering the wollastonite surface, the carbonation is no more barrier-less, yet ending in a localized monolayer. Covered with multilayers of water, the thermodynamic ground state of the wollastonite completely changes due to a metal-proton exchange reaction (MPER, also called early stage hydration) and Ca2+ ions are partially removed from solid phase into the H2O/wollastonite interface. Mobile Ca2+ react again with CO2 and form carbonate complexes, ending in a delocalized layer. By means of high resolution time-of-flight secondary-ion mass-spectroscopy images (ToF-SIMS), we confirm that hydration can lead to a partially delocalization of Ca2+ ions on wollastonite surfaces. Finally, we evaluate the impact of our model surface results by means of Low Energy Ion Scattering (LEIS) spectroscopy combined with careful discussion about the competing reactions of carbonation vs. hydration.

Keywords: Calcium-silicate, carbonation, hydration, metal-proton exchange reaction

Procedia PDF Downloads 363

Authors: Nadia Hammouda, Kamel Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, seawater

Procedia PDF Downloads 417

Authors: Héctor González Espinosa, Ricardo Ivan Cordova Chávez, Alejandra Contreras Ramos, Itzia Irene Padilla Martínez, José Guadalupe Trujillo Ferrara, Marvin Antonio Soriano Ursúa

Abstract:

Boronic acids are able to create diester bonds with carbohydrates because of their hydroxyl groups; in nature, there are some organoborates with these characteristics, such as the calcium fructoborate, formed by the union of two fructose molecules and a boron atom, synthesized by plants. In addition, it has been observed that, in animal cells only the compounds with cis-diol functional groups are capable of linking to boric or boronic acids. The formation of these organoboron compounds could impair the physical and chemical properties of the precursors, even their acute toxicity. In this project, two carbohydrate-derived boron-containing compounds from D-fructose and D-arabinose and phenylboronic acid are analyzed by different spectroscopy techniques such as Raman, Infrared with Fourier Transform Infrared (FT-IR), Nuclear Magnetic Resonance (NMR) and X-ray diffraction crystallography to describe their chemical characteristics. Also, an acute toxicity test was performed to determine their LD50 using the Lorke’s method. It was confirmed by multiple spectra the formation of the adducts by the generation of the diester bonds with a β-D-pyranose of fructose and arabinose. The most prominent findings were the presence of signals corresponding to the formation of new bonds, like the stretching of B-O bonds, or the absence of signals of functional groups like the hydroxyls presented in the reagents used for the synthesis of the adducts. The NMR spectra yielded information about the stereoselectivity in the synthesis reaction, observed by the interaction of the protons and their vicinal atoms in the anomeric and second position carbons; but also, the absence of a racemic mix by the finding of just one signal in the range for the anomeric carbon in the 13C NMR spectra of both adducts. The acute toxicity tests by the Lorke’s method showed that the LD50 value for both compounds is 1265 mg/kg. Those results let us to propose these adducts as highly safe agents for further biological evaluation with medical purposes.

Keywords: acute toxicity, adduct, boron, carbohydrate, diester bond

Procedia PDF Downloads 63

Authors: Chor Nejmeddine, Ines Ben Omrane, Mohamed Abdelwahed

Abstract:

In this paper, we present a posteriori analysis of the discretization of the heat equation by spectral element method. We apply Euler's implicit scheme in time and spectral method in space. We propose two families of error indicators, both of which are built from the residual of the equation and we prove that they satisfy some optimal estimates. We present some numerical results which are coherent with the theoretical ones.

Keywords: heat equation, spectral elements discretization, error indicators, Euler

Procedia PDF Downloads 306

Authors: Nadia Hammouda, K. Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, sea water

Procedia PDF Downloads 481

Authors: Abdullah Faqihi, John Hedley

Abstract:

Biosensors play a significant role in the healthcare sectors, scientific and technological progress. Developing electrodes that are easy to manufacture and deliver better electrochemical performance is advantageous for diagnostics and biosensing. They can be implemented extensively in various analytical tasks such as drug discovery, food safety, medical diagnostics, process controls, security and defence, in addition to environmental monitoring. Development of biosensors aims to create high-performance electrochemical electrodes for diagnostics and biosensing. A biosensor is a device that inspects the biological and chemical reactions generated by the biological sample. A biosensor carries out biological detection via a linked transducer and transmits the biological response into an electrical signal; stability, selectivity, and sensitivity are the dynamic and static characteristics that affect and dictate the quality and performance of biosensors. In this research, a developed experimental study for laser scribing technique for graphene oxide inside a vacuum chamber for processing of graphene oxide is presented. The processing of graphene oxide (GO) was achieved using the laser scribing technique. The effect of the laser scribing on the reduction of GO was investigated under two conditions: atmosphere and vacuum. GO solvent was coated onto a LightScribe DVD. The laser scribing technique was applied to reduce GO layers to generate rGO. The micro-details for the morphological structures of rGO and GO were visualised using scanning electron microscopy (SEM) and Raman spectroscopy so that they could be examined. The first electrode was a traditional graphene-based electrode model, made under normal atmospheric conditions, whereas the second model was a developed graphene electrode fabricated under a vacuum state using a vacuum chamber. The purpose was to control the vacuum conditions, such as the air pressure and the temperature during the fabrication process. The parameters to be assessed include the layer thickness and the continuous environment. Results presented show high accuracy and repeatability achieving low cost productivity.

Keywords: laser scribing, lightscribe DVD, graphene oxide, scanning electron microscopy

Procedia PDF Downloads 120

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 437

Authors: S. V. Prabhakar Vattikuti, Chan Byon

Abstract:

In this paper, we report a facile synthetic strategy of randomly disturbed Bi₂S₃ nanorods on WS₂ nanosheets, which are synthesized via a controlled hydrothermal method without surfactant under an inert atmosphere. We developed a simple hydrothermal method for the formation of heterostructured of Bi₂S₃/WS₂ with a large scale (>95%). The structural features, composition, and morphology were characterized by XRD, SEM-EDX, TEM, HRTEM, XPS, UV-vis spectroscopy, N₂ adsorption-desorption, and TG-DTA measurements. The heterostructured Bi₂S₃/WS₂ composite has significant photocatalytic efficiency toward the photodegradation of organic dye. The time-dependent UV-vis absorbance spectroscopy measurement was consistent with the enhanced photocatalytic degradation of rhodamine B (RhB) under visible light irradiation with the diminishing carrier recombination for the Bi₂S₃/WS₂ photocatalyst. Due to their marked synergistic effects, the supported Bi₂S₃ nanorods on WS₂ nanosheet heterostructures exhibit significant visible-light photocatalytic activity and stability for the degradation of RhB. A possible reaction mechanism is proposed for the Bi₂S₃/WS₂ composite.

Keywords: photocatalyst, heterostructures, transition metal disulfides, organic dye, nanorods

Procedia PDF Downloads 296

Authors: N. Hammouda, K. Belmokre

Abstract:

The paints are used extensively today in the industry to protect the metallic structures of the aggressive environments. This work is devoted to the study of corrosion resistance and aging behavior of a paint coating providing external protection for oil tankers. To avoid problems related to corrosion of these vessels, two protection modes are provided: An electro chemical active protection (cathodic protection of the hull). A passive protection by external painting. Investigations are conducted using stationary and non-stationary electro chemical tools such as electro chemical impedance spectroscopy has allowed us to characterize the protective qualities of these films. The application of the EIS on our damaged in-situ painting shows the existence of several capacitive loops which is an indicator of the failure of our tested paint. Microscopic analysis (micrograph) helped bring essential elements in understanding the degradation of our paint condition and immersion training corrosion products.

Keywords: epoxy paints, electrochemical impedance spectroscopy, corrosion mechanisms, seawater

Procedia PDF Downloads 391

Authors: Nadia Hammouda, Kamel Belmokre

Abstract:

Organic coatings are widely employed in the corrosion protection of most metal surfaces, particularly steel. They provide a barrier against corrosive species present in the environment, due to their high resistance to oxygen, water and ions transport. This study focuses on the evaluation of corrosion protection performance of epoxy paint on the carbon steel surface in sea water by Electrochemical Impedance Spectroscopy (EIS). The electrochemical behavior of painted surface was estimated by EIS parameters that contained paint film resistance, paint film capacitance and double layer capacitance. On the basis of calculation using EIS spectrums it was observed that pore resistance (Rpore) decreased with the appearance of doubled layer capacitance (Cdl) due to the electrolyte penetration through the film. This was further confirmed by the decrease of diffusion resistance (Rd) which was also the indicator of the deterioration of paint film protectiveness.

Keywords: epoxy paints, carbon steel, electrochemical impedance spectroscopy, corrosion mechanisms, sea water

Procedia PDF Downloads 374

Authors: Theo H. G. Moundzounga

Abstract:

Arsenic and 2-chlorophenol are priority pollutants that pose serious health threats to humans and ecology. An electrochemical sensor, based on graphitic carbon nitride (g-C₃N₄) and carbon dots (CDs), was fabricated and used for the determination of arsenic and 2-chlorophenol. The g-C₃N₄/CDs nanocomposite was prepared via microwave irradiation heating method and was dropped-dried on the surface of the glassy carbon electrode (GCE). Transmission electron microscopy (TEM), X-ray diffraction (XRD), photoluminescence (PL), Fourier transform infrared spectroscopy (FTIR), UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS) were used for the characterization of structure and morphology of the nanocomposite. Electrochemical characterization was done by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrochemical behaviors of arsenic and 2-chlorophenol on different electrodes (GCE, CDs/GCE, and g-C₃N₄/CDs/GCE) was investigated by differential pulse voltammetry (DPV). The results demonstrated that the g-C₃N₄/CDs/GCE significantly enhanced the oxidation peak current of both analytes. The analytes detection sensitivity was greatly improved, suggesting that this new modified electrode has great potential in the determination of trace level of arsenic and 2-chlorophenol. Experimental conditions which affect the electrochemical response of arsenic and 2-chlorophenol were studied, the oxidation peak currents displayed a good linear relationship to concentration for 2-chlorophenol (R²=0.948, n=5) and arsenic (R²=0.9524, n=5), with a linear range from 0.5 to 2.5μM for 2-CP and arsenic and a detection limit of 2.15μM and 0.39μM respectively. The modified electrode was used to determine arsenic and 2-chlorophenol in spiked tap and effluent water samples by the standard addition method, and the results were satisfying. According to the measurement, the new modified electrode is a good alternative as chemical sensor for determination of other phenols.

Keywords: electrochemistry, electrode, limit of detection, sensor

Procedia PDF Downloads 144

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 429

Authors: Andile Mkhohlakali, Tien-Chien Jen, James Tshilongo, Happy Mabowa

Abstract:

Among different parameters, oxygen is one of the most important analytes of interest, dissolved oxygen (DO) concentration is very crucial and significant for various areas of physical, chemical, and environmental monitoring. Herein we report oxygen-sensitive luminophores -based lanthanum(III) trifluoromethanesulfonate), [La]³⁺ was encapsulated into SiO₂-based xerogel matrix. The nanosensor is composed of organically modified silica nanoparticles, doped with the luminescent oxygen–sensitive lanthanum(III) trifluoromethanesulfonate complex. The precursor materials used for sensing film were triethyl ethoxy silane (TEOS) and (3-Mercaptopropyltriethoxysilane) (MPTMS- TEOS) used for SiO2-baed matrices. Brunauer–Emmett–Teller (BET), and BJH indicate that the SiO₂ transformed from microporous to mesoporous upon the addition of La³⁺ luminophore with increased surface area (SBET). The typical amorphous SiO₂ based xerogels were revealed with X-Ray diffraction (XRD) and Selected Area Electron Diffraction (SAED) analysis. Scanning electron microscope- (SEM) and transmission electron microscope (TEM) showed the porous morphology and reduced particle for SiO₂ and La-SiO₂ xerogels respectively. The existence of elements, siloxane networks, and thermal stability of xerogel was confirmed by energy dispersive spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), and Thermographic analysis (TGA). UV-Vis spectroscopy and photoluminescence (PL) have been used to characterize the optical properties of xerogels. La-SiO₂ demonstrates promising characteristic features of an active sensing film for dissolved oxygen in the water. Keywords: Sol-gel, ORMOSILs, encapsulation, Luminophores quenching, O₂-sensing

Keywords: sol-gel, ORMOSILs, luminophores quenching, O₂-sensing

Procedia PDF Downloads 122

Authors: Jyoti Yadav, Rini Singh, Anoop M.D, Nisha Yadav, N. Srinivasa Rao, Fouran Singh, Takayuki Ichikawa, Ankur Jain, Kamlendra Awasthi, Manoj Kumar

Abstract:

Nanocrystalline films exhibit defects and strain induced by its grain boundaries. Defects and strain affect the physical as well as topological insulating properties of the Bi2Te3 thin films by changing their electronic structure. In the present studies, the effect of Ni7+ ion irradiation on the physical and electrical properties of Bi2Te3 thin films was studied. The films were irradiated at five different fluences (5x1011, 1x1012, 3x1012, 5x1012, 1x1013 ions/cm2). Thin films synthesized using the e-beam technique possess a rhombohedral crystal structure with the R-3m space group. The average crystallite size, as determined by x-ray diffraction (XRD) peak broadening, was found to be 18.5 ± 5 (nm). It was also observed that irradiation increases the induced strain. Raman Spectra of the films demonstrate the splitting of A_1u^1 modes originating from the vibrations along the c-axis. This is by the variation in the lattice parameter ‘c,’ as observed through XRD. The atomic force microscopy study indicates the decrease in surface roughness up to the fluence of 3x1012 ions/cm2 and further increasing the fluence increases the roughness. The decrease in roughness may be due to the growth of smaller nano-crystallites on the surface of thin films due to irradiation-induced annealing. X-ray photoelectron spectroscopy studies reveal the composition to be in close agreement to the nominal values i.e. Bi2Te3. The resistivity v/s temperature measurements revealed an increase in resistivity up to the fluence 3x1012 ions/cm2 and a decrease on further increasing the fluence. The variation in electrical resistivity is corroborated with the change in the carrier concentration as studied through low-temperature Hall measurements. A crossover from the n-type to p-type carriers was achieved in the irradiated films. Interestingly, tuning of the Fermi level by compensating the bulk carriers using ion-irradiation could be achieved.

Keywords: Annealing, Irradiation, Fermi level, Tuning

Procedia PDF Downloads 136

Authors: Omar Concepcion, Osvaldo De Melo, Arturo Escobosa

Abstract:

Topological insulator (TI) materials are insulating in the bulk and conducting in the surface. The unique electronic properties associated with these surface states make them strong candidates for exploring innovative quantum phenomena and as practical applications for quantum computing, spintronic and nanodevices. Many materials, including Bi₂Te₃, have been proposed as TIs and, in some cases, it has been demonstrated experimentally by angle-resolved photoemission spectroscopy (ARPES), scanning tunneling spectroscopy (STM) and/or magnetotransport measurements. A clean surface is necessary in order to make any of this measurements. Several techniques have been used to produce films and different kinds of nanostructures. Growth and characterization in situ is usually the best option although cleaving the films can be an alternative to have a suitable surface. In the present work, we report a comparison of Bi₂Te₃ grown by physical vapor transport (PVT) and molecular beam epitaxy (MBE). The samples were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and ARPES. The Bi₂Te₃ samples grown by PVT, were cleaved in the ultra-high vacuum in order to obtain a surface free of contaminants. In both cases, the XRD shows a c-axis orientation and the pole diagrams proved the epitaxial relationship between film and substrate. The ARPES image shows the linear dispersion characteristic of the surface states of the TI materials. The samples grown by PVT, a relatively simple and cost-effective technique shows the same high quality and TI properties than the grown by MBE.

Keywords: Bismuth telluride, molecular beam epitaxy, physical vapor transport, topological insulator

Procedia PDF Downloads 192

Authors: Bhargav Baruah, Ali Shemsedin Reshad, Pankaj Tiwari

Abstract:

This work presents a detailed study on the thermal degradation kinetics of co-pyrolysis of oil shale of Upper Assam, India with rubber seed shell, and lab-scale pyrolysis to investigate the influence of pyrolysis parameters on product yield and composition of products. The physicochemical characteristics of oil shale and rubber seed shell were studied by proximate analysis, elemental analysis, Fourier transform infrared spectroscopy and X-ray diffraction. The physicochemical study showed the mixture to be of low moisture, high ash, siliceous, sour with the presence of aliphatic, aromatic, and phenolic compounds. The thermal decomposition of the oil shale with rubber seed shell was studied using thermogravimetric analysis at heating rates of 5, 10, 20, 30, and 50 °C/min. The kinetic study of the oil shale pyrolysis process was performed on the thermogravimetric (TGA) data using three model-free isoconversional methods viz. Friedman, Flynn Wall Ozawa (FWO), and Kissinger Akahira Sunnose (KAS). The reaction mechanisms were determined using the Criado master plot. The understanding of the composition of Indian oil shale and rubber seed shell and pyrolysis process kinetics can help to establish the experimental parameters for the extraction of valuable products from the mixture. Response surface methodology (RSM) was employed usinf central composite design (CCD) model to setup the lab-scale experiment using TGA data, and optimization of process parameters viz. heating rate, temperature, and particle size. The samples were pre-dried at 115°C for 24 hours prior to pyrolysis. The pyrolysis temperatures were set from 450 to 650 °C, at heating rates of 2 to 20°C/min. The retention time was set between 2 to 8 hours. The optimum oil yield was observed at 5°C/min and 550°C with a retention time of 5 hours. The pyrolytic oil and gas obtained at optimum conditions were subjected to characterization using Fourier transform infrared spectroscopy (FT-IR) gas chromatography and mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (NMR).

Keywords: Indian oil shale, rubber seed shell, co-pyrolysis, isoconversional methods, gas chromatography, nuclear magnetic resonance, Fourier transform infrared spectroscopy

Procedia PDF Downloads 146

Authors: Kohei Yamamoto, Jae-Ho Kim, Susumu Yonezawa

Abstract:

The surface of polyethylene terephthalate (PET) was modified with fluorine gas at 25 ℃ and 100 Torr for one h. Moreover, the effect of ethanol washing on surface modification was investigated in this study. The surface roughness of the fluorinated and washed PET samples was approximately six times larger than that (0.6 nm) of the untreated thing. The results of Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy showed that the bonds such as -C=O and -C-Hx derived from raw PET decreased and were converted into fluorinated bonds such as -CFx after surface fluorination. Even after washing with ethanol, the fluorinated bonds stably existed on the surface. These fluorinated bonds showed higher electronegativity according to the zeta potential results. The negative surface charges were increased by washing the ethanol, and it caused to increase in the number of polar groups such as -CHF- and -C-Fx. The fluorinated and washed surface of PET could promote the adsorption of Ag+ ions in AgNO₃ solution because of the increased surface roughness and the negatively charged surface.

Keywords: Ag+ ions adsorption, polyethylene terephthalate, surface fluorination, zeta potential

Procedia PDF Downloads 121

Authors: Surabhi Pandey, Pavuluri Srinivasa Rao

Abstract:

Extrusion processing is a high-temperature short time (HTST) treatment which can improve protein quality and digestibility together with retaining active nutrients. In-vitro protein digestibility of plant protein-based foods is generally enhanced by extrusion. The current study aimed to investigate the effect of extrusion cooking on in-vitro protein digestibility (IVPD) and conformational modification of protein in green banana flour extrudates. Green banana flour was extruded through a co-rotating twin-screw extruder varying the moisture content, barrel temperature, screw speed in the range of 10-20 %, 60-80 °C, 200-300 rpm, respectively, at constant feed rate. Response surface methodology was used to optimise the result for IVPD. Fourier-transform infrared spectroscopy (FTIR) analysis provided a convenient and powerful means to monitor interactions and changes in functional and conformational properties of extrudates. Results showed that protein digestibility was highest in extrudate produced at 80°C, 250 rpm and 15% feed moisture. FTIR analysis was done for the optimised sample having highest IVPD. FTIR analysis showed that there were no changes in primary structure of protein while the secondary protein structure changed. In order to explain this behaviour, infrared spectroscopy analysis was carried out, mainly in the amide I and II regions. Moreover, curve fitting analysis showed the conformational changes produced in the flour due to protein denaturation. The quantitative analysis of the changes in the amide I and II regions provided information about the modifications produced in banana flour extrudates.

Keywords: extrusion, FTIR, protein conformation, raw banana flour, SDS-PAGE method

Procedia PDF Downloads 162

Authors: M. S. Gaafar, S. Y. Marzouk

Abstract:

Sodium borosilicate glasses doped with different content of NdF3 mol % have been prepared by rapid quenching method. Ultrasonic velocities (both longitudinal and shear) measurements have been carried out at room temperature and at ultrasonic frequency of 4 MHz. Elastic moduli, Debye temperature, softening temperature and Poisson's ratio have been obtained as a function of NdF3 modifier content. Results showed that the elastic moduli, Debye temperature, softening temperature and Poisson's ratio have very slight change with the change of NdF3 mol % content. Based on FTIR spectroscopy and theoretical (Bond compression) model, quantitative analysis has been carried out in order to obtain more information about the structure of these glasses. The study indicated that the structure of these glasses is mainly composed of SiO4 units with four bridging oxygens (Q4), and with three bridging and one nonbridging oxygens (Q3).

Keywords: borosilicate glasses, ultrasonic velocity, elastic moduli, FTIR spectroscopy, bond compression model

Procedia PDF Downloads 414

Authors: Stephen Daniel Iduh, Evans Chidi Egwin, Oluwatosin Kudirat Shittu

Abstract:

The process for the development of reliable and eco-friendly metallic Nanoparticles is an important step in the field of Nanotechnology for biomedical application. To achieve this, use of natural sources like biological systems becomes essential. In the present work, extracellular biosynthesis of gold Nanoparticles using aqueous leave and stembark extracts of K. senegalensis has been attempted. The gold Nanoparticles produced were characterized using High Resolution scanning electron microscopy, Ultra Violet–Visible spectroscopy, zeta-sizer Nano, Energy-Dispersive X-ray (EDAX) Spectroscopy and Fourier Transmission Infrared (FTIR) Spectroscopy. The cytotoxicity of the synthesized gold nanoparticles on MCF-7 cell line was evaluated using MTT assay. The result showed a rapid development of Nano size and shaped particles within 5 minutes of reaction with Surface Plasmon Resonance at 520 and 525nm respectively. An average particle size of 20-90nm was confirmed. The amount of the extracts determines the core size of the AuNPs. The core size of the AuNPs decreases as the amount of extract increases and it causes the shift of Surface Plasmon Resonance band. The FTIR confirms the presence of biomolecules serving as reducing and capping agents on the synthesised gold nanoparticles. The MTT assay shows a significant effect of gold nanoparticles which is concentration dependent. This environment-friendly method of biological gold Nanoparticle synthesis has the potential and can be directly applied in cancer therapy.

Keywords: biosynthesis, gold nanoparticles, characterization, calotropis procera, cytotoxicity

Procedia PDF Downloads 490

Authors: Babak Sadeghi, Rony Snyders, Marie-Paule.Delplancke-Ogletree

Abstract:

Nitrogen fixation (NF) is one of the crucial industrial processes. Many attempts have been made in order to artificially fix nitrogen, and among them, the Haber-Bosch’s (H-B) process is widely used. However, it presents two major drawbacks: huge fossil feedstock consumption and noticeable greenhouse gases emission. It is, therefore, necessary to develop alternatives. Plasma technology, as an inherent “green” technology, is considered to have a great potential for reducing the environmental impacts and improving the energy efficiency of the NF process. In this work, we have studied the catalyst assisted microwave plasma for NF application. Heterogeneous catalysts of MoO₃, with various loads 0, 5, 10, 20, and 30 wt%, supported on γ-alumina were prepared by conventional wet impregnation. Crystallinity, surface area, pore size, and microstructure were obtained by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) adsorption isotherm, Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The XRD patterns of calcined alumina confirm the γ- phase. Characteristic picks of MoO₃ could not be observed for low loads (< 20 wt%), likely indicating a high dispersion of metal oxide over the support. The specific surface area along with pores size are decreasing with increasing calcination temperature and MoO₃ loading. The MoO₃ loading does not modify the microstructure. TEM and SEM results for loading inferior to 20 wt% are coherent with a monolayer of MoO₃ on the support as proposed elsewhere. For loading of 20 wt% and more, TEM and Electron diffraction (ED) show nanocrystalline ₃-D MoO₃ particles. The catalytic performances of these catalysts were investigated in the post-discharge of a microwave plasma for NOx formation from N₂/O₂ mixtures. The plasma is sustained by a surface wave launched in a quartz tube via a surfaguide supplied by a 2.45 GHz microwave generator in pulse mode. In-situ identification and quantification of the products were carried out by Fourier-transform infrared spectroscopy (FTIR) in the post-discharge region. FTIR analysis of the exhausted gas reveal NO and NO₂ bands in presence of catalyst while only NO band were assigned without catalyst. On the other hand, in presence of catalyst, a 10% increase of NOₓ formation and of 20% increase in energy efficiency are observed.

Keywords: γ-Al2O₃-MoO₃, µ-waveplasma, N2 fixation, Plasma-catalysis, Plasma diagnostic

Procedia PDF Downloads 176

Authors: Maxim Panov, Evgenia Khairullina, Sergey Ermakov, Oleg Gundobin, Vladimir Kochemirovsky

Abstract:

The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

Keywords: laser-induced deposition, electrochemical electrodes, non-enzymatic sensors, copper

Procedia PDF Downloads 244

Authors: Setareh Shekarsaraei, Marjan Moridi, Nasser L. Hadipour

Abstract:

In this study, nuclear magnetic resonance spectroscopy and nuclear quadrupole resonance spectroscopy parameters of 14N (Nitrogen in imidazole ring) in N–H…O hydrogen bonding for Histidine hydrochloride monohydrate were calculated via density functional theory. We considered a five-molecule model system of Histidine hydrochloride monohydrate. Also, we examined the trends of environmental effect on hydrogen bonds as well as cooperativity. The functional used in this research is M06-2X which is a good functional and the obtained results have shown good agreement with experimental data. This functional was applied to calculate the NMR and NQR parameters. Some correlations among NBO parameters, NMR, and NQR parameters have been studied which have shown the existence of strong correlations among them. Furthermore, the geometry optimization has been performed using M062X/6-31++G(d,p) method. In addition, in order to study cooperativity and changes in structural parameters, along with increase in cluster size, natural bond orbitals have been employed.

Keywords: hydrogen bonding, density functional theory (DFT), natural bond orbitals (NBO), cooperativity effect

Procedia PDF Downloads 456

Authors: Ljerka Kratofil Krehula, Vanja Gilja, Andrea Husak, Sniježana Šuka, Zlata Hrnjak-Murgić

Abstract:

Zinc oxide (ZnO) can be used as photocatalysts for water purification. However, one particular interest is given on the integration of inorganic ZnO nanoclusters with conducting polymers because the resulting nanocomposites may possess unique properties and enhanced photocatalytic activity in comparison to pure ZnO, using UV and also visible light. It is needed to explore the appropriate structure of polypyrrole that can induce activation of ZnO photocatalyst since the synthesis of organic/inorganic hybrid materials can result in a synergistic and complementary feature, increasing ZnO photocatalytic efficiency. In this paper several different composites of polypyrrole/zinc oxide (ZnO) were studied. Composite samples were characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and scanning electron microscopy (SEM). The photocatalytic efficiency of prepared samples was studied as a decomposition of Reactive Red 45 (RR 45) dye, which was monitored by UV-Vis spectroscopy as a change in absorbance of characteristic wavelength at 542 nm. Results show good photocatalytic efficiency of all nanocomposite samples.

Keywords: photocatalysis, polypyrrole, wastewater, zinc oxide

Procedia PDF Downloads 266

Authors: Prasanta Sutradhar, Mitali Saha

Abstract:

With an increasing awareness of green and clean energy, zinc oxide based solar cells were found to be suitable candidates for cost-effective and environmentally friendly energy conversion devices. In this work, we have reported the green synthesis of zinc oxide nanoparticles (ZnO) by thermal method and under microwave irradiation using the aqueous extract of tomatoes as non-toxic and ecofriendly reducing material. The synthesized ZnO nanoparticles were characterised by UV-Visible spectroscopy (UV-Vis), infra-red spectroscopy (IR), particle size analyser (DLS), scanning electron microscopy (SEM), atomic force microscopy (AFM), and X- ray diffraction study (XRD). A series of ZnO nanocomposites with titanium dioxide nanoparticles (TiO2) and graphene oxide (GO) were prepared for photovoltaic application. Structural and morphological studies of these nanocomposites were carried out using UV-vis, SEM, XRD, and AFM. The current-voltage measurements of the nanocomposites demonstrated enhanced power conversion efficiency of 6.18% in case of ZnO/GO/TiO2 nanocomposite.

Keywords: ZnO, green synthesis, microwave, nanocomposites, I-V characteristics

Procedia PDF Downloads 402

Authors: Ayu Minamizawa, Jae-Ho Kim, Susumu Yonezawa

Abstract:

Aqueous peroxotitanium acid solution was prepared by the reaction between H₂O₂ solution and TiO₂ fluorinated using F₂ gas. The coating of TiO₂/SiO₂ multilayer on the surface of polycarbonate (PC) resin was carried out step by step using the TEOS solution and aqueous peroxotitanium acid solution. We confirmed each formation of SiO₂ and TiO₂ layer by scanning electron microscopy and energy-dispersive X-ray spectroscopy, and x-ray photoelectron spectroscopy results. The formation of a TiO₂ thin layer on SiO₂ coated on polycarbonate (PC) was carried out at 120 ℃ and for 15 min ~ 3 h with aqueous peroxotitanium acid solution using a hydrothermal synthesis autoclave reactor. The morphology TiO₂ coating layer largely depended on the reaction time, as shown in the results of SEM-EDS analysis. Increasing the reaction times, the TiO₂ layer expanded uniformly. Moreover, the surface fluorination of the SiO₂ layer can promote the formation of the TiO₂ layer on the surface.

Keywords: aqueous peroxotitanium acid solution, photocatalytic activity, polycarbonate, surface fluorination

Procedia PDF Downloads 118

Authors: M. Benhamida, Kh. Bouamama, P. Djemia

Abstract:

We investigate by first-principles pseudo-potential calculations the composition dependence of lattice parameter, hardness and elastic properties of ternary disordered solid solutions Ti(1-x)Ta(x)N (1>=x>=0) with B1-rocksalt structure. Calculations use the coherent potential approximation with the exact muffin-tin orbitals (EMTO) and hardness formula for multicomponent covalent solid solution proposed. Bulk modulus B shows a nearly linear behaviour whereas not C44 and C’=(C11-C12)/2 that are not monotonous. Influences of vacancies on hardness of off-stoichiometric transition-metal nitrides TiN(1−x) and TaN(1−x) are also considered.

Keywords: transition metal nitride materials, elastic constants, hardness, EMTO

Procedia PDF Downloads 430