Search results for: surface enhanced raman spectroscopy (SERS)

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

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We are reporting a simple and low-cost chemical precipitation method adopted to prepare zinc oxide nanoparticles (ZnO) using polyvinyl pyrrolidone (PVP) as a capping agent. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) was applied on the dried gel sample to record the phase transformation temperature of zinc hydroxide Zn(OH)2 to zinc oxide (ZnO) to obtain the annealing temperature of 800C. The thermal, structure, morphology and optical properties have been employed by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM). X-ray diffraction results confirmed the wurtzite hexagonal structure of ZnO nanoparticles. The two intensive peaks at 160 and 432 cm-1 in the Raman Spectrum are mainly attributed to the first order modes of the wurtzite ZnO nanoparticles. The energy band gap obtained from the UV-Vis absorption spectra, shows a blue shift, which is attributed to increase in carrier concentration (Burstein Moss Effect). Photoluminescence studies of the single crystalline ZnO nanoparticles, show a strong peak centered at 385 nm, corresponding to the near band edge emission in ultraviolet range. The mixed shape of grapes, sphere, hexagonal and rock like structure has been noticed in FESEM. The results showed that PVP is a suitable capping agent for the preparation of ZnO nanoparticles by simple chemical precipitation method.

Keywords: ZnO nanoparticles, simple chemical precipitation route, mixed shape morphology, UV-visible absorption, photoluminescence, Fourier transform infra-Red spectroscopy

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

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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

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Authors: Thabelo Nelushi, Michael Scurrell, Tumelo Seadira

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Global warming is one of the most important environmental issues which arise from occurrence of gases such as carbon dioxide (CO2) and methane (CH4) in the atmosphere. Exposure to these greenhouse gases results in health risk. Hydrogen is regarded as an alternative energy source which is a clean energy carrier for the future. There are different methods to produce hydrogen such as steam reforming, coal gasification etc., however the challenge with these processes is that they emit CO and CO2 gases and are costly. Photocatalytic reforming is a substitute process which is fascinating due to the combination of solar energy and renewable sources and the use of semiconductor materials such as catalysts. TiO2 is regarded as the most promising catalysts. TiO2 nanoparticles prepared by hydrothermal method and Ag/TiO2 are being investigated for photocatalytic production of hydrogen from butanol. The samples were characterized by raman spectroscopy, TEM/SEM, XRD, XPS, EDAX, DRS and BET surface area. 2 wt% Ag-doped TiO2 nanoparticle showed enhanced hydrogen production compared to a non-doped TiO2. The results of characterization and photoactivity shows that TiO2 nanoparticles play a very important role in producing high hydrogen by utilizing solar irradiation.

Keywords: butanol, hydrogen production, silver particles, TiO2 nanoparticles

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Authors: Tasnuva Tamanna, Aimin Yu

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Application of nanoscience in biomedical field has come across as a new era. This study involves the synthesis of nano drug carrier with antibiotic loading. Based on the founding that polydopamine (PDA) nanoparticles could be formed via self-polymerization of dopamine at alkaline pH, one-step synthesis of rifampicin coupled polydopamine (PDA-R) nanoparticles was achieved by adding rifampicin into the dopamine solution. The successful yield of PDA nanoparticles with or without the presence of rifampicin during the polymerization process was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. Drug loading was monitored by UV-vis spectroscopy and the loading efficiency of rifampicin was calculated to be 76%. Such highly capacious nano-reservoir was found very stable with little drug leakage at pH 3.

Keywords: drug loading, nanoparticles, polydopamine, rifampicin

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Authors: José M. Liñeira Del Río, Ramón Rial, Khodor Nasser, María J.G. Guimarey

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The need to develop new lubricants that offer better anti-friction and anti-wear performance in internal combustion vehicles is one of the great challenges of lubrication in the automotive field. The addition of nanoparticles has emerged as a possible solution and, combined with the lubricating power of ionic liquids, may become one of the alternatives to reduce friction losses and wear of the contact surfaces in the conditions to which tribo-pairs are subjected, especially in the contact of the piston rings and the cylinder liner surface. In this study, the improvement in SAE 10W-40 engine oil tribological performance after the addition of magnesium oxide (MgO) nanoadditives and two different phosphonium-based ionic liquids (ILs) was investigated. The nanoparticle characterization was performed by means of transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The tribological properties, friction coefficients and wear parameters of the formulated oil modified with 0.01 wt.% MgO and 1 wt.% ILs compared with the neat 10W-40 oil were performed and analyzed using a ball-on-three-pins tribometer and a 3D optical profilometer, respectively. Further analysis on the worn surface was carried out by Raman spectroscopy and SEM microscopy, illustrating the formation of the protective IL and MgO tribo-films as hybrid additives. In friction tests with sliding steel-steel tribo-pairs, IL3-based hybrid nanolubricant decreased the friction coefficient and wear volume by 7% and 59%, respectively, in comparison with the neat SAE 10W-40, while the one based on IL1 only achieved a reduction of these parameters by 6% and 39%, respectively. Thus, the tribological characterization also revealed that the MgO and IL3 addition has a positive synergy over the commercial lubricant, adequately meeting the requirements for their use in internal combustion engines. In summary, this study has shown that the addition of ionic liquids to MgO nanoparticles can improve the stability and lubrication behavior of MgO nanolubricant and encourages more investigations on using nanoparticle additives with green solvents such as ionic liquids to protect the environment as well as prolong the lifetime of machinery. The improvement in the lubricant properties was attributed to the following wear mechanisms: the formation of a protective tribo-film and the ability of nanoparticles to fill out valleys between asperities, thereby effectively smoothing out the shearing surfaces.

Keywords: lubricant, nanoparticles, phosphonium-based ionic liquids, tribology

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Authors: Hyery Kang, Dong-Yeun Koh, Yun-Ho Ahn, Huen Lee

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Terahertz time-domain spectroscopy (THz-TDS) was used to observe the THF clathrate hydrate system with dosage of polyvinylpyrrolidone (PVP) with three different average molecular weights (10,000 g/mol, 40,000 g/mol, 360,000 g/mol). Distinct footprints of phase transition in the THz region (0.4 - 2.2 THz) were analyzed and absorption coefficients and complex refractive indices are obtained and compared in the temperature range of 253 K to 288 K. Along with the optical properties, ring breathing and stretching modes for different molecular weights of PVP in THF hydrate are analyzed by Raman spectroscopy.

Keywords: clathrate hydrate, terahertz, polyvinylpyrrolidone (PVP), THz-TDS, inhibitor

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Authors: Jung-Hwan Oh, Rajesh Kumar, Il-Kwon Oh

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Porous graphene has extensive potential applications in variety of fields such as hydrogen storage, CO oxidation, gas separation, supercapacitors, fuel cells, nanoelectronics, oil adsorption, and so on. However, the generation of some carbon atoms vacancies for precise small holes have been not extensively studied to prevent the agglomerates of graphene sheets and to obtain porous graphene with high surface area. Recently, many research efforts have been presented to develop physical and chemical synthetic approaches for porous graphene. But physical method has very high cost of manufacture and chemical method consumes so many hours for porous graphene. Herein, we propose a porous graphene contained holes with atomic scale precision by embedding metal nano-particles through microwave irradiation for hydrogen storage and CO oxidation multi- functionalities. This proposed synthetic method is appropriate for fast and convenient production of three dimensional nanostructures, which have nanoholes on the graphene surface in consequence of microwave irradiation. The metal nanoparticles are dispersed quickly on the graphene surface and generated uniform nanoholes on the graphene nanosheets. The morphological and structural characterization of the porous graphene were examined by scanning electron microscopy (SEM), transmission scanning electron microscopy (TEM) and RAMAN spectroscopy, respectively. The metal nanoparticle-embedded porous graphene exhibits a microporous volume of 2.586cm3g-1 with an average pore radius of 0.75 nm. HR-TEM analysis was carried out to further characterize the microstructures. By investigating the RAMAN spectra, we can understand the structural changes of graphene. The results of this work demonstrate a possibility to produce a new class of porous graphene. Furthermore, the newly acquired knowledge for the diffusion into graphene can provide useful guidance for the development of the growth of nanostructure.

Keywords: CO oxidation, hydrogen storage, nanocomposites, porous graphene

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Authors: El Mehdi Haily, Lahcen Bih, Mohammed Azrour, Bouchaib Manoun

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The effects of xBi₂O₃-yBaO-zP₂O₅ (BBP) glass addition on the sintering, structural, and dielectric properties of BaTiO₃ ceramic (BT) are studied. The BT ceramic was synthesized by the conventional solid-state reaction method while the glasses BaO-Bi₂O₃-P₂O₅ (BBP) were elaborated by melting and quenching process. Different composites BT-xBBP were formed by mixing the BBP glasses with BT ceramic. For each glass composition, where the ratio (x:y:z) is maintained constant, we have developed three composites with different glass weight percentage (x = 2.5, 5, and 7.5 wt %). Addition of the glass helps in better sintering at lower temperatures with the presence of liquid phase at the respective sintering temperatures. The results showed that the sintering temperature decreased from more than 1300°C to 900°C. Density measurements of the composites are performed using the standard Archimedean method with water as medium liquid. It is found that their density and molar volume decrease and increase with glass content, respectively. Raman spectroscopy is used to characterize their structural approach. This technique has allowed the identification of different structural units of phosphate and the characteristic vibration modes of the BT. The electrical properties of the composite samples are carried out by impedance spectroscopy in the frequency range of 10 Hz to 1 MHz under various temperatures from 300 to 473 K. The obtained results show that their dielectric properties depend both on the content of the glass in the composite and the Bi/P ratio in the glasses.

Keywords: phosphate, glasses, composite, Raman spectroscopy, dielectric properties

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Authors: Mahtab Assadian, Mohd Hasbullah Idris, Mostafa Rezazadeh Shirdar, Mohammad Mahdi Taheri, ‎S. Izman

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Corrosion behaviour and surface roughness of magnesium substrate were investigated after NaOH pretreatment in different concentrations (1, 5, and 10 molar) and duration of (10 min, 30 min, 1 h, 3 h, 6 h and 24 h). Creation of Mg(OH)2 barrier layer after pretreatment enhanced corrostion resistance as well as wettability of substrate surface. Characterization including Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) was conducted to detect the existence of this barrier layer. Surface roughness and wettability of substrate was evaluated using atomic force microscopy (AFM) and contact angle measurement respectively. It is found that magnesium treated by 1M NaOH for 30 min reveals higher corrosion resistance and lower water contact angle of substrate surface. In addition, this investigation indicates that pH value of SBF solution is strongly influenced by different time and concentration of alkaline pretreatment.

Keywords: magnesium, NaOH pretreatment, corrosion resistance, wettability

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Authors: Poonam Yadav, Dong Bok Lee

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Raman spectroscopy was used for characterization of multi-wall carbon nanotube (MWNT) and Polycarbonate/multi-wall carbon nanotube (PC/MWNT) based fibers with 0.55% and 0.75% of MWNT (PC/MWNT55 and PC/MWNT75). PC/MWNT55 and PC/MWNT75 fibers was prepared by melt spinning device using nanocomposites made by two different route, viz., solvent casting and melt extrusion. Fibers prepared from melt extruded nanocomposites showed smooth and uniform morphology as compared to solvent casting based nanocomposites. The Raman mapping confirmed that the melt extruded based nanocomposites had better dispersion of MWNT in Polycarbonate (PC) than solvent casting carbon nanotube.

Keywords: dispersion, melt extrusion, multi-wall carbon nanotube, mapping

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, Milan Masař, Martin Holek

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ZnFe2O4 spinel ferrite nanoparticles were synthesized by sol-gel auto-combustion method. The synthesized spinel ferrite nanoparticles were annealed at different higher temperature to achieve different size nanoparticles. The as synthesized and annealed samples were characterized by powder X-ray Diffraction Spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, UV-Vis absorption Spectroscopy and Scanning Electron Microscopy. The magnetic properties were studied by vibrating sample magnetometer. The variation in magnetic parameters was noticed with variation in grain size. The dielectric constant and dielectric loss with variation of frequency shows normal behaviour of spinel ferrite. The variation in conductivity with variation in grain size is noticed. Modulus and Impedance Spectroscopy shows the role of grain and grain boundary on the electrical resistance and capacitance of different grain sized spinel ferrite nanoparticles. Acknowledgment: This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: spinel ferrite, nanoparticles, magnetic properties, dielectric properties

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Authors: Rejane Maria P. da Silva, Mariana X. Milagre, João Victor de S. Araujo, Leandro A. de Oliveira, Renato A. Antunes, Isolda Costa

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The Al-Cu-Li alloys are advanced materials for aerospace application because of their interesting mechanical properties and low density when compared with conventional Al-alloys. However, Al-Cu-Li alloys are susceptible to localized corrosion. The near-surface deformed layer (NSDL) induced by the rolling process during the production of the alloy and its removal by polishing can influence on the corrosion susceptibility of these alloys. In this work, the influence of surface preparation effects on the electrochemical activity of AA2098-T351 (Al–Cu–Li alloy) was investigated using a correlation between surface chemistry, microstructure, and electrochemical activity. Two conditions were investigated, polished and as-received surfaces of the alloy. The morphology of the two types of surfaces was investigated using confocal laser scanning microscopy (CLSM) and optical microscopy. The surface chemistry was analyzed by X-ray Photoelectron Spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS). Global electrochemical techniques (potentiodynamic polarization and EIS technique) and a local electrochemical technique (Localized Electrochemical Impedance Spectroscopy-LEIS) were used to examine the electrochemical activity of the surfaces. The results obtained in this study showed that in the as-received surface, the near-surface deformed layer (NSDL), which is composed of Mg-rich bands, influenced the electrochemical behavior of the alloy. The results showed higher electrochemical activity to the polished surface condition compared to the as-received one.

Keywords: Al-Cu-Li alloys, surface preparation effects, electrochemical techniques, localized corrosion

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Authors: Souha Bouagila, Soufiene Ilahi, Noureddine Yacoubi

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We have used Photothermal deflection spectroscopy PTD to investigate the impact of thermal annealing on electronics properties of GaInAsSb/GaSb.GaInAsSb used as an active layer for Vertical Cavity Surface Emitting laser (VCSEL). We have remarked that surface recombination velocity (SRV) from 7963 m / s (± 6.3%) to 1450 m / s (± 3.6) for as grown to sample annealed for 60 min. Accordingly, Force Microscopy images analyses agree well with the measure of surface recombination velocity. We have found that Root-Mean-Square Roughness (RMS) decreases as respect of annealing time. In addition, we have that the diffusion length and minority carrier mobility have been enhanced according to annealing time. However, due to annealing effects, the interface recombination velocity (IRV) is increased from 1196 m / s (± 5) to 6000 m/s (5%) for GaInAsSb in respect of annealed times.

Keywords: nonradiative lifetime, mobility of minority carrier, diffusion length, Surface and interface recombination velocity

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Authors: Josef Sepitka, Petr Vlcak, Tomas Horazdovsky, Vratislav Perina

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An ion implantation technique was used for designing the surface area of a titanium alloy and for irradiation-enhanced hardening of the surface. The Ti6Al4V alloy was treated by nitrogen ion implantation at fluences of 2·10¹⁷ and 4·10¹⁷ cm^-2 and at ion energy 90 keV. The depth distribution of the nitrogen was investigated by Rutherford Backscattering Spectroscopy. The gradient of mechanical properties was investigated by nanoindentation. The continuous measurement mode was used to obtain depth profiles of the indentation hardness and the reduced storage modulus of the modified surface area. The reduced storage modulus and the hardness increase with increasing fluence. Increased fluence shifts the peak of the mechanical properties as well as the peak of nitrogen concentration towards to the surface. This effect suggests a direct relationship between mechanical properties and nitrogen distribution.

Keywords: nitrogen ion implantation, titanium-based nanolayer, storage modulus, hardness, microstructure

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Authors: Chetna Tyagi, Ambuj Tripathi, Devesh Avasthi

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Graphene oxide consists of sp³ hybridization along with sp² hybridization due to the presence of different oxygen-containing functional groups on its edges and basal planes. However, its sp³ / sp² hybridization can be tuned by various methods to utilize it in different applications, like transistors, solar cells and biosensors. Ion beam irradiation can also be one of the methods to optimize sp² and sp³ hybridization ratio for its desirable properties. In this work, graphene oxide films were irradiated with 100 keV Argon ions at different fluences varying from 10¹³ to 10¹⁶ ions/cm². Synchrotron X-ray diffraction measurements showed an increase in crystallinity at the low fluence of 10¹³ ions/cm². Raman spectroscopy performed on irradiated samples determined the defects induced by the ion beam qualitatively. Also, identification of different groups and their removal with different fluences was done using Fourier infrared spectroscopy technique.

Keywords: graphene oxide, ion beam irradiation, spectroscopy, X-ray diffraction

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Authors: Ruolan Zhang, Ryo Imai, Naoko Senda, Tomoyuki Sakai

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Enzymes have attracted increasing attentions in industrial manufacturing for their applicability in catalyzing complex chemical reactions under mild conditions. Directed evolution has become a powerful approach to optimize enzymes and exploit their full potentials under the circumstance of insufficient structure-function knowledge. With the incorporation of cell-free synthetic biotechnology, rapid enzyme synthesis can be realized because no cloning procedure such as transfection is needed. Its open environment also enables direct enzyme measurement. These properties of cell-free biotechnology lead to excellent throughput of enzymes generation. However, the capabilities of current screening methods have limitations. Fluorescence-based assay needs applicable fluorescent label, and the reliability of acquired enzymatic activity is influenced by fluorescent label’s binding affinity and photostability. To acquire the natural activity of an enzyme, another method is to combine pre-screening step and high-performance liquid chromatography (HPLC) measurement. But its throughput is limited by necessary time investment. Hundreds of variants are selected from libraries, and their enzymatic activities are then identified one by one by HPLC. The turn-around-time is 30 minutes for one sample by HPLC, which limits the acquirable enzyme improvement within reasonable time. To achieve the real high-throughput enzyme screening, i.e., obtain reliable enzyme improvement within reasonable time, a widely applicable high-throughput measurement of enzymatic reactions is highly demanded. Here, a high-throughput screening method using broadband coherent anti-Stokes Raman spectroscopy (CARS) was proposed. CARS is one of coherent Raman spectroscopy, which can identify label-free chemical components specifically from their inherent molecular vibration. These characteristic vibrational signals are generated from different vibrational modes of chemical bonds. With the broadband CARS, chemicals in one sample can be identified from their signals in one broadband CARS spectrum. Moreover, it can magnify the signal levels to several orders of magnitude greater than spontaneous Raman systems, and therefore has the potential to evaluate chemical's concentration rapidly. As a demonstration of screening with CARS, alcohol dehydrogenase, which converts ethanol and nicotinamide adenine dinucleotide oxidized form (NAD+) to acetaldehyde and nicotinamide adenine dinucleotide reduced form (NADH), was used. The signal of NADH at 1660 cm⁻¹, which is generated from nicotinamide in NADH, was utilized to measure the concentration of it. The evaluation time for CARS signal of NADH was determined to be as short as 0.33 seconds while having a system sensitivity of 2.5 mM. The time course of alcohol dehydrogenase reaction was successfully measured from increasing signal intensity of NADH. This measurement result of CARS was consistent with the result of a conventional method, UV-Vis. CARS is expected to have application in high-throughput enzyme screening and realize more reliable enzyme improvement within reasonable time.

Keywords: Coherent Anti-Stokes Raman Spectroscopy, CARS, directed evolution, enzyme screening, Raman spectroscopy

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Authors: Alejandro Carrasco-Pena, Mahmoud Omer, Nina Orlovskaya

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The results of studies of microstructure, mechanical behavior, vibrational response, and flow field analysis of critically endangered staghorn coral (Acropora cervicornis) skeletons are reported. The CaCO₃ aragonite structure of a chemically-cleaned coral skeleton of A. cervicornis was studied by optical microscopy and computer tomography. The mechanical behavior was studied using uniaxial compression and Vickers hardness technique. The average maximum stress measured during skeleton uniaxial compression was 10.7 ± 2.24 MPa and Vickers hardness was 3.56 ± 0.31 GPa. The vibrational response of the aragonite structure was studied by micro-Raman spectroscopy, which showed a substantial dependence of the structure on applied compressive stress. The flow-field around a single coral skeleton forming vortices in the wake of the moving skeleton was measured using Particle Image Velocimetry (PIV). The results are important for further analysis of time-dependent mechanical fatigue behavior and predicting the lifetime of staghorn corals.

Keywords: failure, mechanical properties, microstructure, Raman spectroscopy

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Authors: Ke Lin, Steve Wu Qing Yang, Zhang Nan

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The medicine and drugs has in the past been manufactured to the final products and then used laboratory analysis to verify their quality. However the industry needs crucially a monitoring technique for the final batch to batch quality check. The introduction of process analytical technology (PAT) provides an incentive to obtain real-time information about drugs on the production line, with the following optical techniques being considered: near-infrared (NIR) spectroscopy, Raman spectroscopy and imaging, mid-infrared spectroscopy with the use of chemometric techniques to quantify the final product. However, presents problems in that the spectra obtained will consist of many combination and overtone bands of the fundamental vibrations observed, making analysis difficult. In this work, we describe a non-destructive system and method for capsule and liquid medicine identification, more particularly, using terahertz time-domain spectroscopy and/or designed terahertz portable system for identifying different types of medicine in the package of capsule or in liquid medicine bottles. The target medicine can be detected directly, non-destructively and non-invasively.

Keywords: terahertz, non-destructive, non-invasive, chemical identification

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

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

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

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Authors: P. Suchismita Behera, V. G. Sathe, A. K. Nigam, P. A. Bhobe

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Co-existence of long-range ferromagnetism and semi-conductivity with correlated behavior of structural, magnetic, optical and electrical properties in various sites doping at CdCr2Se4 makes it a most promising candidate for spin-based electronic applications and magnetic devices. It orders ferromagnetically below TC = 130 K with a direct band gap of ~ 1.5 eV. The magnetic ordering is believed to result from strong competition between the direct antiferromagnetic Cr-Cr spin couplings and the ferromagnetic Cr-Se-Cr exchange interactions. With an aim of understanding the influence of crystal structure on its magnetic properties without disturbing the magnetic site, we investigated four compositions with 3%, 5%, 7% and 10% of Sn-substitution at Cd-site. Partial substitution of Cd2+ (0.78Å) by small sized nonmagnetic ion, Sn4+ (0.55Å), is expected to bring about local lattice distortion as well as a change in electronic charge distribution. The structural disorder would affect the Cd/Sn – Se bonds thus affecting the Cr-Cr and Cr-Se-Cr bonds. Whereas, the charge imbalance created due to Sn4+ substitution at Cd2+ leads to the possibility of Cr mixed valence state. Our investigation of the local crystal structure using the EXAFS, Raman spectroscopy and magnetic properties using SQUID magnetometry of the Cd1-xSnxCr2Se4 series reflects this premise. All compositions maintain the Fd3m cubic symmetry with tetrahedral distribution of Sn at Cd-site, as confirmed by XRD analysis. Lattice parameters were determined from the Rietveld refinement technique of the XRD data and further confirmed from the EXAFS spectra recorded at Cr K-edge. Presence of five Raman-active phonon vibrational modes viz. (T2g (1), T2g (2), T2g (3), Eg, A1g) in the Raman spectra further confirms the crystal symmetry. Temperature dependence of the Raman data provides interesting insight to the spin– phonon coupling, known to dominate the magneto-capacitive properties in the parent compound. Below the magnetic ordering temperature, the longitudinal damping of Eg mode associated with Se-Cd/Sn-Se bending and T2g (2) mode associated to Cr-Se-Cr interaction, show interesting deviations with respect to increase in Sn substitution. Besides providing the estimate of TC, the magnetic measurements recorded as a function of field provide the values of total magnetic moment for all the studied compositions indicative of formation of multiple Cr valences.

Keywords: exchange interactions, EXAFS, ferromagnetism, Raman spectroscopy, spinel chalcogenides

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Authors: J. Plocek, P. Holec, S. Kubickova, B. Pacakova, I. Matulkova, A. Mantlikova, I. Němec, D. Niznansky, J. Vejpravova

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This article presents summary on preparation and characterization of zinc, copper, cadmium and cobalt chromite nano crystals, embedded in an amorphous silica matrix. The ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2 nano composites were prepared by a conventional sol-gel method under acid catalysis. Final heat treatment of the samples was carried out at temperatures in the range of 900–1200 °C to adjust the phase composition and the crystallite size, respectively. The resulting samples were characterized by Powder X-ray diffraction (PXRD), High Resolution Transmission Electron Microscopy (HRTEM), Raman/FTIR spectroscopy and magnetic measurements. Formation of the spinel phase was confirmed in all samples. The average size of the nano crystals was determined from the PXRD data and by direct particle size observation on HRTEM; both results were correlated. The mean particle size (reviewed by HRTEM) was in the range from ~ 4 to 46 nm. The results showed that the sol-gel method can be effectively used for preparation of the spinel chromite nano particles embedded in the silica matrix and the particle size is driven by the type of the cation A2+ in the spinel structure and the temperature of the final heat treatment. Magnetic properties of the nano crystals were found to be just moderately modified in comparison to the bulk phases.

Keywords: sol-gel method, nanocomposites, Rietveld refinement, Raman spectroscopy, Fourier transform infrared spectroscopy, magnetic properties, spinel, chromite

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Authors: Surjyakanta Rana, Sreekantha B. Jonnalagadda

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Synthesis of well distributed Pd nanoparticles (3 – 7 nm) on organo amine-functionalized graphene is reported, which demonstrated excellent catalytic activity towards Suzuki coupling reaction. The active material was characterized by X-ray diffraction (XRD), BET surface area, X-ray photoelectron spectra (XPS), Fourier-transfer infrared spectroscopy (FTIR), Raman spectra, Scanning electron microscope (SEM), Transmittance electron microscopy (TEM) analysis and HRTEM. FT-IR revealed that the organic amine functional group was successfully grafted onto the graphene oxide surface. The formation of palladium nanoparticles was confirmed by XPS, TEM and HRTEM techniques. The catalytic activity in the coupling reaction was superb with 100% conversion and 98 % yield and also activity remained almost unaltered up to six cycles. Typically, an extremely high turnover frequency of 185,078 h-1 is observed in the C-C Suzuki coupling reaction using organo di-amine functionalized graphene as catalyst.

Keywords: Di-amine, graphene, Pd nanoparticle, suzuki coupling

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Authors: Anna Drzewicz, Marzena Tykarska

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The chiral liquid crystal phases form the helicoidal structure, which is characterized by the helical pitch and the helical twist sense. In anticlinic smectic phase with antiferroelectric properties three types of helix temperature dependence have been obtained: increased helical pitch with temperature and right-handed helix, decreased helical pitch with temperature and left-handed helix and the inversion of both. The change of helical twist sense may be observed during the transition from one liquid crystal phase to another or within one phase for the same substance. According to Gray and McDonnell theory, the helical handedness depends on the absolute configuration of the assymetric carbon atom and its position related to the rigid core of the molecule. However, this theory does not explain the inversion of helical twist sense phenomenon. It is supposed, that it may be caused by the presence of different conformers with opposite handendess, which concentration may change with temperature. In this work, the inversion of helical twist sense in the chiral liquid crystals differing in the length of alkyl chain, in the substitution the benzene ring by fluorine atoms and in the type of helix handedness was tested by vibrational spectroscopy (infrared and raman spectroscopy) and by nuclear magnetic resonance spectroscopy. The results obtained from the vibrational spectroscopy confirm the presence of different conformers. Moreover, the analysis of nuclear magnetic resonance spectra is very useful to check, on which structural fragments the change of conformations are important for the change of helical twist sense.

Keywords: helical twist sense, liquid crystals, nuclear magnetic resonance spectroscopy, vibrational spectroscopy

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Authors: Surinder Singh, Adish Bindal

Abstract:

The effects of the pumping wavelength and their power on the gain flattening of a fiber Raman amplifier (FRA) are investigated. The multi-wavelength pumping scheme is utilized to achieve gain flatness in FRA. It is proposed that gain flatness becomes better with increase in number of pumping wavelengths applied. We have achieved flat gain with 0.27 dB fluctuation in a spectral range of 1475-1600 nm for a Raman fiber length of 10 km by using six pumps with wavelengths with in the 1385-1495 nm interval. The effect of multi-wavelength pumping scheme on gain saturation in FRA is also studied. It is proposed that gain saturation condition gets improved by using this scheme and this scheme is more useful for higher spans of Raman fiber length.

Keywords: FRA, WDM, pumping, flat gain

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Authors: G. Balaji, R. Balasundaraprabhu, S. Prasanna, M. D. Kannan, K. Sivakumaran, David Mcilroy

Abstract:

Copper Zin tin sulphide (Cu2ZnSnS4 or CZTS) is found to be better alternative to Copper Indium gallium diselenide as absorber layers in thin film based solar cells due to the utilisation of earth-abundant materials in the midst of lower toxicity. In the present study, Cu2ZnSnS4 thin films were prepared on soda lime glass using (CuS, ZnS, SnS) targets and were deposited by three different stacking orders, using RF Magnetron sputtering. The substrate temperature was fixed at 300 °C during the depositions. CZTS thin films were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and UV-Vis-NIR spectroscopy. All the samples exhibited X-ray peaks pertaining to (112) kesterite phase of CZTS, along with the presence of a predominant wurtzite CZTS phase. X-ray photoelectron spectroscopy revealed the presence of all the elements in all the samples. The change in stacking order clearly shows that it affects the structural and phase properties of the films. Relative atomic concentrations of Zn, Cu, Sn and S, which are determined by high-resolution XPS core level spectra integrated peak areas revealed that the CZTS films exhibit inhomogeneity in both stoichiometry and elemental composition. Raman spectroscopy studies on the film showed the presence of CZTS phase. The energy band gap of the CZTS thin films was found to be in the range of 1.5 eV to 1.6 eV. The films were then annealed at 450 °C for 5 hrs and it was found that the predominant nature of the X-ray peaks has transformed from Wurtzite to Kesterite phase which is highly desirable for absorber layers in thin film solar cells. The optimized CZTS layer was used as an absorber layer in thin film solar cells. ZnS and CdS were used as buffer layers which in turn prepared by Hot wall epitaxy technique. Gallium doped Zinc oxide was used as a transparent conducting oxide. The solar cell structure Glass/Mo/CZTS/CdS or ZnS/GZO has been fabricated, and solar cell parameters were measured.

Keywords: earth-abundant, Kesterite, RF sputtering, thin film solar cells

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Authors: Nurhafizah Md. Disa, Nurhayati Binti Abdullah, Muhammad Rabie Bin Omar

Abstract:

This research intends to identify the existing knowledge gap because of the lack of substantial studies to fabricate and characterize bio-graphene created from Oil Palm Shell (OPS) through the means of pre-treatment and slow pyrolysis. By fabricating bio-graphene through OPS, a novel material can be found to procure and used for graphene-based research. The characterization of produced bio-graphene is intended to possess a unique hexagonal graphene pattern and graphene properties in comparison to other previously fabricated graphene. The OPS will be fabricated by pre-treatment of zinc chloride (ZnCl₂) and iron (III) chloride (FeCl3), which then induced the bio-graphene thermally by slow pyrolysis. The pyrolizer's final temperature and resident time will be set at 550 °C, 5/min, and 1 hour respectively. Finally, the charred product will be washed with hydrochloric acid (HCL) to remove metal residue. The obtained bio-graphene will undergo different analyses to investigate the physicochemical properties of the two-dimensional layer of carbon atoms with sp2 hybridization hexagonal lattice structure. The analysis that will be taking place is Raman Spectroscopy (RAMAN), UV-visible spectroscopy (UV-VIS), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), and X-Ray Diffraction (XRD). In retrospect, RAMAN is used to analyze three key peaks found in graphene, namely D, G, and 2D peaks, which will evaluate the quality of the bio-graphene structure and the number of layers generated. To compare and strengthen graphene layer resolves, UV-VIS may be used to establish similar results of graphene layer from last layer analysis and also characterize the types of graphene procured. A clear physical image of graphene can be obtained by analyzation of TEM in order to study structural quality and layers condition and SEM in order to study the surface quality and repeating porosity pattern. Lastly, establishing the crystallinity of the produced bio-graphene, simultaneously as an oxygen contamination factor and thus pristineness of the graphene can be done by XRD. In the conclusion of this paper, this study is able to obtain bio-graphene through OPS as a novel material in pre-treatment by chloride ZnCl₂ and FeCl3 and slow pyrolization to provide a characterization analysis related to bio-graphene that will be beneficial for future graphene-related applications. The characterization should yield similar findings to previous papers as to confirm graphene quality.

Keywords: oil palm shell, bio-graphene, pre-treatment, slow pyrolysis

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Authors: Alhulw H. Alshammari, Ahmed Iraqi, S. A. Saad, T. A. Taha

Abstract:

In this work, we present for the first time the study of Raman spectra and dielectric relaxation of polyester polymer-CoFe₂O₄ (5.0, 10.0, 15.0, and 20.0 wt%) nanocomposites. Raman spectroscopy was applied as a sensitive structural identification technique to characterize the polyester-CoFe₂O₄ nanocomposites. The images of AFM confirmed the uniform distribution of CoFe₂O₄ inside the polymer matrix. Dielectric relaxation was employed as an important analytical technique to obtain information about the ability of the polymer nanocomposites to store and filter electrical signals. The dielectric relaxation analyses were carried out on the polyester-CoFe₂O₄ nanocomposites at different temperatures. An increase in dielectric constant ε₁ was observed for all samples with increasing temperatures due to the alignment of the electric dipoles with the applied electric field. In contrast, ε₁ decreased with increasing frequency. This is attributed to the difficulty for the electric dipoles to follow the electric field. The α relaxation peak that appeared at a high frequency shifted to higher frequencies when increasing the temperature. The activation energies for Maxwell-Wagner Sillar (MWS) changed from 0.84 to 1.01 eV, while the activation energies for α relaxations were 0.54 – 0.94 eV. The conduction mechanism for the polyester- CoFe₂O₄ nanocomposites followed the correlated barrier hopping (CBH) model.

Keywords: AC conductivity, activation energy, dielectric permittivity, polyester nanocomposites

Procedia PDF Downloads 81

Authors: Yongkui Cui, Fengping Wang, Hailei Zhao, Muhammad Zubair Iqbal, Ziya Wang, Yan Li, Pengpeng LV

Abstract:

The novel 3D SnO cabbages self-assembled by nanosheets were successfully synthesized via template-free hydrothermal growth method under facile conditions.The XRD results manifest that the as-prepared SnO is tetragonal phase. The TEM and HRTEM results show that the cabbage nanosheets are polycrystalline structure consisted of considerable single-crystalline nanoparticles. Two typical Raman modes A1g=210 and Eg=112 cm-1 of SnO are observed by Raman spectroscopy. Moreover, galvanostatic cycling tests has been performed using the SnO cabbages as anode material of lithium ion battery and the electrochemical results suggest that the synthesized SnO cabbage structures are a promising anode material for lithium ion batteries.

Keywords: electrochemical property, hydrothermal synthesis, lithium ion battery, stannous oxide

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Authors: Alaa Y. Ali, Natalie P. Holmes, John Holdsworth, Warwick Belcher, Paul Dastoor, Xiaojing Zhou

Abstract:

Multi-layered graphene has been produced under low temperature chemical vapour deposition (CVD) growth conditions by utilizing an organic solvent and polymer film source. Poly(methylmethacrylate) (PMMA) was dissolved in chlorobenzene solvent and used as a drop-cast film carbon source on a quartz slide. A source temperature (T_source) of 180 °C provided sufficient carbon to grow graphene, as identified by Raman spectroscopy, on clean copper foil catalytic surfaces.  Systematic variation of hydrogen gas (H₂) flow rate from 25 standard cubic centimeters per minute (sccm) to 100 sccm and CVD temperature (T_growth) from 400 to 800 °C, yielded graphene films of varying quality as characterized by Raman spectroscopy. The optimal graphene growth parameters were found to occur with a hydrogen flow rate of 75 sccm sweeping the 180 °C source carbon past the Cu foil at 600 °C for 1 min. The deposition at 600 °C with a H₂ flow rate of 75 sccm yielded a 2D band peak with ~53.4 cm^-1 FWHM and a relative intensity ratio of the G to 2D bands (I_G/I_2D) of 0.21. This recipe fabricated a few layers of good quality graphene.

Keywords: graphene, chemical vapor deposition, carbon source, low temperature growth

Procedia PDF Downloads 136

Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

Abstract:

In this work, the effect of particle size on the structural and magnetic properties of CoFe2-xGdxO4 (x =0.1) spinel ferrite nanoparticles synthesized by starch-assisted sol-gel auto combustion method was investigated. The different sized CoFe2-xGdxO4 (x =0.1) spinel ferrite nanoparticles were achieved after annealing at different temperature 500, 700 and 900 oC. The structural phases, crystallite size and lattice parameter of synthesized ferrite nanoparticles were estimated from X-ray diffraction studies. The field emission scanning electron microscopy study demonstrated increase in particle size with increase of annealing temperature. Raman spectroscopy study indicated the change in octahedral and tetrahedral site related Raman modes in Gd3+ ions doped cobalt ferrite nanoparticles. An infrared spectroscopy study showed the presence of two absorption bands in the frequency range around 580 cm-1 (ν1) and around 340 cm-1 (ν2); which indicated the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Vibrating Sample magnetometer study showed that the saturation magnetization and coercivity changes with particle size of CoFe2-xGdxO4 (x =0.1) spinel ferrite.

Keywords: magnetic properties, spinel ferrite, nanoparticles, sol-gel synthesis

Procedia PDF Downloads 461