Search results for: energy-dispersive X-ray spectroscopy

Authors: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq

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Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si₃N₄ confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N₂ plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: crystallinity, glow discharge, nitriding, sputtering

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

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In this present work, CoFe2-xNdxO4 (0.0 ≤ x ≥0.1) spinel ferrite nanoparticles were synthesized by starch-assisted sol-gel auto-combustion method. Powder X-ray diffraction patterns were revealed the formation of cubic spinel ferrite with the signature of NdFeO3 phase at higher Nd3+ concentration. The field emission scanning electron microscopy study demonstrated the spherical nanoparticle in the size range between 5-15 nm. Raman and Fourier Transform Infrared spectra supported the formation of the spinel ferrite structure in the nanocrystalline form. The X-ray photoelectron spectroscopy (XPS) analysis confirmed the presence of Co2+ and Fe3+ at octahedral as well as a tetrahedral site in CoFe2-xNdxO4 nanoparticles. The change in magnetic properties with a variation of concentration of Nd3+ ions in cobalt ferrite nanoparticles was observed.

Keywords: nanoparticles, spinel ferrites, sol-gel auto-combustion method, CoFe2-xNdxO4

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Authors: Arslan Usman, Abdul Sattar, Hamid Latif, Afshan Ashfaq, Muhammad Rafique, Martin Koch

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Two-dimensional materials have promising applications in optoelectronic and photonics; MoS₂ is the pioneer 2D material in the family of transition metal dichalcogenides. Its optical, optoelectronic, and structural properties are of practical importance along with its exciton dynamics. Exciton, along with exciton complexes, plays a vital role in realizing quantum devices. MoS₂ monolayers were synthesized using chemical vapour deposition (CVD) technique on SiO₂ and hBN substrates. Photoluminescence spectroscopy (PL) was used to identify the monolayer, which also reflects the substrate based peak broadening due to screening effects. In-plane and out of plane characteristic vibrational modes E¹₂g and A₁g, respectively, were detected in a different configuration on the substrate. The B-excitons and trions showed a dominant feature at low temperatures due to electron-phonon coupling effects, whereas their energies are separated by 100 meV.

Keywords: 2D materials, photoluminescence, AFM, excitons

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Authors: Yamina Zouambia, Khadidja Youcef Ettoumi, Mohamed Krea, Nadji Moulai Mostefa

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Environment pollution through various wastes (particularly by heavy metals) is a major environmental problem due to industrialization and the development of various human activities. Considerable attention has been focused, in recent years, upon the field of biosorption which represents a biotechnological innovation as well as an excellent tool for removal of metal ions from aqueous effluents. So the purpose of this study is to valorize by-product which are orange peels and an extract of these peels (pectin; a heteropolysaccharide) in treatment of water containing heavy metals. All biosorption experiments were carried out at room temperature, an indicated pH, a precise amount of biosorbent and under continuous stirring. Biosorption kinetic was determined by evaluating the residual concentration of the metal ion at different time intervals using UV spectroscopy. The results obtained show that the orange peels and pectin are interesting biosorbents with maximum biosorption capacity of up to 140 mg/g.

Keywords: orange peels, pectin, heavy metals, biosorption

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Authors: Abdelrahman Mohamed

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The ancient Egyptians used canopic vessels in embalming operations in order to preserve the guts of the mummified corpse. Canopic vessels were made of many materials, including pottery and glazed pottery. In this research, we study a pottery canopic vessel and a glazed pottery vessel. An analysis to find out the compounds and elements of the materials from which the container is made and the colors, and also to make some analysis for the organic materials present inside it, such as the Fourier Transform Infrared Spectroscopy analysis and the Gas chromatograph mass spectrometers analysis of the organic residue. Through the study and analysis, it was proved that some of the materials present in the pot were coniferous oil and animal fats. In the other pot, the analysis showed the presence of some plant resins (mastic) inside rolls of linen. Restoration operations were carried out, such as mechanical cleaning, strengthening, and completing the reinforcement of the pots.

Keywords: canopic jar, embalming, FTIR, GCMS, linen.

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Authors: S. Raeis Farshid, B. Raeis Farshid

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Ag-TiO₂ nanocomposites were prepared by the sol-gel method with and without additives such as carboxy methyl cellulose (CMC), polyethylene glycol (PEG), polyvinyl pyrrolidone (PVP), and hydroxyl propyl cellulose (HPC). The characteristics of the prepared Ag-TiO₂ nanocomposites were identified by Fourier Transform Infra-Red spectroscopy (FTIR), X-Ray Diffraction (XRD), and scanning electron microscopy (SEM) methods. The additives have a significant effect on the particle size distribution and photocatalytic activity of Ag-TiO₂ nanocomposites. SEM images have shown that the particle size distribution of Ag-TiO₂ nanocomposite in the presence of HPC was the best in comparison to the other samples. The photocatalytic activity of the synthesized nanocomposites was investigated for decolorization of methyl orange (MO) in water under UV-irradiation in a batch reactor, and the results showed that the photocatalytic activity of the nanocomposites had been increased by CMC, PEG, PVP, and HPC, respectively.

Keywords: sol-gel method, Ag-TiO₂, decolorization, photocatalyst, nanocomposite

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Authors: Mohamed Abd Elfattah Ibraheem Elghrbawy

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Icons are a significant group of cultural heritage objects that deserve to be maintained and conserved, as these ions are performed according to religious standards and norms. The ideal structure of icons is five strata, the lower layer is a wood plate, and the upper layer is the varnish layer that is exposed to photo-oxidation, that is turned into a fragile yellow layer. In addition, the components of the icons are important in dating these ions, so X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), and Scanning Electron Microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) patterns were used. SEM-EDX pattern revealed that the red pigment was vermillion (HgS), that was used in the late period, with a slight difference from the synthesized pigment. Pigments were subjected to chromatic alteration due to different agents, such as microbial agents and pollutants, in particular SO₂, whereas the pigment-based pigments are more sensitive. Moreover, cleaning, varnish removal, and retouching are important processes in the conservation of icons.

Keywords: conservation, cultural heritage, Egyptian icon, pigments

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Authors: Ewelina Nowak, Anna Wisla-Swider, Krzysztof Danel

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Aqueous suspensions of DNA were illuminated with linearly polarized visible light and ultraviolet for 5, 15, 20 and 40 h. In order to check the nature of modification, DNA interactions were characterized by FTIR spectroscopy. For each illuminated sample, weight average molecular weight and hydrodynamic radius were measured by high pressure size exclusion chromatography. Resulting optical changes for illuminated DNA were investigated using UV-Vis spectra and photoluminescent. Optical properties show potential application in sensors based on modified DNA. Then selected DNA-surfactant complexes were illuminated with electromagnetic radiation for 5h. Molecular structure, optical characteristic were examinated for obtained complexes. Illumination led to changes of complexes physicochemical properties as compared with native DNA. Observed changes were induced by rearrangement of the molecular structure of DNA chains.

Keywords: biopolymers, deoxyribonucleic acid, ionic liquids, linearly polarized visible light, ultraviolet

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Authors: Priyanka R. Oberoi, Chandra B. Maurya, Prakash A. Mahanwar

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Ionizing radiation can cause a drastic change in the physical and chemical properties of the material exposed. Numerous medical devices are sterilized by ionizing radiation. In the current research paper, an attempt was made to develop precise and inexpensive polymeric film dosimeter which can be used for controlling radiation dosage. Polymeric film containing (pH sensitive dye) indicator dye Bromophenol blue (BPB) was casted to check the effect of Gamma radiation on its optical and physical properties. The film was exposed to gamma radiation at 4 kGy/hr in the range of 0 to 300 kGy at an interval of 50 kGy. Release of vinyl acetate from an emulsion on high radiation reacts with the BPB fading the color of the film from blue to light blue and then finally colorless, indicating a change in pH from basic to acidic form. The change was characterized by using CIE l*a*b*, ultra-violet spectroscopy and FT-IR respectively.

Keywords: bromophenol blue, dosimeter, gamma radiation, polymer

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Authors: Maryam Kiani, Abdul Basit Kiani

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Simple hydrothermal method to synthesize new nanocomposites consisting of nitrogen-doped graphene and NiFe₂O₄. By analyzing the X-Ray Powder Diffraction (XRD) images, we confirmed that the NiFe₂O₄ phase is pure and has a Face Centered Cubic (FCC) structure. The average size of the NiFe₂O₄ nanoparticles is approximately 40±2 nm. Additionally, we used X-ray photoelectron spectroscopy (XPS) to study the surface chemical composition and cation oxidation states of both the NiFe₂O₄ nanoparticles and the nitrogen-doped graphene/NiFe₂O₄ nanocomposites. A magnetic interaction between nitrogen doped graphene/NiFe₂O₄ was studied. Increases in hydrothermal synthesis temperature lead to the improved crystalline structure of NiFe₂O₄ nanoparticles, which improves the magnetic properties.

Keywords: nickel ferrite spinal, nitrogen doped graphene, magnetic nanocomposite, hydrothermal synthesis

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Authors: Shrikaant Kulkarni, Akshata Naik Nimbalkar

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

Keywords: bifunctional, next generation material, Co3O4, XRD

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Authors: Fatemeh Rezaei, Babak Shokri

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In this study, PMMA films are modified by oxygen plasma treatment for biomedical applications. The plasma generator is capacitively coupled radio frequency (13.56 MHz) power source. The oxygen pressure and gas flow rate are kept constant at 40 mTorr and 30 sccm, respectively and samples are treated for 2 minutes. Hydrophilicity and biocompatibility of PMMA films are studied before and after treatments in different applied powers (10-80 W). In order to monitor the plasma process, the optical emission spectroscopy is used. The wettability and cellular response of samples are investigated by water contact angle (WCA) analysis and MTT assay, respectively. Also, surface free energy (SFE) variations are studied based on the contact angle measurements of three liquids. It is found that RF oxygen plasma treatment enhances the biocompatibility and also hydrophilicity of PMMA films.

Keywords: cellular response, hydrophilicity, MTT assay, PMMA, RF plasma

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

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

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

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Authors: Ali Akbar Kazemi Asl, Mansour Rahsepar

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

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

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Authors: Issam Derkaoui, Mohammed Khenfouch, Bakang M. Mothudi, Malik Maaza, Izeddine Zorkani, Anouar Jorio

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Transition metal oxides nanoparticles with different morphologies have attracted a lot of attention recently owning to their distinctive geometries, and demonstrated promising electrical properties for various applications. In this paper, we discuss the time and annealing effects on the structural and electrical properties of vanadium oxides nanoparticles (VO-NPs) prepared by microwave method. In this sense, transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman Spectroscopy, Ultraviolet-visible absorbance spectra (Uv-Vis) and electrical conductivity were investigated. Hence, the annealing state and the time are two crucial parameters for the improvement of the optoelectronic properties. The use of these nanostructures is promising way for the development of technological applications especially for energy storage devices.

Keywords: Vanadium oxide, Microwave, Electrical conductivity, Optoelectronic properties

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Authors: Bhupinder Kaur, O. P. Pandey

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An automobile industry is using variety of materials for better comfort and utility. The present work describes the details of failure analysis done for windshield glass of a four-wheeler class. The failure occurred in two different models of the heavy duty class of four wheelers, which analysed separately. The company reported that the failure has occurred only in their rear windshield when vehicles parked under shade for several days. These glasses were characterised by dilatometer, differential thermal analyzer, and X-ray diffraction. The glasses were further investigated under scanning electron microscope with energy dispersive X-ray spectroscopy and X-ray dot mapping. The microstructural analysis of the glasses done at the surface as well as at the fractured area indicates that carbon as an impurity got segregated as banded structure throughout the glass. Since carbon absorbs higher heat, it causes thermal mismatch to the entire glass system, and glass shattered down. In this work, the details of sequential analysis done to predict the cause of failure are present.

Keywords: failure, windshield, thermal mismatch, carbon

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Authors: JongWon Han, NoHoon Kim, HyoIk Ahn, HaeWoo Lee

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In this study, shielded metal arc welding was performed as a function of Nb content at 2.24 wt%, 3.25 wt%, and 4.26 wt%. The microstructure was observed using scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and showed the development of a columnar dendrite structure in the specimen having the least Nb content. From the hardness test, the hardness value was confirmed to reduce with decreasing Nb content. From electron backscatter diffraction (EBSD) analysis, the largest grain size was found in the specimen with Nb content of 2.24 wt%. The potentiodynamic polarization test was carried out to determine the pitting corrosion resistance; there was no significant difference in the pitting corrosion resistance with increasing Nb content. To evaluate the degree of sensitization to intergranular corrosion, the Double Loop Electrochemical Potentiodynamic Reactivation(DL-EPR test) was conducted. A similar degree of sensitization was found in two specimens except with a Nb content of 2.24 wt%, while a relatively high degree of sensitization was found in the specimen with a Nb content of 2.24 wt%.

Keywords: inconel 625, Nb content, potentiodynamic test, DL-EPR test

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Authors: Ambrish Singh

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

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

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Authors: Flavio A. F. Da Ponte, Jackson Q. Malveira, Monica C. G. Albuquerque

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In recent years a worldwide interest in renewable resources from the biomass has spurred the industry. In this work the chemical structure of oleic acid chains was modified by homogeneous and heterogeneous catalysis in order to produce esters. The homogeneous epoxidation was carried out at H2O2 to oleic acid unsaturation molar ratio of 20:1. The reaction temperature was 338 K and reaction time 16 h. Formic acid was used as catalyst. For heterogeneous catalysis reaction temperature was 343 K and reaction time 24 h. The esters production was carried out by heterogeneous catalysis of the epoxidized oleic acid and butanol using Mg/SBA-15 as catalyst. The resulting products were confirmed by NMR (1H and 13C) and FTIR spectroscopy. The products were characterized before and after each reaction. The catalysts were characterized by X-ray diffraction, X-ray fluorescence, thermogravimetric analysis (TGA) and BET surface areas. The results were satisfactory for the bioproducts formed.

Keywords: acid oleic, bioproduct, esters, epoxidation

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

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

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

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Authors: Dhuha Albusalih, David Weston, Simon Gill

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Nanocomposites Co-SiC with well dispersed nanoparticles and Co nano grain size has produced using Pulse Reverse Plating (PRP) and using anionic surfactant. Different particle contents of nanocomposites were produced by altering the plating parameters. The method allows great control over the level of nanoparticles in the coating, without changing bath chemistry. Examination by Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDX), TEM and X-Ray Diffraction (XRD) analysis was performed to characterize and study the strengthening mechanisms of these nanocomposites. The primary strengthening mechanisms were shown to be grain refinement and dispersion strengthening. Tribological performances of the produced electroplated nanocomposite Co-SiC coatings were examined. Results showed that the coating with the higher volume fraction (vol. %) of SiC and the smallest grain size has the higher hardness and low wear rate.

Keywords: nanocomposites, pulse reverse plating, tribological performance of cobalt nanocomposites

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Authors: Md. Hafezur Rahaman, Mohd. Maniruzzaman, Md. Shadiqul Islam, Md. Masud Rana

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With the growth of environmental awareness, enormous researches are running to develop the next generation materials based on sustainability, eco-competence, and green chemistry to preserve and protect the environment. Due to biodegradability and biocompatibility, poly (L-lactic acid) (PLLA) has a great interest in ecological and medical applications. Also, cellulose is one of the most abundant biodegradable, renewable polymers found in nature. It has several advantages such as low cost, high mechanical strength, biodegradability and so on. Recently, an immense deal of attention has been paid for the scientific and technological development of α-cellulose based composite material. PLLA could be used for grafting of cellulose to improve the compatibility prior to the composite preparation. Here it is quite difficult to form a bond between lower hydrophilic molecules like PLLA and α-cellulose. Dimmers and oligomers can easily be grafted onto the surface of the cellulose by ring opening or polycondensation method due to their low molecular weight. In this research, α-cellulose extracted from jute fiber is grafted with oligo(D-lactic acid) (ODLA) via graft polycondensation reaction in presence of para-toluene sulphonic acid and potassium persulphate in toluene at 130°C for 9 hours under 380 mmHg. Here ODLA is synthesized by ring opening polymerization of D-lactides in the presence of stannous octoate (0.03 wt% of lactide) and D-lactic acids at 140°C for 10 hours. Composites of PLLA with ODLA grafted α-cellulose are prepared by solution mixing and film casting method. Confirmation of grafting was carried out through FTIR spectroscopy and SEM analysis. A strongest carbonyl peak of FTIR spectroscopy at 1728 cm⁻¹ of ODLA grafted α-cellulose confirms the grafting of ODLA onto α-cellulose which is absent in α-cellulose. It is also observed from SEM photographs that there are some white areas (spot) on ODLA grafted α-cellulose as compared to α-cellulose may indicate the grafting of ODLA and consistent with FTIR results. Analysis of the composites is carried out by FTIR, SEM, WAXD and thermal gravimetric analyzer. Most of the FTIR characteristic absorption peak of the composites shifted to higher wave number with increasing peak area may provide a confirmation that PLLA and grafted cellulose have better compatibility in composites via intermolecular hydrogen bonding and this supports previously published results. Grafted α-cellulose distributions in composites are uniform which is observed by SEM analysis. WAXD studied show that only homo-crystalline structures of PLLA present in the composites. Thermal stability of the composites is enhanced with increasing the percentages of ODLA grafted α-cellulose in composites. As a consequence, the resultant composites have a resistance toward the thermal degradation. The effects of length of the grafted chain and biodegradability of the composites will be studied in further research.

Keywords: α-cellulose, composite, graft polycondensation, oligo(D-lactic acid), poly(L-lactic acid)

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Authors: Brajendra S. Sengar, Vivek Garg, Gaurav Siddharth, Nisheka Anadkat, Amitesh Kumar, Shaibal Mukherjee

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The optimal band gap (~ 1 to 1.5 eV) and high absorption coefficient ~104 cm⁻¹ has made Cu₂ZnSn(S,Se)₄ (CZTSSe) films as one of the most promising absorber materials in thin-film photovoltaics. Additionally, CZTSSe consists of elements that are abundant and non-toxic, makes it even more favourable. The CZTSSe thin films are grown at 100 to 500ᵒC substrate temperature (Tsub) on Soda lime glass (SLG) substrate by Elettrorava dual ion beam sputtering (DIBS) system by utilizing a target at 2.43x10⁻⁴ mbar working pressure with RF power of 45 W in argon ambient. The chemical composition, depth profiling, structural properties and optical properties of these CZTSSe thin films prepared on SLG were examined by energy dispersive X-ray spectroscopy (EDX, Oxford Instruments), Hiden secondary ion mass spectroscopy (SIMS) workstation with oxygen ion gun of energy up to 5 keV, X-ray diffraction (XRD) (Rigaku Cu Kα radiation, λ=.154nm) and Spectroscopic Ellipsometry (SE, M-2000D from J. A. Woollam Co., Inc). It is observed that from that, the thin films deposited at Tsub=200 and 300°C show Cu-poor and Zn-rich states (i.e., Cu/(Zn + Sn) < 1 and Zn/Sn > 1), which is not the case for films grown at other Tsub. It has been reported that the CZTSSe thin films with the highest efficiency are typically at Cu-poor and Zn-rich states. The values of band gap in the fundamental absorption region of CZTSSe are found to be in the range of 1.23-1.70 eV depending upon the Cu/(Zn+Sn) ratio. It is also observed that there is a decline in optical band gap with the increase in Cu/(Zn+Sn) ratio (evaluated from EDX measurement). Cu-poor films are found to have higher optical band gap than Cu-rich films. The decrease in the band gap with the increase in Cu content in case of CZTSSe films may be attributed to changes in the extent of p-d hybridization between Cu d-levels and (S, Se) p-levels. CZTSSe thin films with Cu/(Zn+Sn) ratio in the range 0.86–1.5 have been successfully deposited using DIBS. Optical band gap of the films is found to vary from 1.23 to 1.70 eV based on Cu/(Zn+Sn) ratio. CZTSe films with Cu/ (Zn+Sn) ratio of .86 are found to have optical band gap close to the ideal band gap (1.49 eV) for highest theoretical conversion efficiency. Thus by tailoring the value of Cu/(Zn+Sn), CZTSSe thin films with the desired band gap could be obtained. Acknowledgment: We are thankful to DIBS, EDX, and XRD facility equipped at Sophisticated Instrument Centre (SIC) at IIT Indore. The authors B. S. S and A. K. acknowledge CSIR, and V. G. acknowledges UGC, India for their fellowships. B. S. S is thankful to DST and IUSSTF for BASE Internship Award. Prof. Shaibal Mukherjee is thankful to DST and IUSSTF for BASE Fellowship and MEITY YFRF award. This work is partially supported by DAE BRNS, DST CERI, and DST-RFBR Project under India-Russia Programme of Cooperation in Science and Technology. We are thankful to Mukul Gupta for SIMS facility equipped at UGC-DAE Indore.

Keywords: CZTSSe, DIBS, EDX, solar cell

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Authors: Kiran Jose, Anjana J. G., Venu Anand, Aswathi R. Nair

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This work investigates the change in structural, optical, and electrical properties of Zinc Oxynitride (ZnON) thin film when annealed in different atmospheres. ZnON film is prepared by reactively sputtering the Zinc target using argon, oxygen, and nitrogen. The deposited film is annealed for one hour at 3250C in the Vaccum condition and Nitrogen and oxygen atmospheres. XRD and Raman spectroscopy is used to study the structural properties of samples. The current conduction mechanism is examined by extracting voltage versus current characteristics on a logarithmic scale, and the optical response is quantified by analyzing persistent photoconductivity (PPC) behavior. This study proposes the optimum annealing atmosphere for ZnON thin film for a better transistor and photosensor application.

Keywords: Zinc oxynitride, thin film, annealing, DC sputtering

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Authors: Selma Hamimed, Abdelwaheb Chatti

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

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

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Authors: M. N. Akhtar, J. N. Akhtar

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The present study evaluates the properties of class F fly ash as a replacement of natural materials in civil engineering construction industry. The low-lime flash similar to class F is the prime variety generated in India, although it has significantly smaller volumes of high-lime fly ash as compared to class C. The chemical and physical characterization of the sample is carried out with the number of experimental approaches in order to investigate all relevant features present in the samples. For chemical analysis, elementary quantitative results from point analysis and scanning electron microscopy (SEM)/dispersive spectroscopy (EDS) techniques were used to identify the element images of different fractions. The physical properties found very close to the range of common soils. Furthermore, the fly ash-based bricks were prepared by the same sample of class F fly ash and the results of compressive strength similar to that of Standard Clay Brick Grade 1 available in the local market of India.

Keywords: fly ash, class F, class C, chemical, physical, SEM, EDS

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Authors: L. Rozumová, J. Seidlerová

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

Keywords: blast furnace sludge, lead, zinc, sorption

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Authors: Siva Prasad Peddi

Abstract:

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

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

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Authors: Gurpreet Singh, Hazoor Singh, Buta Singh Sidhu

Abstract:

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

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

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Authors: M. Shopska, D. Paneva, G. Kadinov, Z. Cherkezova-Zheleva, I. Mitov

Abstract:

The iron containing materials are used as catalysts in different processes. The chemical methods of their synthesis use toxic and expensive chemicals; sophisticated devices; energy consumption processes that raise their cost. Besides, dangerous waste products are formed. At present time such syntheses are out of date and wasteless technologies are indispensable. The bioinspired technologies are consistent with the ecological requirements. Different microorganisms participate in the biomineralization of the iron and some phytochemicals are involved, too. The methods for biogenic production of iron containing materials are clean, simple, nontoxic, realized at ambient temperature and pressure, cheaper. The biogenic iron materials embrace different iron compounds. Due to their origin these substances are nanosized, amorphous or poorly crystalline, porous and have number of useful properties like SPM, high magnetism, low toxicity, biocompatibility, absorption of microwaves, high surface area/volume ratio, active sites on the surface with unusual coordination that distinguish them from the bulk materials. The biogenic iron materials are applied in the heterogeneous catalysis in different roles - precursor, active component, support, immobilizer. The application of biogenic iron oxide materials gives rise to increased catalytic activity in comparison with those of abiotic origin. In our study we investigated the catalytic behavior of biomasses obtained by cultivation of Leptothrix bacteria in three nutrition media – Adler, Fedorov, and Lieske. The biomass composition was studied by Moessbauer spectroscopy and transmission IRS. Catalytic experiments on CO oxidation were carried out using in situ DRIFTS. Our results showed that: i) the used biomasses contain α-FeOOH, γ-FeOOH, γ-Fe2O3 in different ratios; ii) the biomass formed in Adler medium contains γ-FeOOH as main phase. The CO conversion was about 50% as evaluated by decreased integrated band intensity in the gas mixture spectra during the reaction. The main phase in the spent sample is γ-Fe2O3; iii) the biomass formed in Lieske medium contains α-FeOOH. The CO conversion was about 20%. The main phase in the spent sample is α-Fe2O3; iv) the biomass formed in Fedorov medium contains γ-Fe2O3 as main phase. CO conversion in the test reaction was about 19%. The results showed that the catalytic activity up to 200°C resulted predominantly from α-FeOOH and γ-FeOOH. The catalytic activity at temperatures higher than 200°C was due to the formation of γ-Fe2O3. The oxyhydroxides, which are the principal compounds in the biomass, have low catalytic activity in the used reaction; the maghemite has relatively good catalytic activity; the hematite has activity commensurate with that of the oxyhydroxides. Moreover it can be affirmed that catalytic activity is inherent in maghemite, which is obtained by transformation of the biogenic lepidocrocite, i.e. it has biogenic precursor.

Keywords: nanosized biogenic iron compounds, catalytic behavior in reaction of CO oxidation, in situ DRIFTS, Moessbauer spectroscopy

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