Search results for: HRTEM

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: I. Shuro

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The crystal structure of Tin Sulfide prepared by certain chemical methods is investigated using High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), and X-ray diffraction (XRD) methods. An anomalous HRTEM Fast Fourier Transform (FFT) exhibited a central scatter of diffraction spots, which is surrounded by secondary clusters of spots arranged in a hexagonal pattern around the central cluster was observed. FFT analysis has revealed a long lattice parameter and mostly viewed along a hexagonal axis where there many columns of atoms slightly displaced from one another. This FFT analysis has revealed that the metal sulfide has a long-range order interwoven chain of atoms in its crystal structure. The observed crystalline structure is inconsistent with commonly observed FFT patterns of chemically synthesized Tin Sulfide nanocrystals and thin films. SEM analysis showed the morphology of a myriad of multi-shaped crystals ranging from hexagonal, cubic, and spherical micro to nanostructured crystals. This study also investigates the presence of quasi-crystals as reflected by the presence of mixed local symmetries.

Keywords: fast fourier transform, high resolution transmission electron microscopy, tin sulfide, crystalline structure

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Authors: Elitsa N. Kolentsova, Dimitar Y. Dimitrov, Petya Cv. Petrova, Georgi V. Avdeev, Diana D. Nihtianova, Krasimir I. Ivanov, Tatyana T. Tabakova

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Recently, copper and manganese-containing systems are recognized as active and selective catalysts in many oxidation reactions. The main idea of this study is to obtain more information about γ-Al₂O₃ supported Cu-La catalysts and to evaluate their activity to simultaneous oxidation of CO, CH₃OH and dimethyl ether (DME). The catalysts were synthesized by impregnation of support with a mixed aqueous solution of nitrates of copper, manganese and lanthanum under different conditions. XRD, HRTEM/EDS, TPR and thermal analysis were performed to investigate catalysts’ bulk and surface properties. The texture characteristics were determined by Quantachrome Instruments NOVA 1200e specific surface area and pore analyzer. The catalytic measurements of single compounds oxidation were carried out on continuous flow equipment with a four-channel isothermal stainless steel reactor in a wide temperature range. On the basis of XRD analysis and HRTEM/EDS, it was concluded that the active component of the mixed Cu-Mn-La/γ–alumina catalysts strongly depends on the Cu/Mn molar ratio and consisted of at least four compounds – CuO, La₂O₃, MnO₂ and Cu_1.5Mn_1.5O₄. A homogeneous distribution of the active component on the carrier surface was found. The chemical composition strongly influenced catalytic properties. This influence was quite variable with regards to the different processes.

Keywords: Cu-Mn-La oxide catalysts, carbon oxide, VOCs, deep oxidation

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Authors: Michael Regev, Shai Essel, Alexander Katz-Demyanetz

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Magnesium alloys are characterized by good physical properties: They exhibit high strength, are lightweight and have good damping absorption and good thermal and electrical conductivity. Amorphous magnesium alloys, moreover, exhibit higher strength, hardness and a large elastic domain in addition to having excellent corrosion resistance. These above-mentioned advantages make magnesium based metallic glasses attractive for industrial use. Among the various existing magnesium alloys, Mg₆₅Cu₂₅Y₁₀ alloy is known to be one of the best glass formers. In the current study, Mg₆₅Cu₂₅Y₁₀ ribbons were produced by melt spinning, their microstructure was investigated in its as-cast condition, after pressing under 0.5 GPa for 5 minutes under different temperatures - RT, 500C, 1000C, 1500C and 2000C - and after five minute exposure to the above temperatures without pressing. The microstructure was characterized by means of X-ray Diffraction (XRD), Differential Scanning Calorimetry (DSC), High Resolution Scanning Electron Microscope (HRSEM) and High Resolution Transmission Electron Microscopy (HRTEM). XRD and DSC studies showed that the as-cast material had an amorphous character and that the material crystallized during exposure to temperature with or without applying stress. HRTEM revealed that the as-cast Mg65Cu25Y10, although known to be one of the best glass formers, is nano-crystalline rather than amorphous. The current study casts light on the question what an amorphous alloy is and whether there is any clear borderline between amorphous and nano-crystalline alloys.

Keywords: metallic glass, magnesium, melt spinning, amorphous alloys

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Authors: Fatai O. Oladoyinbo, Felix O. Sanni, Akinwunmi Fatai, Kamoli A. Amusa, Saheed A. Ganiyu, Wasiu B. Ayinde, Tajudeen A. Afolabi, Enock O. Dare

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Silver (Ag) and silica (SiO2) nanoparticles were synthesized using the chemical reduction method from silver nitrate and sodium silicate, respectively. X-ray Diffraction (XRD), High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), Uv-Visible spectroscopy, Energy Dispersive X-ray (EDX) spectroscopy and N2 adsorption-desorption techniques were utilized to characterize the composition and structure of the samples. The crystallinity pattern of Ag nanoparticles was indexed as (111), (200), (220) and (311), which allowed reflections from face-centered cubic silver. XRD of SiO2 showed good porosity with a broad-spectrum band at Bragg’s angle 2θ of 22° while that of Ag-SiO2 showed distinct peaks at 2θ values of 39°, 43°, 66° and 79°. The XRD result agreed perfectly with the SEM and HRTEM images which showed Ag-SiO2 isotropic and anisotropic under the varying concentration of reactants. The elemental composition of Ag-SiO2, as displayed by EDX, confirmed Ag enrichment in the Ag-SiO2 heterostructure. The Uv-Visible peak at 421 nm confirmed the Surface Plasmon Resonance absorption peak of silver nanoparticles. N2 adsorption-desorption result showed a broad band of Ag-SiO2 from 3 to 8 nm, which indicated relatively narrow pore size distributions. Humidity sensing measurements performed in a controlled humidity chamber showed very high sensitivity with a sensitivity factor (SF) of 4.63 and high linearity with a steady decrease in resistance to humidity from 880 Ω at 10% RH to 190 Ω at 100% RH, indicating that Ag-SiO2 nanocomposite is a good sensing material with high sensitivity and linearity.

Keywords: silver, silica, nanocomposite, synthesis, heterostructure, core shell

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Authors: Nneka Augustina Akwu, Yougasphree Naidoo

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Molecular advancement in technology has created a means whereby the atoms and molecules (solid forms) of certain materials such as plants, can now be reduced to a range of 1-100 nanometres. Green synthesis of silver nanoparticles (AgNPs) was carried out at room temperature (RT) 25 ± 2°C and 80°C, using the metabolites in the aqueous extracts of the leaves and stem bark of Grewia lasiocarpa as reductants and stabilizing agents. The biosynthesized AgNPs were characterized by UV-Vis spectrophotometry, attenuated total reflectance - Fourier transforms infrared (ATR-FTIR) spectroscopy, nanoparticle tracking analysis (NTA), Energy Dispersive X-ray fluorescence scanning electron microscope (SEM-EDXRF) and high-resolution transmission electron microscopy (HRTEM). The AgNPs were biologically evaluated for antioxidant, antibacterial and cytotoxicity activities. The phytochemical and FTIR analyses revealed the presence of metabolites that act as reducing and capping agents, while the UV-Vis spectroscopy of the biosynthesized NPs showed absorption between 380-460 nm, confirming AgNP synthesis. The Zeta potential values were between -9.1 and -20.6 mV with a hydrodynamics diameter ranging from 38.3 to 46.7 nm. SEM and HRTEM analyses revealed that AgNPs were predominately spherical with an average particle size of 2- 31 nm for the leaves and 5-27 nm for the stem bark. The cytotoxicity IC50 values of the AgNPs against HeLa, Caco-2 and MCF-7 were >1 mg/mL. The AgNPs were sensitive to all strains of bacteria used, with methicillin-resistant Staphylococcus aureus (MRSA), Staphylococcus aureus (ATCC 25923) and Escherichia coli (ATCC 25922) being more sensitive to the AgNPs. Our findings propose that antibacterial and anticancer agents could be derived from these AgNPs of G. lasiocarpa, and warrant their further investigation.

Keywords: antioxidant, cytotoxicity, Grewia lasiocarpa, silver nanoparticles, Zeta potentials

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Authors: Haiming Wen, Isabella J. Van Rooyen

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Tristructural isotropic (TRISO)-coated fuel particles are designed as nuclear fuel for high-temperature gas reactors. TRISO coating consists of layers of carbon buffer, inner pyrolytic carbon (IPyC), SiC, and outer pyrolytic carbon. The TRISO coating, especially the SiC layer, acts as a containment system for fission products produced in the kernel. However, release of certain metallic fission products across intact TRISO coatings has been observed for decades. Despite numerous studies, mechanisms by which fission products migrate across the coating layers remain poorly understood. In this study, scanning transmission electron microscopy (STEM), energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS) were used to examine the distribution, composition and structure of fission products in a TRISO coated particle neutron irradiated to 3.6 x 1021 n/cm² fast fluence at 1040 ⁰C. Precession electron diffraction was used to investigate characters of grain boundaries where specific fission product precipitates are located. The retention fraction of 110mAg in the investigated TRISO particle was estimated to be 0.19. A high density of nanoscale fission product precipitates was observed in the SiC layer close to the SiC-IPyC interface, most of which are rich in Pd, while Ag was not identified. Some Pd-rich precipitates contain U. Precipitates tend to have complex structure and composition. Although a precipitate appears to have uniform contrast in STEM, EDS indicated that there may be composition variations throughout the precipitate, and HRTEM suggested that the precipitate may have several parts different in crystal structure or orientation. Attempts were made to measure charge states of precipitates using EELS and study their possible effect on precipitate transport.

Keywords: TRISO particle, fission product, nuclear fuel, electron microscopy, neutron irradiation

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Authors: S. Manjunatha, M. S. Dharmaprakash

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Well-defined 2D Eu⁺³ co-doped ZrO₂: Gd⁺³ nanoparticles were successfully synthesized by microwave assisted solution combustion technique for luminescent applications. The present investigation reports the rapid and effective method for the synthesis of the Eu⁺³ co-doped ZrO₂:Gd⁺³ nanoparticles and study of the luminescence behavior of Eu⁺³ ion in ZrO₂:Gd⁺³ nanostructures. The optical properties of the prepared nanostructures were investigated by using UV-visible spectroscopy and photoluminescence spectra. The phase formation and the morphology of the nanoplatelets were studied by XRD, FESEM and HRTEM. The average grain size was found to be 45-50 nm. The presence of Gd³⁺ ion increases the crystallinity of the material and hence acts as a good nucleating agent. The ZrO₂:Gd³⁺ co-doped with Eu⁺³ nanoplatelets gives an emission at 607 nm, a strong red emission under the excitation wavelength of 255 nm.

Keywords: nanoparticles, XRD, TEM, photoluminescence

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Authors: Ali Moafi, Kourosh Kalantarzadeh, Richard Kaner, Parviz Parvin, Ebrahim Asl Soleimani, Dougal McCulloch

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In-situ Raman spectroscopy of flexible graphene-oxide films examined upon exposure to hydrogen gas, air, and synthetic air. The changes in D and G peaks are attributed to defects responding to atomic hydrogen spilled over from the catalytic behavior of Pt nanoparticles distributed all over the film. High-resolution transmission electron microscopy images (HRTEM) as well as electron energy loss spectroscopy (EELS) were carried out to define the density of the samples.

Keywords: in situ Raman Spectroscopy, EELS, TEM, graphene oxide, graphene, atomic hydrogen

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Authors: Mingmei Zhang, Xinyong Li

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AgInS₂/SnS₂ (AIS) nanocomposites were synthesized by a simple hydrothermal method. The morphology and composition of the fabricated AIS nanocomposites were investigated by field-emission scanning electron microscopy (SEM), X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). Moreover, the as-prepared AIS photocatalysts exhibited excellent photocatalytic activities for the degradation of Norfloxacin (NOR), mainly due to its high optical absorption and separation efficiency of photogenerated electron-hole pairs, as evidenced by UV–vis diffusion reflection spectra (DRS) and Surface photovoltage (SPV) spectra. Furthermore, the interfacial charges transfer mechanism was also discussed by DFT calculations.

Keywords: AIS nanocomposites, electron-hole pairs, charges transfer, DFTcaculations

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

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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: Masood Hussain, Erol Pehlivan, Ahmet Avci, Ecem Guder

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Green synthesis of silver nanoparticles (AgNPs) was carried out by using echinacea flower extract as reducing/protecting agent. The effects of various operating parameters and additives on the dimensions such as stirring rate, temperature, pH of the solution, the amount of extract and concentration of silver nitrate were optimized in order to achieve monodispersed spherical and small size echinacea protected silver nanoparticles (echinacea-AgNPs) through biosynthetic method. The surface roughness and topography of synthesized metal nanoparticles were confirmed by using Atomic Force Microscopy (AFM). High-Resolution Transmission Electron Microscopic (HRTEM) results elaborated the formation of uniformly distributed Echinacea protected AgNPs (Echinacea-AgNPs) having an average size of 30.2±2nm.

Keywords: Echinacea flower extract, green synthesis, silver nanoparticles, morphology

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Authors: Z. Ghorannevis, E. Akbarnejad, B. Aghazadeh, M. Ghoranneviss

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Carbon nanotubes (CNTs) modified with semiconductor nanocrystalline particles may find wide applications due to their unique properties. Here Cadmium Sulfide (CdS) nanoparticles were successfully grown on Multi-Walled Carbon Nanotubes (MWNTs) via a magnetron sputtering method for the first time. The CdS/MWNTs sample was characterized with X-ray diffraction (XRD), Field Emission Scanning and High Resolution Transmission Electron Microscopies (SEM/TEM) and four point probe. The obtained images show clearly the decoration of the MWNTs by the CdS nanoparticles, and the XRD measurements indicate the CdS structure as hexagonal type. Moreover, the physical properties of the CdS/MWNTs were compared with the physical properties of the CdS nanoparticles grown on the silicon. Electrical measurements of CdS and CdS/MWNTs reveal that CdS/MWNTs has lower resistivity than the CdS sample which may be due to the higher carrier concentrations.

Keywords: CdS, MWNTs, HRTEM, magnetron sputtering

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Authors: Alak Kumar Patra, Nilanjan Mitra

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Higher strength to weight ratio is the main advantage of sandwich composite structures. Interfacial delamination between the face sheet and core is a major problem in these structures. Many research works are devoted to improve the interfacial fracture toughness of composites majorities of which are on nano and laminated composites. Work on influence of multiwalled carbon nano-tubes (MWCNT) dispersed resin system on interface fracture of glass-epoxy PVC core sandwich composite is extremely limited. Finite element study is followed by experimental investigation on interface fracture toughness of glass-epoxy (G/E) PVC core sandwich composite with and without MWCNT. Results demonstrate an improvement in interface fracture toughness values (Gc) of samples with a certain percentages of MWCNT. In addition, dispersion of MWCNT in epoxy resin through sonication followed by mixing of hardener and vacuum resin infusion (VRI) technology used in this study is an easy and cost effective methodology in comparison to previously adopted other methods limited to laminated composites. The study also identifies the optimum weight percentage of MWCNT addition in the resin system for maximum performance gain in interfacial fracture toughness. The results agree with finite element study, high-resolution transmission electron microscope (HRTEM) analysis and fracture micrograph of field emission scanning electron microscope (FESEM) investigation. Interface fracture toughness (GC) of the DCB sandwich samples is calculated using the compliance calibration (CC) method considering the modification due to shear. Compliance (C) vs. crack length (a) data of modified sandwich DCB specimen is fitted to a power function of crack length. The calculated mean value of the exponent n from the plots of experimental results is 2.22 and is different from the value (n=3) prescribed in ASTM D5528-01for mode 1 fracture toughness of laminate composites (which is the basis for modified compliance calibration method). Differentiating C with respect to crack length (a) and substituting it in the expression GC provides its value. The research demonstrates improvement of 14.4% in peak load carrying capacity and 34.34% in interface fracture toughness GC for samples with 1.5 wt% MWCNT (weight % being taken with respect to weight of resin) in comparison to samples without MWCNT. The paper focuses on significant improvement in experimentally determined interface fracture toughness of sandwich samples with MWCNT over the samples without MWCNT using much simpler method of sonication. Good dispersion of MWCNT was observed in HRTEM with 1.5 wt% MWCNT addition in comparison to other percentages of MWCNT. FESEM studies have also demonstrated good dispersion and fiber bridging of MWCNT in resin system. Ductility is also observed to be higher for samples with MWCNT in comparison to samples without.

Keywords: carbon nanotube, epoxy resin, foam, glass fibers, interfacial fracture, sandwich composite

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Authors: Mingmei Zhang, Xinyong Li

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Novel AgInS2/SnS2/RGO (AISR) heterojunctions photocatalysts were synthesized by simple hydrothermal method. The morphology and composition of the fabricated AISR nanocomposites were investigated by field-emission scanning electron microscopy (SEM), X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS). Moreover, the as-prepared AISR photocatalysts exhibited excellent photocatalytic activities for the degradation of Norfloxacin (NOR), mainly due to its high optical absorption and separation efficiency of photogenerated electron-hole pairs, as evidenced by UV–vis diffusion reflection spectra (DRS) and Surface photovoltage (SPV) spectra. Furthermore, laser flash photolysis technique was conducted to test the lifetime of charge carriers of the fabricated nanocomposites. The interfacial charges transfer mechanism was also discussed.

Keywords: AISR heterojunctions, electron-hole pairs, SPV spectra, charges transfer mechanism

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Authors: S. V. Prabhakar Vattikuti, Chan Byon

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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

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Authors: Huiwu Yu, Xiangyou Li, Xiaoyan Zeng

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Porous spheres have been widely used in many fields due to their attractive features. In this work, an approach for fabricating porous spheres of nanoparticles was presented, in which the nanoparticles were welded together to form micro spheres by simply irradiating the nanoparticles in liquid medium by a picosecond laser. As an example, anatase titanium dioxide was chosen as a typical material on account of its metastability. The structure and morphologies of the products were characterised by X-ray diffraction (XRD), scanning electron microscope (SEM), Raman, and high-resolution transmission electron microscopy (HRTEM), respectively. The results showed that, anatase titanium dioxide micro spheres (2-10 μm) with macroporous (10-100 nm) were prepared from nano-anatase titanium dioxide nanoparticles (10-100 nm). The formation process of polycrystalline anatase titanium dioxide microspheres was investigated with different liquid mediums and the input laser fluences. Thus, this facile laser irradiation approach might provide a way for the fabrication of porous microspheres without phase-transition.

Keywords: titanium dioxide, porous microspheres, picosecond laser, nano-welding

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Authors: Khamael M. Abualnaja, Lidija Šiller, Benjamin R. Horrocks

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Metal-enhanced luminescence of silicon nano crystals (SiNCs) was determined using two different particle sizes of silver nano particles (AgNPs). SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photo electron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. AgNPs were synthesized using photochemical reduction of AgNO3 with sodium dodecyl sulphate (SDS). The enhanced luminescence of SiNCs by AgNPs was evaluated by confocal Raman microspectroscopy. Enhancement up to ×9 and ×3 times were observed for SiNCs that mixed with AgNPs which have an average particle size of 100 nm and 30 nm, respectively. Silver NPs-enhanced luminescence of SiNCs occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs.

Keywords: silver nanoparticles, surface enhanced raman spectroscopy (SERS), silicon nanocrystals, luminescence

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Authors: Seyed Mahdi Rafiaei

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In this investigation, firstly Eu3+ doped YVO4 phosphor was synthesized using solid-state method. Then silica was coated on the surface of particles via sol-gel method. To study the influence of SiO2 addition on microstructure and photoluminescence characteristics of YVO4:4% Eu3+ phosphor materials, we employed X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High-Resolution Transmitted Electron Microscope (HRTEM), Focused Ion Beam (FIB), Brunauer Emmett Teller (BET), Inductively coupled plasma (ICP), Electron Spin Resonance (ESR) and Photoluminescence (PL) equipments. The XPS characterization confirmed the formation of Y–O–Si and V-O-Si bondings between YVO4:Eu3+ phosphor particle and SiO2 coating. In addition, it was found that although the amounts of added SiO2 were not remarkable, but it resulted in enhancement of emission intensity of the phosphors. Finally by employing ESR analysis, it was shown that surface oxygen vacancies, result in reduction of V5+ to the lower valence state of V4+.

Keywords: solid state, sol-gel, silica, coating, photoluminescence

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Authors: Alak Kumar Patra, Nilanjan Mitra

Abstract:

Interface fracture toughness of glass-epoxy (G/E) PVC core sandwich composite with and without MWCNT has been investigated through experimental methods. Results demonstrate an improvement in interface fracture toughness values (GC) of samples with a certain percentages of MWCNT. In addition, dispersion of MWCNT in epoxy resin through sonication followed by mixing of hardener and vacuum assisted resin transfer method (VARTM) used in this study is an easy and cost effective methodology in comparison to previously adopted other methods limited to laminated composites. The study also identifies the optimum weight percentage of MWCNT addition in the resin system for maximum performance gain in interfacial fracture toughness. The results are supported by high resolution transmission electron microscope (HRTEM) analysis and fracture micrograph of field emission scanning electron microscope (FESEM) investigation.

Keywords: carbon nanotube, foam, glass-epoxy, interfacial fracture, sandwich composite

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Authors: Sudip Kumar Sinha, Saptarshi Ghosh

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While there’s a perpetual buzz around zinc oxide (ZnO) superstructures for their unique optical features, the versatile material has been constantly utilized to manifest tailored electronic properties through rendition of distinct morphologies. And yet, the unorthodox approach of implementing the novel 1D nanostructures of ZnO (pristine or doped) for volatile sensing applications has ample scope to accommodate new unconventional morphologies. In the last two decades, solid-state sensors have attracted much curiosity for their relevance in identifying pollutant, toxic and other industrial gases. In particular gas sensors based on metal oxide semiconducting (wide Eg) nanomaterials have recently attracted intensive attention owing to their high sensitivity and fast response and recovery time. These materials when exposed to air, the atmospheric O2 dissociates and get absorb on the surface of the sensors by trapping the outermost shell electrons. Finally a depleted zone on the surface of the sensors is formed, that enhances the potential barrier height at grain boundary . Once a target gas is exposed to the sensor, the chemical interaction between the chemisorbed oxygen and the specific gas liberates the trapped electrons. Therefore altering the amount of adsorbate is a considerable approach to improve the sensitivity of any target gas/vapour molecule. Likewise, this study presents a spontaneous but self catalytic creation of Sn-doped ZnO hexagonal nanoprisms on Si (100) substrates through thermal evaporation-condensation method, and their subsequent deployment for volatile sensing. In particular, the sensors were utilized to detect molecules of ethanol, acetone and ammonia below their permissible exposure limits which returned sensitivities of around 85%, 80% and 50% respectively. The influence of Sn concentration on the growth, microstructural and optical properties of the nanoprisms along with its role in augmenting the sensing parameters has been detailed. The single-crystalline nanostructures have a typical diameter ranging from 300 to 500 nm and a length that extends up to few micrometers. HRTEM images confirmed the hexagonal crystallography for the nanoprisms, while SAED pattern asserted the single crystalline nature. The growth habit is along the low index <0001>directions. It has been seen that the growth mechanism of the as-deposited nanostructures are directly influenced by varying supersaturation ratio, fairly high substrate temperatures, and specified surface defects in certain crystallographic planes, all acting cooperatively decide the final product morphology. Room temperature photoluminescence (PL) spectra of this rod like structures exhibits a weak ultraviolet (UV) emission peak at around 380 nm and a broad green emission peak in the 505 nm regime. An estimate of the sensing parameters against dispensed target molecules highlighted the potential for the nanoprisms as an effective volatile sensing material. The Sn-doped ZnO nanostructures with unique prismatic morphology may find important applications in various chemical sensors as well as other potential nanodevices.

Keywords: gas sensor, HRTEM, photoluminescence, ultraviolet, zinc oxide

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Authors: Ouafek Nora, Keghouche Nassira, Dehdouh Heider, Untidt Carlos

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A lot of knowledge has been accumulated on the metal clusters supported on oxide surfaces because of their multiple applications in microelectronics, heterogeneous catalysis, and magnetic devices. In this work, the surface state of Ni / MgO has been studied by XPS (X-ray Photoemission Spectroscopy). The samples were prepared by impregnation with ion exchange Ni²⁺ / MgO, followed by either a thermal treatment in air (T = 100 -350 ° C) or a gamma irradiation (dose 100 kGy, 25 kGy dose rate h -1). The obtained samples are named after impregnation NMI, NMR after irradiation, and finally NMC(T) after calcination at the temperature T (T = 100-600 °C). A structural study by XRD and HRTEM reveals the presence of nanoscaled Ni-Mg intermetallic phases (Mg₂Ni, MgNi₂, and Mg₆Ni) and magnesium hydroxide. Mg(OH)₂ in nanometric range (2- 4 nm). Mg-Ni compounds are of great interest in energy fields (hydrogen storage…). XPS spectra show two Ni2p peaks at energies of about 856.1 and 861.9 eV, indicating that the nickel is primarily in an oxidized state on the surface. The shift of the main peak relative to the pure NiO (856.1 instead of 854.0 eV) suggests that in addition to oxygen, nickel is engaged in another link with magnesium. This is in agreement with the O1s spectra which present an overlap of peaks corresponds to NiO and MgO, at a calcination temperature T ≤ 300 °C.

Keywords: XPS, XRD, nanoparticules, Ni-MgO

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Authors: Zhiqiang Xu, Hongfang Ma, Haitao Zhang, Weixin Qian, Weiyong Ying

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SSZ-13 materials with different Si/Al ratio were prepared by varying the composition of aluminosilicate precursor solutions upon hydrothermal treatment at 150 °C. The Si/Al ratio of the initial system was systematically changed from 12.5 to infinity in order to study the limits of Al composition in precursor solutions for constructing CHA structure. The intermediates and final products were investigated by complementary techniques such as XRD, HRTEM, FESEM, and chemical analysis. NH₃-TPD was used to study the Brønsted acidity of SSZ-13 samples with different Si/Al ratios. The effect of the Si/Al ratio on the precursor species, ultimate crystal size, morphology and yield was investigated. The results revealed that Al species determine the nucleation rate and the number of nuclei, which is tied to the morphology and yield of SSZ-13. The size of SSZ-13 increased and the yield decreased as the Si/Al ratio was improved. Varying Si/Al ratio of the initial system is a facile, commercially viable method of tailoring SSZ-13 crystal size and morphology. Furthermore, SSZ-13 materials with different Si/Al ratio were tested as catalysts for the methanol to olefins (MTO) reaction at 350 °C. SSZ-13 with the Si/Al ratio of 35 shows the best MTO catalytic performance.

Keywords: crystallization, MTO, Si/Al ratio, SSZ-13

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Authors: A. Gürses, Z. Eroğlu, E. Şahin, K. Güneş, Ç. Doğar

Abstract:

In recent years, polymer/clay nanocomposites have generated great interest in the polymer industry as a new type of composite material because of their superior properties, which includes high heat deflection temperature, gas barrier performance, dimensional stability, enhanced mechanical properties, optical clarity and flame retardancy when compared with the pure polymer or conventional composites. The investigation of change of the tensile properties of organoclay/linear low density polyethylene (LLDPE) nanocomposites with the use of Dioctyl terephthalate (DOTP) (as plasticizer) and calcite (as filler) has been aimed. The composites and organoclay synthesized were characterized using the techniques such as XRD, HRTEM and FTIR techniques. The spectroscopic results indicate that platelets of organoclay were well dispersed within the polymeric matrix. The tensile properties of the composites were compared considering the stress-strain curve drawn for each composite and pure polymer. It was observed that the composites prepared by adding the plasticizer at different ratios and a certain amount of calcite exhibited different tensile behaviors compared to pure polymer.

Keywords: linear low density polyethylene, nanocomposite, organoclay, plasticizer

Procedia PDF Downloads 254

Authors: Fisseha Zewdie, Naresh Bhatnagar

Abstract:

Lightweight and strong aluminum foam is developed by reinforcing Al-Si-Cu alloy (LM24) with Cermet Hollow Spheres (CHS) as porous creating agents. The foam samples were prepared by mixing the CHS in molten LM24 at 750°C, using gravity and stir casting. The CHSs were fabricated using a blend of silicon carbide and stainless-steel powders using the powder metallurgy technique. It was found that CHS reinforcement greatly enhances the performance of the composite metal foam, making it suitable for high impact loading applications such as crash protection and shock absorption. This study examined the strength, density, energy absorption and possible applications of the new aluminum foam. The results revealed that the LM24 foam reinforced with the CHS has the highest energy absorption of about 88 MJ/m3 among all categories of foam samples tested. Its density was found to be 1.3 g/cm3, while the strength, densification strains and porosity were 420 MPa, 34% and 70%, respectively. Besides, the matrix and reinforcement's microstructure, chemical composition, X-ray diffraction, HRTEM and related micrographic analyses are performed for characterization and verifications.

Keywords: composite metal foam, hollow spheres, gravity casting, energy absorption

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Authors: Magdalena Hałupka-Bryl, Magdalena Bednarowicz, Ryszard Krzyminiewski, Yukio Nagasaki

Abstract:

Due to their unique physical properties, superparamagnetic iron oxide nanoparticles are increasingly used in medical applications. They are very useful carriers for delivering antitumor drugs in targeted cancer treatment. Magnetic nanoparticles (PEG-PIONs/DOX) with chemotherapeutic were synthesized by coprecipitation method followed by coating with biocompatible polymer PEG-derivative (poly(ethylene glycol)-block-poly(4-vinylbenzylphosphonate). Complete physicochemical characterization was carried out (ESR, HRTEM, X-ray diffraction, SQUID analysis) to evaluate the magnetic properties of obtained PEG-PIONs/DOX. Nanoparticles were investigated also in terms of their stability, drug loading efficiency, drug release and antiproliferative effect on cancer cells. PEG-PIONs/DOX have been successfully used for the efficient delivery of an anticancer drug into the tumor region. Fluorescent imaging showed the internalization of PEG-PIONs/DOX in the cytoplasm. Biodistribution studies demonstrated that PEG-PIONs/DOX preferentially accumulate in tumor region via the enhanced permeability and retention effect. The present findings show that synthesized nanosystem is promising tool for potential magnetic drug delivery.

Keywords: targeted drug delivery, magnetic properties, iron oxide nanoparticles, biodistribution

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Authors: Ayed S. Al-Shihri, Abul Kalam, Abdullah G. Al-Sehemi, Gaohui Du, Tokeer Ahmad, Ahmad Irfan

Abstract:

We report here the synthesis of nickel oxide (NiO) nanoparticles by microwave-assisted method, using a common precipitating agent followed by calcination in air at 400°C. The effect of the microwave and pH on the crystallite size, morphology, structure, energy band gap and surface area of NiO have been investigated by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), ultraviolet visible spectroscopy (UV-vis) and BET surface area studies. X-ray diffraction studies showed the formation of monophasic and highly crystalline cubic NiO. TEM analysis led to decrease the average grain size of NiO nanoparticles from 16.5 nm to 14 nm on increasing the amount of NaOH. FTIR studies also confirm the formation of NiO nanoparticles. It was observed that on increasing the volume of NaOH, the optical band gap energy (2.85 eV to 2.95 eV) and specific surface area (33.1 to 39.8 m2/g) increases, however the average particles size decreases (16.5 nm to 14 nm). This method may be extended to large scale synthesis of other metal oxides nanoparticles and the present study could be used for the potential applications in water treatment and many other fields.

Keywords: BET surface area analysis, electron microscopy, optical properties, X-ray techniques

Procedia PDF Downloads 363

Authors: A. N. Fouda

Abstract:

A novel well identified hexagonal graphene oxide (GO) nano-sheets were synthesized using modified Hummer method. Low temperature thermal reduction at 350°C in air ambient was performed. After thermal reduction, typical few layers of thermal reduced GO (TRGO) with dimension of few hundreds nanometers were observed using high resolution transmission electron microscopy (HRTEM). GO has a lot of structure models due to variation of the preparation process. Determining the atomic structure of GO is essential for a better understanding of its fundamental properties and for realization of the future technological applications. Structural characterization was identified by x-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR) measurements. A comparison between exper- imental and theoretical IR spectrum were done to confirm the match between experimentally and theoretically proposed GO structure. Partial overlap of the experimental IR spectrum with the theoretical IR was confirmed. The electrochemical properties of TRGO nano-sheets as electrode materials for supercapacitors were investigated by cyclic voltammetry and electrochemical impedance spectroscopy (EIS) measurements. An enhancement in supercapacitance after reduction was confirmed and the area of the CV curve for the TRGO electrode is larger than those for the GO electrode indicating higher specific capacitance which is promising in super-capacitor applications

Keywords: hexagonal graphene oxide, thermal reduction, cyclic voltammetry

Procedia PDF Downloads 467

Authors: Ahmad Alazemi, M. Sherif El-Eskandrany, Mohamad Kishk, Thanyan AlOnaizi, Ahmad Alduweesh, Shorouq Abdullaleel

Abstract:

Arc melting technique followed by top-down approach, using a high-energy ball milling technique were employed to synthesize nanocrystalline of Cu50(Zr50-xNix)50 (x = 0, 10, 20 and 30 at.%) powder particles. The end-products of the alloy powders obtained after 50 h of the ball milling time were uniform in composition and had spherical-like morphology with an average particle size of 0.75 µm in diameter. The powders, which consisted of nanocrystalline grains with an average grain size of 10 nm in diameter, were used as feedstock materials for double face coating of stainless (SUS304) sheets, using cold spraying process. The coating materials enjoyed nanocrystalline structure and uniform composition. Biofilms were grown on 20-mm2 SUS304 sheets coated coupons inoculated with 1.5 × 108 CFU ml−1 E. coli. Significant biofilm inhibition was recorded in the nanoparticles coated coupons in comparison to non-coated SUS304 coupon. In conclusion, this study demonstrates that formation of biofilms can be significantly inhibited by Cu-based alloys especially in case of high (Ni) content. The inhibition of biofilm formation by nanocrystalline powders of Cu-based provides a practical approach to achieve the inhibition of biofilms formed by an emerging pathogen.

Keywords: biofilm, Cu, E.coli, FE-HRTEM/EDS, nanomaterials, nanocrystalline

Procedia PDF Downloads 392