Search results for: transmission electron spectroscopy

Authors: D. P. Evdokimov, A. N. Kirichenko, V. D. Blank, V. N. Denisov, B. A. Kulnitskiy

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In this study we investigated the stability of polyhedral carbon onions under influence of shear deformation and high pressures above 43 GPa by means of by transmission electron microscopy (TEM) and Raman spectroscopy (RS). It was found that at pressures up to 29 GPa and shear deformations of 40 degrees the onions are stable. At shear deformation applying at pressures above 30 GPa carbon onions collapsed with formation of amorphous carbon. At pressures above 43 GPa diamond-like carbon (DLC) was obtained.

Keywords: carbon onions, Raman spectroscopy, transmission electron spectroscopy

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Authors: Shahab Zomorodbakhsh, Hayron Nesa Motevasel

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Water soluble compoundes were attached to single-walled carbon nanotubes (SWNTs) to form water-soluble nano pigments. functionalized SWNTs were then characterized by Fourier Transform Infrared spectroscopy (FT-IR), Raman spectroscopy, UV analysis, Transmission electron microscopy (TEM)and defunctionalization test and Representative results concerning the solubility. The product can be dissolved in water and High-resolution transmission electron microscope images showed that the SWNTs were efficiently functionalized, thus the p-stacking interaction between aromatic rings and COOH of SWNTs was considered responsible for the high solubility and High transmission electron in singlewall nanotubes.

Keywords: functionalized CNTs, singlewalled carbon nanotubes, water soluble compoundes, nano pigments

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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: Muhammad A. Nadeem, Shaheed Ullah

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The article reports the synthesis of Cr2O3/C nanocomposites obtained by the direct carbonization of PFA/MIL-101(Cr) bulk composite. The nanocomposites were characterized by various instrumental techniques like powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and the surface characterized were investigated via N2 adsorption/desorption analysis. TEM and SAED analysis shows that turbostatic graphitic carbon was obtained with high crystallinity. The nanocomposites were tested for electrochemical supercapacitor and the faradic and non-Faradic processes were checked through cyclic voltammetry (CV). The maximum specific capacitance calculated for Cr2O3/C 900 sample from CV measurement is 301 F g-1 at 2 mV s-1 due to its maximum charge storing capacity as confirm by frequency response analysis.

Keywords: nanocomposites, transmission electron microscopy, non-faradic process

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Authors: Rashad Al-Gaashani, Muataz A. Atieh

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In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

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

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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

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Authors: Manel Bouloudenine, Karima Djeddou, Hadjer Ben Manser, Hana Soualah Alila, Mohmed Bououdina

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This survey research involves the elaboration and characterization of silver nanoparticles for therapeutic and environmental applications. The silver nanoparticles "Ag NPs" were synthesized by reducing AgNO3 with microwaves. The characterization of nanoparticles was done by using Transmission Electron Microscopy " TEM ", Energy Dispersive Spectroscopy "EDS", Selected Area Electron Diffraction "SEAD", UV-Visible Spectroscopy and Dynamic Light Scattering "DLS". Transmission Electron Microscopy and Electron Diffraction have confirmed the nanoscale, the shape, and the crystalline quality of as synthesized silver nanoparticles. Elementary analysis has proved the purity of Ag NPs and the presence of the Surface Plasmon Resonance phenomenon "SPR". A strong absorption shift was observed in the visible range of the UV-visible spectrum of as synthesized Ag NPs, which indicates the presence of metallic silver. When the strong absorption in the ultraviolet range of the spectrum has revealed the presence of ionic Ag NPs ionic Ag aggregates species. The autocorrelation function measured by the Dynamic Light Scattering has shown a strong monodispersed character of Ag NPs, which is indicated by the presence of a single size population, with a minima and a maxima laying between 40 and 111 nm. Related to other research, our results confirm the performance properties of as synthesized Ag NPs, which allows them to be performing in many technological applications, including therapeutic and environmental ones.

Keywords: silvers nanoparticles, microwaves, EDS, TEM

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Authors: Andrea Alfaro Barajas, Arturo I. Martinez

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3D photothermal structure of carbon was synthesized using PET bottles waste and sodium chloride through controlled carbonization. Characterization techniques such as X-ray photoelectron spectroscopy, X-ray diffraction, BET, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, spectrophotometry, and mechanical compression were carried out. The carbon showed physical integrity > 90%, an absorbance > 90% between 300-1000nm of the solar spectrum, and a high specific surface area from 450 to 620 m2/g. The X-ray was employed to examine the phase structure; the obtained pattern shows an amorphous material. A higher intensity of band D with respect to band G was confirmed by Raman Spectroscopy. C-OH, COOH, C-O, and C-C bonds were obtained from the deconvolution of the high-resolution C1s orbital. Macropores of 160 to 180µm and micropores of 0.5 to 2nm were observed by SEM and TEM images, respectively. Such combined characteristics of carbon confer efficient evaporation of water under 1 sun irradiation > 60%.

Keywords: solar-absorber, carbon, water-evaporation, interfacial

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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: Hanan Alenezi

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Membrane performance depends on the kind of solvent used in preparation. A membrane made by Polyetherimide (PEI) was evaluated for gas separation using X-Ray Diffraction (XRD), Scanning electron microscope (SEM), and Energy Dispersive X-Ray Spectroscopy (EDS). The purity and the thickness are detected to evaluate the membrane in order to optimize PEI membrane preparation.

Keywords: Energy Dispersive X-Ray Spectroscopy (EDS), Membrane, Polyetherimide PEI, Scanning electron microscope (SEM), Solvent, X-Ray Diffraction (XRD)

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Authors: C. L. Popa, S. L. Iconaru, A. Costescu, C. S. Ciobanu, M. Motelica Heino, R. Guegan, D. Predoi

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Surface functionalization of ceramic composites with a special focus on tetraethyl orthosilicate (TEOS) and hydroxyapatite (HAp) is discoursed. Mesoporous ceramic HAp-TEOS composites were prepared by the incorporation of hydroxyapatite into tetraethyl orthosilicate by sol-gel method. The resulting samples were analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and Raman spectroscopy and nitrogen physisorption. The removal of Pb2+ ions from aqueous solutions was evaluated using Atomic Absorbtion Spectroscopy (AAS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled Pb2+ at pH ~ 3 and pH ~ 5. After removal experiment of Pb2+ at pH 3 and pH 5, porous hydroxyapatite nanoparticles is transformed into PbHAp_3 and PbHAp_5 via the adsorption of Pb2+ ions followed by the cation exchange reaction. The diffraction patterns show that THAp nanoparticles were successfully coated with teos without any structural changes. On the other, the AAS analysis showed that THAp can be useful in the removal Pb2+ from water contaminated.

Keywords: teos, hydroxyapatite, environment applications, biosystems engineering

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Authors: Duygu Çimen, Nilay Bereli, Adil Denizli

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In this study is to synthesis magnetic nanoparticles for purify protein C. For this aim, N-Methacryloyl-(L)-histidine methyl ester (MAH) containing 2-hydroxyethyl methacrylate (HEMA) based magnetic nanoparticles were synthesized by using micro-emulsion polymerization technique for templating protein C via metal chelation. The obtained nanoparticles were characterized with Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), zeta-size analysis and electron spin resonance (ESR) spectroscopy. After that, they were used for protein C purification from aqueous solution to evaluate/optimize the adsorption condition. Hereby, the effecting factors such as concentration, pH, ionic strength, temperature, and reusability were evaluated. As the last step, protein C was determined with sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

Keywords: immobilized metal affinity chromatography (IMAC), magnetic nanoparticle, protein C, hydroxyethyl methacrylate (HEMA)

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Authors: Uma Shanker, Vidhisha Jassal

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A novel green route was used to synthesize few metal hexacyanoferrates (FeHCF, NiHCF, CoHCF and CuHCF) nanoparticles using Sapindus mukorossias a natural surfactant and water as a solvent. The synthesized nanoparticles were characterized by Powder X-ray diffraction (PXRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR) and Thermo gravimetric techniques. Trasmission electron microscopic images showed that synthesized MHCF nanoparticles exhibited cubic and spherical shapes with exceptionally small sizes ranging from 3nm - 186 nm.

Keywords: metal hexacyanoferrates, natural surfactant, Sapindus mukorossias, nanoparticles

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Authors: L. R. Shobin, S. Manivannan

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One dimensional silver nanowires and nanoparticles gained more interest in developing transparent conducting films, catalysis, biological and chemical sensors. Silver nanostructures can be synthesized by varying reaction conditions such as the precursor concentration, molar ratio of the surfactant, injection speed of silver ions, etc. in the polyol process. However, the reaction proceeds for greater than 2 hours for the formation of silver nanowires. The introduction of etchant in the medium promotes the growth of silver nanowires from silver nanoparticles along the [100] direction. Rapid growth of silver nanowires is accomplished using the Cl- ions from NaCl and polyvinyl pyrrolidone (PVP) as surfactant. The role of Cl- ion was investigated in the growth of the nanostructured silver. Silver nanoparticles (<100 nm) were harvested from glycerol medium in the absence of Cl- ions. Trace amount of Cl- ions (2.5 mM -NaCl) produced the edge joined nanowires of length upto 2 μm and width ranging from 40 to 65 nm. Formation and rapid growth (within 25 minutes) of long, uniform silver nanowires (upto 5 μm) with good yield were realized in the presence of 5 mM NaCl at 200ºC. The growth of nanostructures was monitored by UV-vis-NIR spectroscopy. Scanning and transmission electron microscopes reveal the morphology of the silver nano harvests. The role of temperature in the reduction of silver ions, growth mechanism for nanoparticles, edge joined and straight nanowires will be discussed.

Keywords: silver nanowires, glycerol mediated polyol process, scanning electron microscopy, UV-Vis- NIR spectroscopy, transmission electron microscopy

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Authors: Sajjad Sedaghat

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In this work, facile and green biosynthesis and characterization of silver–montmorillonite (MMT) nanocomposite is reported at room temperature. Silver nanoparticles (Ag–NPs) were synthesized into the interlamellar space of (MMT) by using water extract of Satureja hortensis L as reducing agent. The MMT was suspended in the aqueous AgNO₃ solution, and after the absorption of silver ions, Ag⁺ was reduced using water extract of Satureja hortensis L to Ag°. Evaluation of the antibacterial properties are also reported. The nanocomposite was characterized by ultraviolet-visible spectroscopy (UV–Vis), powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). TEM study showed the formation of nanocomposite using water extract of Satureja hortensis L in the 4.88 – 26.70 nm range and average particles size were 15.79 nm also the XRD study showed that the particles have a face-centered cubic (fcc) structure. The nanocomposite showed the antibacterial properties against Gram-positive and Gram-negative bacteria.

Keywords: antibacterial effects, montmorillonite, Satureja hortensis l, transmission electron microscopy, nanocomposite

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Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

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The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

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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: Mingmei Zhang, Xinyong Li

Abstract:

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: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

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Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: ceramics, energy storage, electrochemical measurements, transmission electron microscope

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Authors: S. Melvin Samuel, Jayanta Bhattacharya

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In the present study, a graphene oxide/chitosan (GO-CS) composite material was prepared and used as an adsorbent for the removal of methylene blue (MB) from aqueous solution. The synthesized GO-CS adsorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopes (SEM), transmission electron microscopy (TEM), Raman spectroscopy and thermogravimetric analysis (TGA). The removal of MB was conducted in batch mode. The effect of parameters influencing the adsorption of MB such as pH of the solution, initial MB concentration, shaking speed, contact time and adsorbent dosage were studied. The results showed that the GO-CS composite material has high adsorption capacity of 196 mg/g of MB solution at pH 9.0. Further, the adsorption of MB on GO-CS followed pseudo second order kinetics and equilibrium adsorption data well fitted by the Langmuir isotherm model. The study suggests that the GO-CS is a favorable adsorbent for the removal of MB from aqueous solution.

Keywords: Methylene blue, Graphene oxide-chitosan, Isotherms, Kinetics.

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Authors: Leila Samiee, Amir Yadegari, Saeedeh Tasharrofi

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In the work presented here, nitrogen-doped graphene materials were synthesized and used as metal-free electrocatalysts for oxygen reduction reaction (ORR) under alkaline conditions. Paraphenylenediamine was used as N precursor. The N-doped graphene was synthesized under hydrothermal treatment at 200°C. All the materials have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM) and X-ray photo-electron spectroscopy (XPS). Moreover, for electrochemical evaluation of samples, Rotating Disk electrode (RDE) and Cyclic Voltammetry techniques (CV) were employed. The resulting material exhibits an outstanding catalytic activity for the oxygen reduction reaction (ORR) as well as excellent resistance towards methanol crossover effects, indicating their promising potential as ORR electrocatalysts for alkaline fuel cells.

Keywords: alkaline fuel cell, graphene, metal-free catalyst, paraphenylen diamine

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Authors: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: Mai M. Khalaf, Hany M. Abd El-Lateef

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A new good application for the sol gel method is to improve the corrosion inhibition properties of carbon steel by the dip coating method of Nano TiO2 films and its modification with Poly Ethylene Glycol (PEG). The prepared coating samples were investigated by different techniques, X-ray diffraction, Scanning Electron Microscopy (SEM), transmission electron microscopy and Energy Dispersive X-ray Spectroscopy (EDAX). The corrosion inhibition performance of the blank carbon steel and prepared coatings samples were evaluated in 0.5 M H2SO4 by using Electrochemical Impedance Spectroscopy (EIS) and potentiodynamic polarization measurements. The results showed that corrosion resistance of carbon steel increases with increasing the number of coated layers of both nano–TiO2 films and its modification of PEG. SEM-EDAX analyses confirmed that the percentage atomic content of iron for the carbon steel in 0.5 M H2SO4 is 83% and after the deposition of the steel in nano TiO2 sol and that with PEG are 94.3% and 93.7% respectively.

Keywords: dip-coatings, corrosion protection, sol gel, TiO2 films, PEG

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Authors: Nazli Darkhal

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The use of gems and ornaments has been common in Iran since the beginning of history. The prosperity of the country, the wealth, and the interest of the people of this land in luxurious and glorious life, combined with beauty, have always attracted the attention of the gems and ornaments of the Iranian people. Iranians are famous in the world for having a long history of collecting and recognizing precious stones. In this case, we can use the unique treasure of national jewelry. Raman spectroscopy method is one of the oscillating spectroscopy methods that is classified in the group of nondestructive study methods, and like other methods, in addition to several advantages, it also has disadvantages and problems. Micro Raman spectroscopy is one of the different types of Raman spectroscopy in which an optical microscope is combined with a Raman device to provide more capabilities and advantages than its original method. In this way, with the help of Raman spectroscopy and a light microscope, while observing more details from different parts of the historical sample, natural or artificial pigments can be identified in a small part of it. The EDX electron microscope also functions as the basis for the interaction of the electron beam with the matter. The beams emitted from this interaction can be used to examine samples. In this article, in addition to introducing the micro Raman spectroscopy method, studies have been conducted on the structure of three samples of existing stones in the historic citadel of Bam. Using this method of study on precious and semi-precious stones, in addition to requiring a short time, can provide us with complete information about the structure and theme of these samples. The results of experiments and gemology of the stones showed that the selected beads are agate and jasper, and they can be placed in the chalcedony group.

Keywords: bam citadel, precious and semi-precious stones, Raman spectroscopy, scanning electron microscope

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Authors: A. Pourahmad, Sh. Gharipour

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The present work describes the preparation and characterization of nanosized SiO₂@PbS core-shell particles by using a simple wet chemical route. This method utilizes silica spheres formation followed by successive ionic layer adsorption and reaction method assisted lead sulphide shell layer formation. The final product was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–vis spectroscopic, infrared spectroscopy (IR) and transmission electron microscopy (TEM) experiments. The morphological studies revealed the uniformity in size distribution with core size of 250 nm and shell thickness of 18 nm. The electron microscopic images also indicate the irregular morphology of lead sulphide shell layer. The structural studies indicate the face-centered cubic system of PbS shell with no other trace for impurities in the crystal structure.

Keywords: core-shell, nanostructure, semiconductor, optical property, XRD

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Authors: Jiazhen Liao, Xiaolan Zeng

Abstract:

A series of BiOCl nanoplates with different oxygen vacancies (OVs) concentrations were successfully synthesized via a facile solvothermal method. The concentration of OVs of BiOCl can be tuned by the ratios of water/ethylene glycol. Such nanoplates containing oxygen vacancies served as an efficient visible-light-driven photocatalyst for NO oxidation. Compared with pure BiOCl, the enhanced photocatalytic performance was mainly attributed to the introduction of OVs, which greatly enhanced light absorption, promoted electron transfer, activated oxygen molecules. The present work could provide insights into the understanding of the role of OVs in photocatalysts for reference. Combined with characterization analysis, such as XRD（X-ray diffraction）, XPS（X-ray photoelectron spectroscopy), TEM（Transmission Electron Microscopy）, PL（Fluorescence Spectroscopy）, and DFT (Density Functional Theory) calculations, the effect of vacancies on photoelectrochemical properties of BiOCl photocatalysts are shown. Furthermore, the possible reaction mechanisms of photocatalytic NO oxidation were also revealed. According to the results of in situ DRIFTS （ Diffused Reflectance Infrared Fourier Transform Spectroscopy）, various intermediates were produced during different time intervals of NO photodegradation. The possible pathways are summarized below. First, visible light irradiation induces electron-hole pairs on the surface of OV-BOC (BiOCl with oxygen vacancies). Second, photogenerated electrons form superoxide radical with the contacted oxygen. Then, the NO molecules adsorbed on the surface of OV-BOC are attacked by superoxide radical and form nitrate instead of NO₂ (by-products). Oxygen vacancies greatly improve the photocatalytic oxidation activity of NO and effectively inhibit the production of harmful by-products during the oxidation of NO.

Keywords: OVs-BiOCl nanoplate, oxygen vacancies, NO oxidation, photocatalysis

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

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

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

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Authors: Temesgen Geremew

Abstract:

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

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

Procedia PDF Downloads 55

Authors: Indu Elizabeth

Abstract:

Antimony/Multi Walled Carbon nano tube nanocomposite (Sb/MWCNT) is synthesized using ethylene glycol mediated reduction process. Binder free, self-supporting and flexible Sb/MWCNT nanocomposite paper has been prepared by employing the vacuum filtration technique. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy (RS), and thermal gravimetric analysis (TGA) to evaluate the structure of anode and tested for its performance in a Lithium rechargeable cell. Electrochemical measurements demonstrate that the Sb/MWCNT composite paper anode delivers a specific discharge capacity of ~400 mAh g-1 up to a current density of 100 mA g-1.

Keywords: antimony, lithium ion battery, multiwalled carbon nanotube, specific capacity

Procedia PDF Downloads 375