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Synthesis of V2O3/C composites with different morphologies by a facile route and phase transition properties of the compounds

Abstract

V2O3 and amorphous carbon composites (V2O3/C composites) with different morphologies (e.g. nanospheres, nanorods and nanosheets) were, for the first time, successfully synthesized by a facile hydrothermal route and subsequent calcination. The as-obtained samples were characterized by X-ray powder diffraction (XRD), energy dispersive spectrometery (EDS), elemental analysis (EA), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The morphology of V2O3/C composites could be easily controlled by varying the reaction time, and, as a result, V2O3/C composites with nanospheres, nanorods and nanosheets were selectively synthesized. Furthermore, the phase transition property of V2O3/C composites was measured by differential scanning calorimetry (DSC), suggesting that V2O3/C composites exhibit the phase transition similar to V2O3, which could expand the potential applications of materials related to V2O3 in the future.

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Synthesis and characterization of hollow V2O5 microspheres for supercapacitor electrode with pseudocapacitance

(FE-SEM, NOVA NanoSEM 450, FEI). The phase and composition of the products was identified by X-ray powder diffraction (XRD, PANalytical X’Pert Powder Diffractometer at 40 kV and 40 mA with Ni-filtered CuKα radiation). Infrared spectroscopy (IR) pattern of the solid samples was measured using KBr pellet technique (about 1 wt.% of the sample and 99 wt.% of KBr were mixed homogeneously, and then the mixture was pressed into a pellet) and recorded on a Nicolet 6700 spectrometer from 4000 cm –1 to 400 cm –1 with a resolution of 4 cm –1 . Surface area was determined by

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Selective crystallization of gamma glycine for NLO applications using magnesium sulfate (MgSO4) as an additive

Abstract

Crystallization of γ-glycine in the presence of selected concentration (9 g/mL) of tailor-made additive magnesium sulfate heptahydrate salt (MgSO4·7H2O) has been studied at ambient temperature by adopting slow solvent evaporation procedure. The morphological modifications of glycine crystals grown from pure aqueous solutions of glycine and from glycine solutions containing magnesium species in the amount of 0.1 g/mL to 16 g/mL have been investigated thoroughly. The crystalline nature and phase identification of the crystalline material were confirmed by X-ray powder diffraction and SXRD studies. NMR studies revealed the information about the molecular conformation in solution, phase changes, functional groups and chemical environment. FT-IR spectra revealed distinct difference between α and γ-glycine polymorphs in the region around 880 cm−1 to 930 cm−1. The grown γ-glycine crystal had a lower cut-off value at 200 nm and the bandgap value evaluated from the Tauc plot was found to be 5.83 eV. The marked differences between α and γ-polymorphs of glycine were also revealed by DSC thermograms. The mechanical strength of the γ-glycine crystal was studied with the help of Vickers microhardness instrument. Kurtz-powder NLO study proved the generation of second harmonics (i.e. green light emission) in the grown γ-glycine crystal and its efficiency was calculated as 1.44 times better than that of the reference material potassium dihydrogen phosphate.

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Synthesis and characterization of Zn/ZnO microspheres on indented sites of silicon substrate

Abstract

Self-assembled Zn/ZnO microspheres have been accomplished on selected sites of boron doped P-type silicon substrates using hydrothermal approach. The high density Zn/ZnO microspheres were grown on the Si substrates by chemical treatment in mixed solution of zinc sulfate ZnSO4·7H2O and ammonium hydroxide NH4(OH) after uniform heating at 95 °C for 15 min. The Zn/ZnO microspheres had dimensions in the range of 1 μm to 20 μm and were created only on selected sites of silicon substrate. The crystal structure, chemical composition and morphology of as-prepared samples were studied by using scanning electron microscope SEM, X-ray diffraction XRD, energy dispersive X-ray spectroscopy EDS, Fourier transform infrared spectroscopy FT-IR and UV-Vis diffuse reflectance absorption spectra DRS. The energy band gap Eg of about 3.28 eV was obtained using Tauc plot. In summary, this study suggests that interfacial chemistry is responsible for the crystal growth on indented sites of silicon substrate and the hydrothermal based growth mechanism is proposed as a useful methodology for the formation of highly crystalline three dimensional (3-D) Zn/ZnO microspheres.

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Synthesis, characterization and fabrication of copper nanoparticles in N-isopropylacrylamide based co-polymer microgels for degradation of p-nitrophenol

Abstract

Poly(N-isopropylacrylamide-co-acrylic acid) [P(NIPAM-co-AAc)] microgels were synthesized by precipitation polymerization. Copper nanoparticles were successfully fabricated inside the microgels by in-situ reduction of copper ions in an aqueous medium. The microgels were characterized by Fourier Transform Infrared Spectroscopy (FT-IR) and Dynamic Light Scattering (DLS). Hydrodynamic radius of P(NIPAM-co-AAc) microgel particles increased with an increase in pH in aqueous medium at 25 °C. Copper-poly(N-isopropylacrylamide-co-acrylic acid) [Cu-P(NIPAM-co-AAc)] hybrid microgels were used as a catalyst for the reduction of 4-nitrophenol (4-NP). Effect of temperature, concentration of sodium borohydride (NaBH4) and catalyst dosage on the value of apparent rate constant (kapp) for catalytic reduction of 4-NP in the presence of Cu-P(NIPAM-co-AAc) hybrid microgels were investigated by UV-Vis spectrophotometry. It was found that the value of kapp for catalytic reduction of 4-NP in the presence of Cu-P(NIPAM-co-AAc) hybrid microgel catalyst increased with an increase in catalyst dosage, temperature and concentration of NaBH4 in aqueous medium. The results were discussed in terms of diffusion of reactants towards catalyst surface and swelling-deswelling of hybrid microgels.

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Preparation and spectroscopic analysis of zinc oxide nanorod thin films of different thicknesses

Abstract

Zinc oxide thin films with different thicknesses were prepared on microscopic glass slides by sol-gel spin coating method, then hydrothermal process was applied to produce zinc oxide nanorod arrays. The nanorod thin films were characterized by various spectroscopic methods of analysis. From the images of field emission scanning electron microscope (FESEM), it was observed that for the film thickness up to 200 nm the formed nanorods with wurtzite hexagonal structure were uniformly distributed over the entire surface substrate. From X-ray diffraction analysis it was revealed that the thin films had good polycrystalline nature with highly preferred c-axis orientation along (0 0 2) plane. The optical characterization done by UV-Vis spectrometer showed that all the films had high transparency of 83 % to 96 % in the visible region and sharp cut off at ultraviolet region of electromagnetic spectrum. The band gap of the films decreased as their thickness increased. Energy dispersive X-ray spectroscopy (EDS) showed the presence of zinc and oxygen elements in the films and Fourier transform infrared spectroscopy (FT-IR) revealed the chemical composition of ZnO in the film.

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Green synthesis and characterization of Ag1/2Al1/2TiO3 nanoceramics

Abstract

Single phase silver aluminum titanate (Ag1/2Al1/2)TiO3, later called AAT, nanoceramic powder (particle size 2 to 7.5 nm) was synthesized by a low-cost, green and reproducible tartaric acid gel process. X-ray, FT-IR, energy dispersive X-ray and high resolution transmission electron microscopy analyses were performed to ascertain the formation of AAT nanoceramics. X-ray diffraction data analysis indicated the formation of monoclinic structure having the space group P2/m(10). UV-Vis study revealed the surface plasmon resonance at 296 nm. Dielectric study revealed that AAT nanoceramics could be a suitable candidate for capacitor applications and meets the specifications for “Z7R” of Class I dielectrics of Electronic Industries Association. Complex impedance analyses suggested the dielectric relaxation to be of non-Debye type. To find a correlation between the response of the real system and idealized model circuit composed of discrete electrical components, the model fittings were performed using the impedance data. Electric modulus studies supported the hopping type of conduction in AAT. The correlated barrier hopping model was employed to successfully explain the mechanism of charge transport in AAT. The ac conductivity data were used to evaluate the density of states at Fermi level and minimum hopping length of the compound.

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Synthesis and characterization of fluorescent polyphenols anchored Schiff bases via oxidative polycondensation

Abstract

A series of polyimines, bearing phenolic groups were successfully synthesized in aqueous alkaline solution via chemical oxidative polycondensation. Polymeric Schiff bases were synthesized by condensation of 2,4-dihydroxybenzaldehyde and 3-hydroxy-4-metoxybenzaldehyde with 2-aminophenol and 3-aminophenol. The molecular structures of the synthesized Schiff bases and their corresponding polymers were studied by FT-IR, UV-Vis, 1H-NMR and 13C-NMR spectroscopic methods. Thermal stability of the imine polymers was evidenced by their initial degradation temperatures found in the range of 170 °C to 271 °C without any sign of melting. The results of UV-Vis and cyclic voltammetry (CV) measurements were coherent with the optical Eg and the electrochemical E′g band gaps of the polyimines which were lower than those of their corresponding Schiff bases. Fluorescence spectral analysis of P4 (Schiff base polymer P4 derived from 3-aminophenol and 3-hydroxy-4-methoxybenzaldehyde) revealed a bicolor emission with blue and green light. Electrical conductivity of the synthesized imine polymers was measured by four-point probe technique. P4 showed the highest electrical conductivity as a result of iodine vapor contact time. Morphology characterization of the synthesized polyimines was carried out using a scanning electron microscope SEM at different magnifications. The study revealed that P4 is a promising candidate for both blue and green light emitters which could be used in the production of photovoltaic materials and solar cells.

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Optical and structural properties of nanostructured copper oxide thin films as solar selective coating prepared by spray pyrolysis method

Abstract

Copper (II) oxide thin films were prepared by spray pyrolysis method on soda-lime glass substrates using copper acetate precursor solution. Influence of substrate temperature on structural and optical properties was investigated. Structural analysis of these layers were carried out by X-ray diffraction (XRD). Single phase nature and high crystallinity of CuO nanostructures were observed on XRD patterns. The general appearance of the films was uniform and black in color. FT-IR transmittance spectra confirmed the results from the XRD study. Selective solar absorber coatings of copper oxide (CuO) on stainless steel substrates was prepared by spray pyrolysis method. Effect of deposition temperature on optical properties of thin films was investigated. Optical parameters, absorbance (α) and emittance (α) were evaluated from reflectance data. It can be deduced that the porous structure, such as a light traps, can greatly enhance absorbance, while the composition, thickness and roughness of thin films can greatly influence the emissivity. Single phase nature and high crystallinity of CuO nanostructures were observed by XRD patterns. Solar absorbance of thin films were in the range of 85 % to 92 %.

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Transparent fluorinate acrylic polyurethane with hydrophobicity obtained by crosslinking of hydroxyl-containing fluoroacrylate copolymer with HDI trimer

Abstract

Hydroxyl-containing fluoroacrylate copolymers with different fluorine and hydroxyl concentrations were synthesized via free-radical solution polymerization. Transparent fluorinated polyurethane (FPU) films were prepared by curing the copolymers with HDI (hexamethylene diisocyanate) trimer. The Fourier transform infrared spectroscopy (FT-IR) results revealed introduction of fluorine both into the copolymer and polyurethane. X-ray photoelectron spectroscopy (XPS) analyses indicated that a gradient concentration of fluorine existed in the depth profile of the fluorinated polyurethane films. The highest contact angle (CA) was obtained for the FPU film with fluoroacrylate monomer concentration of 22 wt.% because of fluorine present on the film surface. The surface topographies detected by SEM and AFM indicated that surface roughness contributed little to the film hydrophobicity. By increasing the fluoroacrylate monomer concentration, the decreasing of crosslinking degree of hard segment resulted in lowering the first degradation temperature, while more C-F groups in soft segment led to higher second degradation temperature. UV-Vis spectrophotometer measurements indicated that the FPU film with the fluoroacrylate monomer concentration of 16 wt.% still had a high transmittance of more than 90 % in the whole visible wavelength range.

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