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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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Facile microwave-assisted synthesis of Al:Mn co-doped PbI2 nanosheets: structural, vibrational, morphological, dielectric and radiation activity studies

Abstract

Herein, we report a successful development of nano-scale pure and Al and Mn co-doped PbI2 using facile microwaveassisted route. Structural study was done through X-ray diffraction analysis of grain size, dislocation density and lattice strain. The crystallite size was found to vary from 28 nm to 40 nm due to Al:Mn co-doping in PbI2. The presence of various vibrational modes was confirmed by FT-IR spectroscopy and red shifting was observed in peak positions compared to the bulk. Surface morphology, examined using a scanning electron microscope, confirmed the formation of single crystal nanosheets of a thickness in the range of 10 nm to 30 nm. The single crystal nanosheets were found to be transformed to large area nanosheets due to the doping. Enhancement in dielectric constant from ~7.5 to 11 was observed with increasing Al doping concentration. Linear attenuation coefficient was calculated and showed the enhancement of blocking gamma rays with increasing doping concentration. Its value was found to increase from 7.5 to 12.8 with the doping. The results suggest that the synthesized nanostructures can be used for detection and absorption of gamma rays emitted by 137Cs and 241Am sources.

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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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Luminescent homo- and hetero-metallic hybrid molecular materials constructed by covalent grafting

Abstract

In this paper, 3-(triethoxysilyl)-propyl isocyanate (abbreviated as TESPIC) was modified by ethylparaben (EPB) to produce corresponding organic-inorganic monomers (EPB-TESPIC) with two components equipped with covalent bonds, which not only can coordinate to RE ions (Tb3+ and Eu3+) but also act as a sol-gel precursor. Luminescent hybrid materials consisting of terbium-europium complex, covalently bonded to silica-based network, have been obtained in situ via a sol-gel approach. Proton nuclear magnetic resonance spectroscopy (1HNMR) and Fourier transform infrared spectroscopy (FT-IR) were applied to characterize the structure of EPB-TESPIC. UV-visible, phosphorescence, and luminescence spectra were obtained to characterize the photophysical properties of the obtained hybrid material. Through co-hydrolysis and polycondensation, Tb3+ and Eu3+ can be introduced into the same organic-inorganic hybrid monomer, forming Si-O backbones. The experimental results show that the strong luminescence of rare-earth ions substantiates the optimum energy match and effective intramolecular energy transfer between the triplet state energy of coordination complex and the emissive energy level of the rare-earth ions. The hybrid material systems are expected to have potential applications in photophysical sensors.

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Optimization of sol-gel technique for coating of metallic substrates by hydroxyapatite using the Taguchi method

Abstract

In this study, the Taguchi method of design of experiment (DOE) was used to optimize the hydroxyapatite (HA) coatings on various metallic substrates deposited by sol-gel dip-coating technique. The experimental design consisted of five factors including substrate material (A), surface preparation of substrate (B), dipping/withdrawal speed (C), number of layers (D), and calcination temperature (E) with three levels of each factor. An orthogonal array of L18 type with mixed levels of the control factors was utilized. The image processing of the micrographs of the coatings was conducted to determine the percentage of coated area (PCA). Chemical and phase composition of HA coatings were studied by XRD, FT-IR, SEM, and EDS techniques. The analysis of variance (ANOVA) indicated that the PCA of HA coatings was significantly affected by the calcination temperature. The optimum conditions from signal-to-noise (S/N) ratio analysis were A: pure Ti, B: polishing and etching for 24 h, C: 50 cm min−1, D: 1, and E: 300 °C. In the confirmation experiment using the optimum conditions, the HA coating with high PCA of 98.5 % was obtained.

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Influence of aluminium concentration in Zn0:9V0:1O nanoparticles on structural and optical properties

Abstract

The (V,Al) co-doped ZnO nano-structured powders (Zn0.9-xV0.1AlxO, where x = 0.02, 0.03 and 0.04) were synthesized via the sol-gel technique and their structural and optical properties were investigated. The effect of Al concentration on the structural and optical properties of the Zn0.9-xV0.1AlxO nanopowders was studied using various techniques. The XRD patterns indicate that the samples have a polycrystalline wurtzite structure. The crystallite size increases with increasing the Al content and lies in the range of 23 to 30 nm. The lattice strain, estimated by the Stokes-Wilson equation, decreases when Al content increases. SEM and TEM micrographs show that Zn0.9-xV0.1AlxO powders are the agglomeration of nanoparticles having spherical and hexagonal shapes with dimensions ranging from 20 to 30 nm. FT-IR spectra show a distinct absorption peak at about 500 cm-1 for ZnO stretching modes and other peaks related to OH and H2O bands. Raman spectra confirm the wurtzite structure of the Zn0.9-xV0.1AlxO nanoparticles. The direct band gaps of the synthesized Zn0.9-xV0.1AlxO nanopowders, estimated from the Brus equation and the crystallite sizes deduced from XRD, are around 3.308 eV. The decomposition process of the dried gel system was investigated by thermal gravimetric analysis (TGA).

Open access
Green synthesis, characterization and biological activities of silver nanoparticles using the bark extract of ailanthus altissima

Abstract

Due to their potential application in various fields of science and technology, the eco-friendly bio-synthesis of silver (Ag) nanoparticles (NPs) is a growing area for researchers. In this study, we report the green synthesis of Ag nanoparticles and their characterization by using various techniques. For the preparation of Ag particles, aqueous plant extract of ailanthus altissima was used as a reducing medium for Ag+ ions of silver nitrate to Ag0. UV-Vis spectrophotometry was used to trace the formation of Ag particles by noting their surface plasmon resonance peaks (400 nm to 440 nm). Fourier transform infrared spectroscopy (FT-IR) was employed to reveal the chemical composition of Ag nanoparticles which were capped by plant extract. Scanning electron microscopy (SEM) was used to get the lattice image, morphology and average size of Ag particles. The average size distribution of Ag NPs dispersed in aqueous media was also measured using dynamic light scattering (DLS). It was found that DLS results are in good agreement with those obtained from SEM. The synthesized particles were then subjected to the antibacterial and antifungal activities by studying them against various species, such as bacillus cereus, staphylococcus aureus, pseudomonas aeruginosa, E. coli and A. parasiticus, A. niger and A. flavus fungi. It was noted from the growth curves of both bacteria and fungi that in the presence of silver nanoparticles they show more in-zone growth as compared to the plant extract.

Open access
Structural and optical properties of VO2+ doped methacrylic acid ethylacrylate (MAA:EA) copolymer films

Abstract

Pure and VO2+ doped methacrylic acid ethylacrylate (MAA:EA) copolymer films were prepared by using a solution casting method. Various techniques including X-ray diffraction, Fourier transform infrared spectroscopy, ultraviolet-visible spectroscopy, scanning electron microscopy and electron paramagnetic resonance were employed for characterization of the samples. XRD patterns showed some degree of crystallinity of the doped polymer films due to interaction of the MAA:EA copolymer with VO2+. FT-IR spectral studies of pure and VO2+ doped MAA:EA copolymer films displayed significant structural changes within the doped copolymer film indicating the complexation. The optical absorbance of the pure and VO2+ doped films were measured in the 200 nm to 800 nm wavelength range. The values of the absorption edge and indirect band gaps were calculated. The optical band gap decreased with the increase of mol% of VO2+. From the EPR spectra, the spin- Hamiltonian parameters (g and A) were evaluated. The values of the spin-Hamiltonian parameters confirmed that the vanadyl ions were present in MAA:EA copolymer films as VO2+ molecular ions in an octahedral site with a tetragonal compression (C4v). The morphology of the copolymer samples was examined by scanning electron microscopy. The enhanced crystalline nature of the doped copolymer was identified from SEM analysis.

Open access
In vitro evaluation of bioactivity of SiO2-CaO-P2O5-Na2O-CaF2-ZnO glass-ceramics

Abstract

Zinc is an essential trace element that stimulates bone formation but it is also known as an inhibitor of apatite crystal growth. In this work addition of ZnO to SiO2-CaO-P2O5-Na2O-CaF2 glass-ceramic system was made by conventional melt-quenching technique. DSC curves showed that the addition of ZnO moved the endothermic and exothermic peaks to lower temperatures. X-ray diffraction analysis did not reveal any additional phase caused by ZnO addition and showed the presence of wollastonite and hydroxyapatite crystalline phases only in all the glass-ceramic samples. As bio-implant apatite forming ability is an essential condition, the surface reactivity of the prepared glass-ceramic specimens was studied in vitro in Kokubo’s simulated body fluid (SBF) [1] with ion concentration nearly equal to human blood plasma for 30 days at 37 °C under static condition. Atomic absorption spectroscopy (AAS) was used to study the changes in element concentrations in soaking solutions and XRD, FT-IR and SEM were used to elucidate surface properties of prepared glass-ceramics, which confirmed the formation of HCAp on the surface of all glass-ceramics. It was found that the addition of ZnO had a positive effect on bioactivity of glass-ceramics and made it a potential candidate for restoration of damaged bones.

Open access
A novel photoelectrode of NiO@ZnO nanocomposite prepared by Pechini method coupled with PLD for efficiency enhancement in DSSCs

Abstract

The dye-sensitized solar cells made of NiO@ZnO nanoparticles were synthesized by a novel Pechini route using different NiO molar concentration ratios. The thermal, structural morphological, optical and electrical properties of the prepared samples were investigated using thermal gravimetric analysis and differential scanning calorimetery (TGA/DSC), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), FT-IR and Raman spectroscopy, UV-diffuse reflectance (UV-DRS), photoluminescence (PL) and current-voltage (I-V) measurements. The success of doping process was confirmed by the XRD patterns, which revealed the existence of new peak at 43.2° corresponding to secondary phase NiO. UV spectra exhibited red shifts in NiO doped ZnO NCs and PL spectra showed strong emission band at 355 nm. The doping of ZnO with NiO was intended to enhance the surface defects of ZnO. The current-voltage measurements showed an improvement of the short circuit photocurrent (Jsc) and fill factor (FF) and a decrease in the open circuit voltage (VOC) for dye-sensitized solar cell (DSSC) based on NiO-ZnO NCs. A clear enhancement in efficiency of DSSC from 1.26±0.10 % for pure ZnO to 3.01±0.25 % for NiO-ZnO NCs at the optimum doping with 1.5 mol% of NiO to ZnO (ZN1.5) was observed. The obtained material can be a suitable candidate for photovoltaic applications.

Open access