Synthesis and characterization of fine lithium niobate powders by sol‐ gel method

Lithium niobate (LN) nanocrystal powders were prepared by low‐temperature sol‐gel method. Dihydrate lithium acetate as lithium source, and niobium chloride as niobium source were used as starting materials. The gel and powders were characterized by thermogravimetry and differential scanning calorimetry (TG/DSC), X‐ray diffraction (XRD), transmission electronmicroscopy (TEM) and Fourier transform infrared (FTIR) spectra. The results show that when the gel was heat‐treated at 600°C, the fine LN nanocrystals with the size of 40‐60 nm were obtained, and the size of the powders become larger with the heat‐treated temperature increasing. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of Cu2ZnSnSe4 nanocrystals prepared by one pot route

Quaternary compound Cu₂ZnSnSe₄ (CZTSe) is one of the most promising absorber layer materials for thin film solar cells. In present work, the CZTSe nanocrystals were successfully synthesized via one pot route, and the influences of reaction temperature on the structural, compositional, morphological and optical properties of as‐synthesized CZTSe nanocrystals were investigated in detail via X‐ray powder diffraction (XRD), energy dispersive X‐ray spectrometry (EDS), transmission electron microscopy (TEM) and UV‐Vis spectrophotometry, respectively. The characterization results of as‐synthesized nanocrystals, under optimal synthesis condition (250 °C, 1 h), indicated that the nanocrystals was monodispersed with polycrystalline, the size was in the range of 10–15 nm, and the band gap energy was around 1.44 eV which is very closed to the best band gap energy for the solar cell. All results suggested that the as‐synthesized CZTSe nanocrystals were good light absorber layer material for thin film solar cell.     

Effects of Er3+ doping concentration and calcination on fluorescence properties of La3Ga5.5Nb0.5O14 nanocrystals

The effects of Er³⁺ doping concentration and calcination were examined on the fluorescence properties of La₃Ga_5.5Nb_0.5O₁₄ (Er:LGN) nanoparticles for the first time. High quality Er:LGN nanoparticles were synthesized by sol‐gel method. The room temperature fluorescence spectra showed a green emission, which can be attributed to ²H_11/2‐⁴I_15/2 and ⁴S_3/2‐⁴I_15/2 transition. The relationship between the relative emission intensity and the doping concentration was investigated. The maximum of the Er³⁺ doping concentration in LGN nanopowders is 2.0%. The fluorescent lifetime of 2.0% Er:LGN nanoparticles is 1.45ns. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and characterization of electrodeposited indium selenide thin films

Indium Selenide (InSe) thin films were deposited from a mixture of Indium chloride and selenium dioxide in aqueous solution by electrodeposition technique on Indium Tin oxide coated glass substrates. The effects of the parameters during deposition such as current density, deposition potential versus saturated calomel electrode, pH value and concentration of source material were studied. X‐ray diffraction studies were carried out on the films to analyze the microstructure using an x‐ray diffractometer and were examined by RAMAN spectroscopy. The Raman peak position did not change much with chemical concentrations. Raman scattering due to the (LO) phonon was observed at 211 cm^–1. Optical absorption studies were performed with a double beam ultra violet‐visible –NIR spectrophotometer in the wavelength 300–1100 nm. The surface morphology of the layer was examined using a scanning electron micrograph. The composition of the films was studied using an Energy Dispersive Analysis by X‐Rays (EDAX).     

Effect of ferric ions on the morphology and size of magnetite nanocrystals synthesized by ultrasonic irradiation

Two‐dimensional plate‐like Fe₃O₄ nanocrystals and nanoparticles could be synthesized by a simple one‐step sonochemical method through ultrasonic irradiation in reverse co‐precipitation solution at low temperature. This technique provided a facile and rapid way to prepare Fe₃O₄nanocrystals with different morphology and size. Magnetite nanoplates were synthesized with only ferrous salt adding into alkali solution, and adding ferric ions with low molar ratio in the metal salts solution would lead to the formation of very small magnetite nanoparticles (∼10 nm). The size of as‐prepared magnetite nanoparticles increased with increasing reaction temperature and showed narrow size distribution, the standard deviation less than 2 nm. This investigation indicated that ferric ions had significant influence on the morphology of Fe₃O₄ nanocrystals. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis via an organic molten salt solvent route and characterization of PbS nanocrystals

In this paper, four petals flowers‐like and quasi sphere‐like PbS nanostructures were successfully synthesized by an environment friendly organic molten salt solvent (OMSS) route at 200 °C, with different sulfur sources, e.g. thiourea and sodium thiosulfate, respectively. The as‐synthesized products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), UV–vis absorption spectrum and photoluminescence (PL) spectrum, respectively. It was shown that four petals flowers‐like and quasi sphere‐like PbS nanocrystals were formed. It was also demonstrated that the morphologies of PbS nanocrystals were significantly influenced by different sulfur sources. The ultraviolet‐visible absorption peaks of PbS nanocrystals exhibited a large blue‐shift and the luminescence spectra had strong and broad emission bands centered at 488 nm and 492 nm. The possible formation mechanisms of the PbS nanostructures were discussed. The organic molten salt solvent (OMSS) method is preferable for synthesizing high‐quality PbS nanocrystals. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of colloidal gallium selenide nanowires

We report first to date ‘green’ metalorganic‐free synthesis of colloidal GaSe nanocrystals. Structure and optical properties of gallium selenide nanocrystals dispersed in oleylamine are discusses in respect to that conventionally prepared in alkylphosphonic solutions. We explore the organization of the particles into nanowires and propose appropriate growth mechanism. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of L‐phenylalanine

L‐Phenylalanine (C₉H₁₁NO₂), having the morphology of spherulitic needles, an amino acid constituent, responsible for brain nutrition is crystallized in silica gel of pH 6.0 by single diffusion method in a period of 30 minutes. The grown crystals were characterized by X‐ray powder diffraction, Fourier Transform infrared spectroscopy and Visible Ultraviolet spectroscopy. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural and optical response of 2‐Mercaptoethonal capped CdS nanocrystals to Fe3+ ions

Cadmium sulfide (CdS) semiconductor nanocrystals (NCs) doped with Fe³⁺ have been synthesized via a solution‐based method utilizing dopant concentrations of (0–5%) and employing 2‐mercaptoehonal as a capping agent. X‐ray diffraction (XRD) results showed that the undoped CdS NCs are in mixed phase of cubic and hexagonal, where as the doped CdS NCs are in hexagonal phase. The crystallite size was increased from ∼1.2 nm to ∼2 nm. Diffuse reflectance spectroscopy studies (DRS) reveals that the band gap energy was decreased with Fe doping and it lies in the range of 2.58 ‐ 2.88 eV. Photoluminescence (PL) spectra of undoped CdS NCs show a strong green emission peak centered at 530 nm and a weak red emission shoulder positioned at 580 nm. After doping all the luminescence intensity was highly quenched and the green emission peak was shifted to orange region (580 nm), but the position of weak red emission shoulder was unaltered with doping. FTIR studies revealed that the NCs were sterically stabilized by 2‐mercaptoethanol. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Co nanoclusters as origin of ferromagnetism in sol‐gel synthesized Zn1‐xCoxO (x = 0.05, 0.10 and 0.15) samples

We report on the structural and magnetic properties of the polycrystalline samples of Zn_1‐xCo_xO (x = 0.05, 0.10 and 0.15) synthesized via sol‐gel route. The air sintered samples of all compositions exhibit paramagnetic behaviour at room temperature, on the other hand the same samples on annealing in Ar/H₂ atmosphere show room temperature ferromagnetism (RTFM) with enhanced magnetization. The value of magnetization increases with the Co concentration (x) in both the air sintered and Ar/H₂ annealed samples. The observed ferromagnetism in the Ar/H₂ annealed Zn_1‐xCo_xO (x = 0.05, 0.10 and 0.15) samples is attributed to the presence of Co nanoclusters as detected by XRD and FESEM‐EDAX. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and characterization of Nd doped gadolinium gallium garnet nanopowders and crystals

The structural and optical features of gallium gadolinium garnet (GGG) nanopowders doped with neodymium were investigated. Nanopowders of GGG:Nd were prepared by modified sol‐gel method using acetic acid as complexing agent. This way permitted to incorporate large amounts of dopant (up to 10 %) without destroying garnet structure. Small single crystals of Nd:GGG were grown by a μ‐pulling down method and spectroscopic features of nanopowders and their single crystal counterparts were compared. It has concluded that the Nd³⁺ ions are located preferentially in the same type of sites in crystal lattices of GGG:Nd nanopowders and their single crystal counterparts. In addition, it follows from the perfect agreement of emission wavelengths and line width recorded for nanopowders and single crystal samples that the crystal lattice of GGG in nanopowders is not distorted. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of Nd,Yb – yttrium oxide nanopowders obtained by sol‐gel method

Nanopowders of Y₂O₃ pure, doped and codoped by Nd³⁺, Yb³⁺ were obtained by sol‐gel method. Solution with ethylene glycol was choosed as the proper solution where crystallites of powder with Nd and Yb dopants had the same size. Finally the one‐phased compounds of Y₂O₃ doped 0.5 at% Nd and 1, 2 or 4 at% Yb were obtained. Grain growth and their morphology were investigated in various temperature and time of heating. The changes of crystallite sizes and lattice constants in relation to the heating time and temperature for the composition Y₂O₃ doped 0.5 at% Nd and 2 at% Yb are presented. Y₂O₃ containing 0,5 at% of Nd exhibits intense luminescence bands centered at 920 nm, 1100 nm and 1360 nm whereas a single band at about 1020 nm appears in samples co‐doped with neodymium and ytterbium. Luminescence spectra recorded did not depend on the sample preparation procedure and size of grains. OH impurity affects critically the relaxation dynamics of luminescent ion in nanopowders. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of YCOB single crystals by flux technique and their characterization

Nonlinear optical single crystals of YCOB with good optical quality were grown by the flux technique for the first time. Polycrystalline YCOB samples were synthesized by solid state reaction method. The thermal analysis of the sample was performed with lithium carbonate flux in different weight proportions and the growth temperature was optimised. Single crystals of YCOB with dimensions 3 × 3 × 5 mm³ were obtained by the method of ‘slow‐cooling’. The grown crystals were characterized by XRD, UV‐VIS‐NIR, EDAX, FTIR and etching studies. The powder XRD pattern revealed the formation of YCOB compound. The lattice parameters were identified through single crystal XRD studies. The UV‐VIS‐NIR results showed that the crystal has a sharp cutoff at 220 nm and is nearly 55% transparent over a wide wavelength range enabling applications in the UV region. The EDAX measurement revealed the ‘flux‐free’ crystal formation. The presence of the functional groups belonging to the YCOB crystals was identified by the FTIR results. ‘Hillock‐like’ patterns are observed in the etching studies. The primary emphasis in this study is laid to describe ‘flux technique’ as an alternative method to grow YCOB crystals. The results are presented and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of cadmium tartrate single crystals

Efforts have been successful to crystallize the electroceramic compound of cadmium tartrate through silica hydrogel. Analysis of thermograms reveals decomposition of the crystals to take place within the temperature range 65 to 442°C in air atmosphere. Some important characteristic data, i.e., valance electron plasma energy, Penn gap, Fermi energy, interionic distance, electronic polarizability have been obtained. The DC conductivity of the crystal typically lies between the conductivities of metal and insulator and we derived several pertinent parameters such as hopping energy, hopping distance, coulomb gap, etc. The micromechanical indentation of the crystal shows nonlinear variation of the impact microhardness as a function of the applied load. The estimation of fracture toughness, fragility coefficient and yield strength has too been made for the synthesized crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Sol‐gel synthesis of electrospun BaO/MnO nanocomposite fibers and their magnetic characterization

A new approach, combining in‐situ sol‐gel process with electrospinning, was used to prepare magnetic barium acetate/manganese acetate/poly (vinyl alcohol) (PVA) composite nanofibers. The composite gel was synthesized by sol‐gel method in the presence of 10 wt.% PVA aqueous solution. PVA was used as stabilizer and polymeric matrix. The resultant barium acetate/manganese acetate/PVA composite nanofibers were calcined at 1023 K for 5 h. This formed BaO/MnO nanocomposite crystalline fibers with average diameter less than 100 nm and were characterized with Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Energy Dispersive X‐ray Analysis (EDAX), powder X‐ray diffractometer (XRD), UV‐Vis‐Spectroscopy (UV) and Vibrating Sample Magnetometer (VSM) respectively. These composite fibers exhibited a uniform cylindrical morphology, with the BaO/MnO nanoparticles implanted in the fibers. M‐H curves were obtained at 300 K and 20 K. From the M‐H curves, room temperature ferromagnetism was observed at 300 K. At low temperatures, the ferromagnetic behavior was masked by the paramagnetic behavior. The saturation magnetization at 300 K was found to be 0.004 emu /g and the saturation magnetization at 20 K was found to be 0.658 emu /g. The magnetization at 20 K was found to be very large and it was several times larger than at 300 K. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of borono phenylalanine

Borono phenylalanine abbreviated as BPA is a biologically important compound which is obtained from L‐Phenylalanine (C₉H₁₁NO₂) in which a boron atom is bonded. BPA is an amino acid analogue, helpful in the treatment of glioblastoma multiforme, a highly malignant form of brain tumor is crystallized in silica gel under pH 6.0 by single diffusion method in a period of 30 minutes. The grown crystals were characterized by x‐ray powder diffraction, Fourier Transform infrared spectroscopy and visible ultraviolet spectroscopy. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of MnTe nanocrystals in glass

The first evidence of the growth of MnTe nanocrystals successfully synthesized in a glass matrix (SiO₂–Na₂CO₃–Al₂O₃–B₂O₃) using the fusion method is reported. Measurements of optical absorption, photoluminescence, electronic paramagnetic resonance and atomic force microscopy were carried out in order to characterize the produced nanocrystals.     

Preparation and characterisation of Ag incorporated Al2O3 nanocomposite films obtained by sol‐gel method

Sol‐gel route has been applied for a deposition of the thin films of aluminum oxide and Ag embedded in Al₂O₃ films. The films are spin‐coated on Si and quartz substrates with the film thickness of 120 nm. XRD analysis has been used for the determination of the film structure. FTIR spectroscopy is applied for studying vibrational properties of the obtained coatings. Optical characterization is done by UV‐VIS spectroscopy. The formation of Ag nanoparticles has been confirmed by XRD and optical data. The sol‐gel process is found to be useful technology for incorporation of Ag nanoparticles in the metal oxide matrices. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterisation of gadolinium samarium oxalate single crystals

Single crystals of Gadolinium Samarium Oxalate (GSO) are grown by gel method. The crystals are pale yellowish in colour. Morphology and size of the crystals are found to depend on pH of the medium, gel density, concentration of the reactants and acidity of the feed solution. The crystallinity of the grown sample was confirmed by X‐ray diffraction studies and the lattice parameters were determined. X‐ray diffractogram shows well defined peaks. IR spectrum confirms the presence of water molecules and carboxylic group. EDAX analysis confirms the presence of Gd and Sm in the sample. The thermal decomposition behaviour of the crystal was analysed using TGA and DTA studies. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of magnesium doped lead titanate

Magnesium (Mg) doped lead titanate powders (PT: Mg) ceramics, with various Mg contents (0, 2.5, 5, 7.5, 10, 12.5, 15, 17.5, 20, and 30 mole %), are prepared by the sol‐gel method and characterized by X‐Ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy. XRD results show that the magnesium diminishes the lattice tetragonality of PT:Mg. The average particle size and morphology were studied by SEM. The investigations done by Raman spectroscopy allow the analyzis of the substitution mechanism behavior related to the Mg incorporation into PT structure. A concentration threshold appears around 10% of Mg corresponding in a change of the compensation process with Mg²⁺ ions replacing Pb²⁺ ions below and both Pb²⁺ and Ti⁴⁺ above. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)