Synthesis and characterization of Zn1-xMnxS nanocrystalline films prepared on glass substrates

Nanocrystalline Zn1-xMnxS films (x=0.04, 0.08 and 0.12) were deposited on glass substrates at 400 K using a simple resistive thermal evaporation technique. All the deposited films were characterized by chemical, structural, morphological, optical and magnetic properties. Scanning electron microscopy and atomic force microscopy studies showed that all the films investigated were in nanocrystalline form with the grain size lying in the range 10–20 nm. All the films exhibited cubic structure and the lattice parameters increase linearly with composition. The absorption edge shifted from the higher-wavelength region to lower wavelengths with increase in Mn concentration. The magnetization increased sharply with increase of the Mn content up to x=0.08 and then decreased with further increase of the Mn content. Particularly, Zn0.92Mn0.08S concentration samples show a weak ferromagnetic nature, which might be the optimum concentration for optoelectronic and spintronic device applications.

Unusual Hydrogenation of Fumarate Anion Followed by Metal−Carbon Bond Formation: Synthesis and Characterization of Two Metallochelates

The treatment of [M(dppf)(H2O)2](OTf)2 (dppf =1,1′-bis(diphenylphosphino)ferrocene; M = Pd, Pt) with 1 equiv of disodium fumarate in methanol medium showed an unusual hydrogenation of the ethylenic bond followed by the formation of metallochelates linking M through one of the carboxylates and the β-carbon with respect to COO−. Despite the possibility of formation of a [2 + 2] or [4 + 4] self-assembled macrocycle, the reduction of fumarate to succinate, and in particular the linking through the β-carbon, is unique since a similar treatment using disodium succinate instead of disodium fumarate yielded an expected metallochelate where both the carboxylates were coordinated to the square-planar metal.

Hydrothermal synthesis and characterization of CaSO4 pseudomicrorods

Calcium sulphate (CaSO4) pseudomicrorods have been synthesized by alow-temperature hydrothermal method using CaSO4 powder as a precursor and hexadecylamine as a surfactant at 180 degrees C for at different intervals of time. The powder X-ray diffraction pattern indicates that the as-formed pseudomicrorods are of orthorhombic phase with lattice parameters a = 7.0023(4) angstrom, b = 6.9939(5) angstrom and c = 6.2434(4) angstrom. Scanning electron microscopy images show that the pseudomicrorods have diameters of about 0.2-2.5 mm and lengths of about 2-10 mm. Fourier transform infrared spectroscopy shows a strong doublet near 609 and 681 cm(-1) arising from nu(4) (SO42) bending vibrations. The strongest band observed at 1132 cm(-1) is associated with nu(3) (SO42-) stretching vibrations. The band near 420-450 cm(-1) is attributed to nu(2) (SO42-) bending vibrations. The Raman spectrum exhibits an intense peak at 1008 cm(-1) associated with the SO42- mode. The photoluminescence spectrum exhibits UV bands (330, 350 nm), strong green bands (402, 436 nm) and weak blue bands (503 nm). A widening of the optical band gap was observed as the particle size decreased.

Synthesis and Characterization of a Class of Donor-Acceptor Conjugated Molecules: Experiments and Theoretical Calculations

A class of conjugated molecules containing donor (thiophene) and acceptor (malononitrile) is synthesized by Knoevenagel condensation reaction between 2-(2,6-dimethy1-4H-pyran-4-ylidene) malononitrile and thiophene carbaldehyde containing two and three thiophene units. The resulting molecules are characterized by H-1 and C-13 NMR. We have performed UV-vis absorption, fluorescence, and cyclic voltammetry measurements on these materials. The spectroscopic and electrochemical measurements proved beyond doubt that these materials possess lowexcitation gap and are suitable for being an active material in various electronic devices. We have also performed electronic structure calculations using density functional theory (DFT) and INDO/SCI methods to characterize the ground and excited states of this class of molecules. These donor-acceptor molecules show a strong charge transfercharacter that increases with the increase in the number of thiophene rings coupled to the malononitrile acceptor moiety. We have also calculated the pi-coherence length, Stoke's shift, and effect of solvents on excited states for this class of molecules, Our theoretical values agree well with experimental results.

Chain structures in alkali metal borophosphates: synthesis and characterization of K3[BP3O9(OH)3] and Rb3[B2P3O11(OH)2]

Two new alkali metal borophosphates, K-3[BP(3)o(9)(OH)(3)] and Rb-3[B2P3O11(OH)(2)], were synthesized by applying solvothermal techniques using ethanol as solvent. The crystal structures were solved by means of single-crystal X-ray diffraction (K-3[BP3O9(OH)(3)], monoclinic, C2/c (No. 15), a = 2454.6(8) pm, b = 736.3(2) pm, c = 1406.2(4) pm, beta = 118.35(2)degrees, Z = 8; Rb-3[B2P3O11(OH)(2)], monoclinic, P2(1)/c (No. 14), a = 781.6(2) pm, b:= 667.3(2) pm, c = 2424.8(5) pm, beta = 92.88(1)degrees, Z = 4). Both crystal structures comprise borophosphate chain anions. While for the rubidium compound a loop-branched chain motif is found as common for most of the chain anions in alkali metal borophosphates, the crystal structure of the potassium phase comprises the first open-branched chain with the highest phosphate content found so far in this group of compounds. Both chain anions are Closely related to known anhydrous or hydrated phases, and the structural relations are discussed in terms of how the presence of OH groups and hydrogen bonds as well as number, charge, and size of charge balancing cations influence the 3D structural arrangement. The anionic entities are classified in terms of general principles of structural systematics for borophosphates.

Synthesis and characterization of polyaniline salts with phenoxy acetic acids by emulsion polymerization

Polyaniline salts have been synthesized by chemical oxidative polymerization of aniline in the presence of phenoxy acetic acid and its two derivatives using emulsion method at room temperature and characterized by different techniques such as infrared, H-1 and C-13 NMR, UV-visible spectroscopy, SEM, wide angle X-ray diffractograms and conductivity measurements. These polyaniline salts have the desirable property of high solubility for processibility in solvents such as DNIF, DMSO and a mixture of CHCl3 and acetone and they exhibit fairly good conductivity of similar to 3.0 x 10(-3) S cm(-1). The variations in solubility, conductivity and morphology with the protonating strength of the dopants are examined.

A simple synthesis and characterization of CuS nanocrystals

Water-soluble CuS nanocrystals and nanorods were prepared by reacting copper acetate with thioacetamide in the presence of different surfactants and capping agents. The size of the nanocrystals varied from 3-20 nm depending on the reaction parameters such as concentration, temperature, solvent and the capping agents. The formation of nanocrystals was studied by using UV-visible absorption spectroscopy.

Synthesis and characterization of Ti5Te4-type molybdenum cluster compounds, AxMo5As4(A = Cu, Al, or Ga)

A new series of molybdenum cluster compounds of the general formula AxMo5As4(A = Cu, Al, or Ga) has been synthesized. They are isostructural with the host Mo5As4(Ti5Te4-type) consisting of trans-vertex shared Mo6 octahedral chains. Investigations by X-ray photoelectron and Auger electron spectroscopies revealed a charge transfer from A to Mo5As4 in AxMo5As4. The occurrence of metallic (CuxMo5As4) and non-metallic (Al2Mo5As4 and Ga2Mo5As4) properties in this isostructural series of solids is consistent with the electronic structure of Ti5Te4-type solids involving M–M bonding in the cluster chains.

Synthesis and characterization of Pd(0), PdS, and Pd@PdO core-shell nanoparticles by solventless thermolysis of a Pd-thiolate cluster

Colloids of palladium nanoparticles have been prepared by the solvated metal atom dispersion (SMAD) method. The as-prepared Pd colloid consists of particles with an average diameter of 2.8 +/- 0.1 nm. Digestive ripening of the as-prepared Pd colloid, a process involving refluxing the as-prepared colloid at or near the boiling point of the solvent in the presence of a passivating agent, dodecanethiol resulted in a previously reported Pd-thiolate cluster, Pd(SC12H25)(2)](6) but did not render the expected narrowing down of the particle size distribution. Solventless thermolysis of the Pd-thiolate complex resulted in various Pd systems such as Pd(0), PdS, and Pd@PdO core-shell nanoparticles thus demonstrating its versatility. These I'd nanostructures have been characterized using high-resolution electron microscopy and powder X-ray diffraction methods. (C) 2010 Elsevier Inc. All rights reserved.

Synthesis and characterization of metal substituted AlxCr1-x(acetylacetonate)(3) single-source precursors for their application to MOCVD of thin films

A detailed study, involving the synthesis of a single-source precursor containing two metal ions sharing the same crystallographic site, has been undertaken to elucidate the use of such a single-source precursor in a CVD process for growing thin films of oxides comprising these two metals, ensuring a uniform composition and distribution of metal ions. The substituted complexes Cr1-xAlx(acac)(3), where acac = acetyl-acetonate, have been prepared by a co-synthesis method, and characterized using UV-Vis spectroscopy. TGA/DTA measurements, and single crystal X-ray diffraction at low temperature. All the studied compositions crystallize in the monoclinic space group P2(1)/c with Z = 4 in the unit cell. It was observed that the ratio (Al:Cr) of the site occupancy for the metal ions, obtained from single crystal refinement, is in agreement with the results obtained from complexometric titrations. All the solid state structures have the metal in an octahedral environment forming six-membered chelate rings. M-O acac bond lengths and disorder in the terminal carbon have been studied in detail for these substituted metal-organic complexes. One composition among these was chosen to evaluate their suitability as a single-source precursor in a LPMOCVD process (low-pressure metal-organic chemical vapour deposition) for the deposition of a substituted binary metal oxide thin film. The resulting thin films were characterized by X-ray diffraction, scanning electron microscopy, and infrared spectroscopy. (C) 2010 Elsevier Ltd. All rights reserved.

Synthesis and characterization of thiocarbonohydrazone-based epoxy resins

Novel epoxy resins of various thiocarbonohydrazones have been synthesized by reacting the aldehyde or ketone derivatives of thiocarbohydrazide with excess of epichlorohydrin. The resins have been characterized by elemental analyses, epoxy equivalents, 1H-NMR and IR spectra, thermal analyses, and viscosity measurements. Curing of the resins has been carried out by mixing with thiocarbohydrazide or ethylenediamine and heating at 80°C for 48 h. A comparison of the thermal stability of the cured resin samples has been made.

Synthesis and characterization of flexible epoxy nanocomposites reinforced with amine functionalized alumina nanoparticles: a potential encapsulant for organic devices

Research on conducting polymers, organic light emitting diodes and organic solar cells has been an exciting field for the past decade. The challenge with these organic devices is the long term stability of the active material. Organic materials are susceptible to chemical degradation in the presence of oxygen and moisture. The sensitivity of these materials towards oxygen and moisture makes it imperative to protect them by encapsulation. Polymer nanocomposites can be used as encapsulation materials in order to prevent material degradation. In the present work, amine functionalized alumina was used as a cross-linking and reinforcing material for the polymer matrix in order to fabricate the composites to be used for encapsulation of devices. Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and Raman spectroscopy were used to elucidate the surface chemistry. Thermogravimetric analysis techniques and CHN analysis were used to quantify grafting density of amine groups over the surface of the nanoparticles. Mechanical characterizations of the composites with various loadings were carried out with dynamic mechanical analyzer. It was observed that the composites have good thermal stability and mechanical flexibility, which are important for an encapsulant. The morphology of the composites was evaluated using scanning electron microscopy and atomic force microscopy.