Synthesis and structural characterization of perovskite 0.65Pb(Mg1/3Nb2/3)O-3-0.35PbTiO(3) nanotubes

We report the synthesis and structural characterization of 0.65Pb(Mg1/3Nb2/3)O-3-0.35PbTiO(3) (PMN-PT) nanotubes prepared by a novel sal-gel template method. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) investigations demonstrated that the postannealed (650 degrees C for 1 h) PMN-PT nanotubes were polycrystalline with perovskite crystal structure. The field emission scanning electron microscope (FE-SEM) shows that as prepared PMN-PT nanotubes were hollow with diameter to be about 200 nm. High resolution transmission electron microscope (HRTEM) analysis confirmed that the obtained PMN-PT nanotubes made up of nanoparticles (10-20 nm) which were randomly aligned in the nanotubes. Energy-dispersive X-ray spectroscopy (EDX) analysis confirmed the stoichiometric 0.65Pb(Mg1/3Nb2/3)O-3-0.35PbTiO(3). The possible formation mechanism of PMN-PT nanotubes was proposed at the end. (C) 2011 Elsevier B.V. All rights reserved.

Sensors based on the dissipation characteristics of n-BaTiO3 ceramics and its solid solutions

The humidity, heat flux and mass flow sensing capability of n-BaTiO3 and its solid solutions were evaluated based on their dissipation characteristics. The cubic/tetragonal phase content of the ceramics seem to play an important role in their sensitivity towards the measurand. The humidity-sensitive characteristics of these perovskites were studied with respect to different moisture sensitive coating materials. The sensor was also used to determine the heat of hydration during the curing process of cements and the mass flow rate of the gases. For all these applications, suitable operating points have been fixed from the highly non-linear I-V characteristics with the retention of good stability and high sensitivity. (C) 1997 Elsevier Science S.A.

Synthesis and characterization of epoxy resins based on N,N'-aliphatic dicarboxyl bis(hydrazones)

A new class of epoxy resins having N-N bonds in their structure has been synthesized by reacting N,N'-aliphatic dicarboxyl bis(hydrazones) (the aldehyde/ketone derivatives of malonic, adipic, and sebacic dihydrazides) with epichlorohydrin. The reactivity of the[GRAPHICS] protons as a function of the substituent group and the number of methylene spacer groups present in the hydrazone has been examined. The resins obtained have been characterized by elemental and epoxy equivalent analyses and IR and NMR spectra. All these resins are found to have adequate viscosity and cure easily with amine curatives at elevated temperatures. Relevant properties for their use as binders in propellant formulations, such as thermal stability, heat of combustion, density, temperature dependence of viscosity, and mechanical strength of the composites, have been evaluated. (C) 1997 John Wiley & Sons, Inc.

Synthesis and characterization of N,N'-aliphatic dicarboxylbis(hydrazones)

N,N'-Malonylbis-,N,N'-adipinylbis- and N,N'-sebacoylbis-(hydrazones) 1 of various aldehydes and ketones have been prepared and characterized by elemental analyses, melting points, and H-1 NMR and IR spectral data.

The effect of aluminosilicate on the delayed onset of upturn voltages of zinc oxide varistor ceramics

The effect of aluminosilicate (Al2SiO5) on the upturn characteristics of ZnO varistor ceramics has been investigated. Addition of Al2SiO5 shifts the point of upturn above 10(4) A cm(-2). The extended nonlinearity in the high current density region is better correlatable to the presence of higher density of trap stales and changing pattern of trap depths at the grain boundary interface as much as the grain interior conductivity. Microstructure studies show the formation and involvement of a liquid phase during sintering. The secondary phases, predominantly are antimony spinel, Zn7Sb2O12, zinc silicate, Zn2SiO4 and magnesium aluminium silicate. MgAl2Si3O10. Energy dispersive X-ray analyses (EDAX) show that Al and Si are distributed more in the grain boundaries and within the secondary phases than in the grain interiors. Capacitance-voltage analyses and dielectric dispersion studies indicate the presence of negative capacitance and associated resonance, indicative of the oscillatory charge redistribution involving increased trapping at the interface states. The admittance spectroscopy data show that the type of trap slates remains unaltered whereas the addition of Al2SiO5 increases the density of low energy traps. (C) 1997 Published by Elsevier Science S.A.

The two-step positive temperature coefficient in resistance characteristics of n-(Ba,Pb)TiO3 ceramics created through inclusion of grain boundary modifier additives

Donor-doped n-(Ba,Pb)TiO3 polycrystalline ceramics exhibit distinctly two-step positive temperature coefficient of resistance (PTCR) characteristics when formulated with suitable combinations of B2O3 and Al2O3 as grain boundary modifiers by heterogeneous addition. B2O3 or Al2O3 when added singularly resulted in either steep or broad PTCR jumps respectively across the phase transition. The two-step PTCR is attributed to the activation of the acceptor states, created through B2O3 and Al2O3, for various temperature regimes above the Curie point (T-c). The changing pattern of trap states is evident from the presence of Ti4+-O--Al3+ type hole centres in the grain boundary layer regions, identified in the electron paramagnetic resonance (EPR) spectra. That charge redistribution occurs among the inter-band gap defect states on crossing the Curie temperature is substantiated by the temperature coefficient in the EPR results. Capacitance-voltage results clearly show that there is an increase in the density of trap states with the addition of B2O3 and Al2O3. The spread in energy values of these trap states is evident from the large change in barrier height (phi similar or equal to 0.25-0.6 eV) between 500 and 650 K.

Low temperature fabrication and impedance spectroscopy of PMN-PT ceramics

Single phase perovskite 0.9Pb(Mg1/3Nb2/3)O-3-0.1(PbTiO3) ceramics were prepared using the columbite precursor method after optimizing the synthesis conditions. X-ray diffraction (XRD) studies were carried out to verify the phase formation at each processing step. Scanning electron microscopy (SEM) was employed to observe the microstructure of the sintered ceramics. Impedance and modulus spectroscopic data were used to gain an insight into the electrical properties of the samples and with a view to observing the relaxations in them. (C) 1999 Elsevier Science Ltd.

Synthesis, spectral characterization and in vitro microbiological evaluation of novel glyoxal, biacetyl and benzil bis-hydrazone macrocyclic Schiff bases and their Co(II), Ni(II) and Cu(II) complexes

A series of binuclear Co(II), Ni(II) and Cu(II) complexes were synthesized by the template condensation of glyoxal, biacetyl or benzil bis-hydrazide, 2,6-diformyl-4-methylphenol and Co(11), Ni(II) or Cu(II) chloride in a 2:2:2 M ratio in ethanol. These 22-membered macrocyclic complexes were characterized by elemental analyses, magnetic, molar conductance, spectral, thermal and fluorescence studies. Elemental analyses suggest the complexes have a 2:1 stoichiometry of the type (M2LX2]center dot nH(2)O and Ni(2)LX(2)2H(2)O]center dot nH(2)O (where M = Co(II) and Cu(II); L = H2L1, H2L2 and H2L3; X = Cl; n = 2). From the spectroscopic and magnetic studies, it has been concluded that the Co(11) and Cu(11) complexes display a five coordinated square pyramidal geometry and the Ni(II) complexes have a six coordinated octahedral geometry. The Schiff bases and their metal complexes have also been screened for their antibacterial and antifungal activities by the MIC method. (C) 2011 Elsevier Ltd. All rights reserved.

Structural characterization and chain dynamics of poly(alpha-methylstyrene peroxide) by NMR spectroscopy

Poly(alpha-methylstyrene peroxide) has been synthesized and characterized spectroscopically. The H-1 and C-13 NMR spectra are shown to reveal the stereochemical features and the endgroups in the peroxide chain. The preliminary studies on the chain dynamics of the polyperoxide chain has been done by measuring the spin-lattice relaxation times (T-1) of the main chain as well as the side chain carbons. It has been shown from the dependence of the spin-lattice relaxation times that the polyperoxide chain is more flexible compared to the corresponding hydrocarbon-backbone analog.

Synthesis and characterization of novel charge transfer complexes formed by N,N%-bis(ferrocenylmethylidene)-p-phenylenediamine and N-(ferrocenylmethylidene)aniline

N,N'-Bis(ferrocenylmethylidene)-p-phenylenediamine 1 and N-(ferrocenylmethylidene) aniline 2 are readily synthesized by Schiff base condensation of appropriate units. Iodine (I-2), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), tetrachloro-1,4-benzoquinone (CA), tetracyanoethylene (TCNE) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) form charge transfer complexes with 1 and 2. IR spectroscopy suggests an increase in the amount of charge transferred from the ferrocenyl ring to the oxidant in the order, I-2 < CA < TCNQ < TCNE approximate to DDQ. EPR spectra of the oxidized binuclear complexes are indicative of localized species containing iron- and carbon-centered radicals. The Mossbauer spectrum of the iodine oxidized complex of 1 reveals the presence of both Fe(III) and Fe(II) centers. Variable temperature magnetic and Mossbauer studies show that the ratio of Fe(III)/Fe(II) centers varies as a function of temperature. The larger Fe(II)/Fe(III) ratio at lower temperatures is best explained by a retro charge transfer from the iodide to the iron(III) metal center. There is negligible solvent effect on the formation of the iodine oxidized charge transfer complex of 1. (C) 1999 Elsevier Science S.A. All rights reserved.

Synthesis and characterization of some new dimesogenic compounds

We have synthesized four different types of dimesogenic compounds involving the cholesteryl moiety as one of the mesogenic constituents, and have investigated their liquid crystalline properties. The molecular structures of these dimesogens have been confirmed by spectral analyses; they exhibit a rich polymorphism, as revealed by optical microscopic and differential scanning calorimetric observations. The studies show that the mesomorphic behaviour is sensitive to the nature of the terminal alkyl chains, and to the structure of the 'second mesogen' that is attached to the cholesteryl unit through a polymethylene spacer.

A Complete Characterization of an Optimal Timer Based Selection Scheme

Timer-based mechanisms are often used in several wireless systems to help a given (sink) node select the best helper node among many available nodes. Specifically, a node transmits a packet when its timer expires, and the timer value is a function of its local suitability metric. In practice, the best node gets selected successfully only if no other node's timer expires within a `vulnerability' window after its timer expiry. In this paper, we provide a complete closed-form characterization of the optimal metric-to-timer mapping that maximizes the probability of success for any probability distribution function of the metric. The optimal scheme is scalable, distributed, and much better than the popular inverse metric timer mapping. We also develop an asymptotic characterization of the optimal scheme that is elegant and insightful, and accurate even for a small number of nodes.

Characterization and catalytic properties of combustion synthesized Au/CeO2 catalyst

Ceria-supported Au catalyst has been synthesized by the solution combustion method for the first time and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Au is dispersed as Au as well as Au3+ states on CeO2 surface of 20-30 nm crystallites. On heating the as-prepared 1% Au/CeO2 in air, the concentration of Au3- ions on CeO2 increases at the expense of Au. Catalytic activities for CO and hydrocarbon oxidation and NO reduction over the as-prepared and the heat-treated 1% Au/CeO2 have been carried out using a temperature-programmed reaction technique in a packed bed tubular reactor. The results are compared with nano-sized Au metal particles dispersed on alpha-Al2O3 substrate prepared by the same method. All the reactions over heat-treated Au/CeO2 occur at lower temperature in comparison with the as-prepared Au/CeO2 and Au/Al2O3. The rate of NO + CO reaction over as-prepared and heat-treated 1% Au/CeO2 are 28.3 and 54.0 mumol g(-1) s(-1) at 250 and 300 degreesC respeceively. Activation energy (E,) values are 106 and 90 kJ mol(-1) for CO + O-2 reaction respectively over as-prepared and heat-treated 1% Au/CeO2 respectively.

Characterization of alkyl chain conformation in an intercalated cationic lipid bilayer by IR spectroscopy

A structural analysis of alkyl chain conformation of an intercalated cationic lipid bilayer is described. Dialkyl dimethylammonium ions (di-C(n)DA) were ion exchanged into the galleries of layered cadmium thiophosphate to give Cd0.83PS3(di-C(n)DA)(0.34). The grafting density and interlayer expansions were identical to those for the intercalated single chain alkyl trimethylammonium (C(n)TA) bilayers. The increased methylene chain density in the galleries, however, forces the intercalated lipid to adopt a more trans ordered structure. Progression bands arising from the coupling of vibrational modes of trans methylene units are used to establish the extent of trans registry. Two types of ordered structures of the intercalated cationic lipid may be distinguished. One in which both alkyl chains adopt an all-trans geometry, and one in which the methylene bond adjacent to the headgroup on one of the alkyl chains is gauche. The latter structure is typically found in the crystalline state of these cationic lipids. The concentrations of the two structures were determined from the ratio of the intensities of the progression bands and were found to remain unchanged with temperature.

Characterization of electrochemically deposited Cu-Ni black coatings

Electrochemically deposited Cu-Ni black coatings on molybdenum substrate from ethylenediaminetetraacetic acid (EDTA) bath solution are shown to exhibit good optical properties (alpha = 0.94, epsilon = 0.09). The deposit is characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Cu is present in metallic and +2 oxidation states in the as-prepared Cu-Ni black coating, whereas Ni2+ as well as Ni3+ species are observed in the same coating. Cu and Ni are observed in their metallic state after 10 and 20 min sputtering. X-ray initiated Auger electron spectroscopy (XAES) of Cu and Ni also agrees well with XPS investigations. (C) 2002 Elsevier Science Ltd. All rights reserved.