Structural characterization of organometallic-derived 9.5/65/35 PLZT ceramics

This study consisted of an investigation of the influence of powder preparation on the phase and chemical compositions and microstructure of 9.5/65/35 PLZT materials sintered in an oxygen atmosphere. The powders with the formula Pb0.905La0.095(Zr0.65Ti0.35)(0.976)O-3+3.5 wt.% PbO were prepared by the polymeric organometallic precursor method (the Pechini method and the partial oxalate procedure). Phase composition was determined by X-ray diffraction of powder and EDS analysis, while grain size was determined based on the micrograph obtained from SEM. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Titanium and zirconium complexes containing sterically hindered hydrotris(pyrazolyl)borate ligands: synthesis, structural characterization, and ethylene polymerization studies

The synthesis, characterization and ethylene polymerization behavior of a set of Tp'MCl3 complexes (4, M = Ti, Tp' HB(3-neopentyl-pyrazolyl)(3)(-) (Tp(NP)); 5, M = Ti, Tp'= HB(3-tert-butyl-pyrazolyl)(3)(-) (Tp(tBu)); 6, M = Ti, Tp' = HB(3-phenyl-pyrazolyl)(3)(-) (Tp(Ph)); 7, M = Zr, Tp' = HB(3-phenyl-pyrazolyl)(3)(-) (Tp(ph)); 8, M = Zr, Tp' = HB(3-tert-butyl-pyrazolyl)(3)(-) (Tp(tBu))) is described. Treatment of these tris(pyrazolyl)borate Group IV compounds with methylalumoxane (MAO) generates active catalysts for ethylene polymerization. For the polymerization reactions performed in toluene at 60 degreesC and 3 atm of ethylene pressure, the activities varied between 1.3 and 5.1 X 10(3) g of PE/mol[M](.)h. The highest activity is reached using more sterically open catalyst precursor 4. The viscosity-average molecular weights ((M-v) over bar) of the PE's produced with these catalyst precursors varying from 3.57 to 20.23 x 10(5) gmol(-1) with melting temperatures in the range of 127-134 degreesC. Further polymerization studies employing 7 varying Al/Zr molar ratio and temperature of polymerization showed that the activity as well as the polymer properties are dependent on these parameters. In that case, higher activity was attained at 60 degreesC. The viscosity-average molecular weights of the polyethylene's decreases with increasing AI/Zr molar ratio. (C) 2003 Elsevier B.V. All rights reserved.

Synthesis and structural characterization of dichlorobis (1-phenyl-3-methylpyrazole) palladium(II) and diazidobis (1-phenyl-3-methylpyrazole) palladiium(II)

Mononuclear pyrazolyl Pd(II) complexes of the type [PdX2(phmPz)(2)] (X = Cl-, N-3(-)) have been prepared. The 1-phenyl-3-methylpyrazole displaces acetonitrile from [PdCl2(CH3CN)(2)] to form [PdCl2(PhMPz)(2)] (phmPz = 1-phenyl-3-methylpyrazole) (1). [Pd(N-3)(2)(PhmPz)(2)] (2) could be obtained by metathesis from [PdCl2(CH3CN)(2)] or by substitution of the chloride in (1) by the azide ion. Both complexes were characterized by elemental analysis, infrared spectroscopy, H-1 and C-13 NMR and by single crystal X-ray diffraction. The coordination geometry around Pd(II) in these complexes is nearly square-planar, with the ligands in a trans configuration.

Pyrosol preparation and structural characterization of SnO2 thin films

Polycrystalline tin oxide thin films were prepared from ethanol solution of SnCl2.H2O (concentrations: 0.05, 0.1, 0.2 and 0.4 mol/dm(3)) at different substrate temperatures ranging from 300 to 450 degreesC. The kinetic deposition processes were studied in terms of various process parameters. The crystal phases, crystalline structure, grain size and surface morphology are revealed in accordance to X-ray diffractometry and scanning electron microscopy (SEM). Texture coefficients (TCs) for (110), (2 0 0), (2 11) and (3 0 1) reflections of the tetragonal SnO2 were calculated. Structural characteristics of deposited films with respect to varying precursor chemistry and substrate temperature are presented and discussed. (C) 2003 Published by Elsevier B.V.

Synthesis and structural characterization of a new polymeric zinc(II) complex with thiophene-2-carboxylic acid

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

New Ni(II)-sulfonamide complexes: Synthesis, structural characterization and antibacterial properties. X-ray diffraction of [Ni(sulfisoxazole)(2)(H2O)(4)] center dot 2H(2)O and [Ni(sulfapyridine)(2)]

The synthesis, structural characterization, voltammetric experiments and antibacterial activity of [Ni(sulfisoxazole)(2)(H2O)(4)] center dot 2H(2)O and [Ni(sulfapyridine)(2)] were studied and compared with similar previously reported copper complexes. [Ni(sulfisoxazole)(2)(H2O)(4)] center dot 2H(2)O crystallized in a monoclinic system, space group C2/c where the nickel ion was in a slightly distorted octahedral environment, coordinated with two sulfisoxazole molecules through the heterocyclic nitrogen and four water molecules. [Ni(sulfapyridine)(2)] crystallized in a orthorhombic crystal system, space group Pnab. The nickel ion was in a distorted octahedral environment, coordinated by two aryl amine N from two sulfonamides acting as monodentate ligands and four N atoms (two sulfonamidic N and two heterocyclic N) from two different sulfonamide molecules acting as bidentate ligands. Differential pulse voltammograms were recorded showing irreversible peaks at 1040 and 1070 mV, respectively, attributed to Ni(II)/Ni(III) process. [Ni(sulfisoxazole)(2)(H2O)(4)] center dot 2H(2)O and [Ni(sulfapyridine)(2)] presented different antibacterial behavior against Staphylococcus aureus and Escherichia coli from the similar copper complexes and they were inactive against Mycobacterium tuberculosis. (c) 2007 Elsevier B.V. All rights reserved.

Thermal and structural characterization of SrTi(1-x)Nd(x)O(3)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Structural characterization of the cell wall D-glucans isolated from the mycelium of Botryosphaeria rhodina MAMB-05

Three D-glucans were isolated from the mycelium of the fungus Botryosphaeria rhodina MAMB-05 by sequential extraction with hot-water and hot aqueous KOH (2% w/v) followed by ethanol precipitation. Following their purification by gel permeation chrornatography on Sepharose CL-4B, the structural characteristics of the D-glucans were determined by FT-IR and C-13 NMR spectroscopy and, after methylation, by GC-MS. The hot-water extract produced a fraction designated Q(1A) that was a beta-(1 -> 6)-D-glucan with the following structure:[GRAPHICS]The alkaline extract, when subjected to repeated freeze-thawing, yielded two fractions: KIP (insoluble) that comprised a beta-(1 -> 3)-D-glucan with beta-D-glucose branches at C-6 with the structure:[GRAPHICS]and K1SA (soluble) consisting of a backbone chain of alpha-(1 -> 4)-linked D-glucopyranosyl residues substituted at O-6 with alpha-D-glucopyranosyl residues:[GRAPHICS](c) 2008 Elsevier Ltd. All rights reserved.

New chelate complexes of trivalent Y and lanthanides (Eu, Ho, Yb) with a triazene N-oxide: Synthesis, structural characterization and luminescence properties

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Synthesis and solid-state structural characterization of bis (thiocyanatemercury)tetracarbonyliron

The bis (thiocyanatemercury)tetracarbonyliron, [Fe(CO)4(HgSCN)2], was prepared from [Fe(CO) 5] and Hg(SCN)2, and studied by IR spectroscopy and X-ray diffraction. The compound crystallizes in the tetragonal space group I4,1/a. The unit cell, with dimensions of a = 13.778(3), c = 13.234(3) Å, V = 2512.3(9) Å3, contains four molecules. The iron atom is octahedrally coordinated by four carbonyl groups and two mercury atoms in cis positions. The coordination of the mercury atoms is distorted square-planar, since, besides mercury-iron and mercury-sulphur bonds, there are also mercury-mercury and mercury-nitrogen interactions. The FeHg distance is 2.506(5)Å and the HgFeHg angle is 78.0(1)°. © 1987.

Synthesis and solid-state structural characterization of di-μ-azido-bis[{azido(N, N-diethylethylenediamine)}copper(II)]

The 1:1 mixed-ligand [{Cu(N3)2(diEten)}2] (diEten=N,N-diethylethylenediamine) complex has been synthesized and characterized by i.r. spectroscopy and X-ray diffraction. The compound crystallizes in the triclinic space group P1. Its structure consists of a centrosymmetric Cu2N2 unit whose N atoms belong to end-on azido bridges. Each copper atom is also surrounded by three nitrogen atoms; two from one N, N-diethylethylenediamine, and one from the remaining azide. The five nitrogen atoms altogether occupy the vertices of a slightly distorted trigonal bipyramid, and the azidobridges produced a rather short Cu...Cu distance of 3.37 Å. © 1989 Chapman and Hall Ltd.

Structural characterization of a tin oxyhydroxide gel and its precursor sol

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Structural characterization of nuclear phenotypes during Scinax fuscovarius spermatogenesis (Anura, Hylidae)

In anuran amphibian Scinax fuscovarius, the spermatogenesis occurs in structures called seminiferous loculi, in which germ epithelium is organized in spermatocysts. Each cyst contains cells in the same stage of cytodifferentiation. Characteristics of each cellular type and their groups made the identification and differentiation of the germ lineage cells possible. In the basis of the epithelium there are the spermatogonia I, the biggest cells and always associated with the Sertoli cell. After the phase of mitotic proliferation, the cysts containing variable number of spermatogonia II are originated, quite smaller and with cellular boundaries a little distinct. After differentiation and growth in volume, the spermatocytes I appear, the nuclei of which are spherical and with different degrees of compaction of the nuclear material. Starting the meiotic process, the spermatocytes II are originated, which by means of the second meiotic division become haploid cells, the spermatids I. These two last spermatocysts are very similar. In this phase, the cells will go through a prominent process of differentiation until they form the spermatids II, which are elongated and begin to be organized in bundles supported by prominent Sertoli cells. With the process of spermiogenesis, spermatozoa appear, usually observed in compact bundles with tails turned to the lumen and their heads fitted in their support cells. In more advanced stages, the spermatozoa can be observed free in the locular lumen, ready to follow the spermatic path.

Microstructural characterization of layers produced by plasma nitriding on austenitic and superaustenitic stainless steel grades

High chromium content is responsible for the formation of a protective passive surface layer on austenitic stainless steels (ASS). Due to their larger amounts of chromium, superaustenitic stainless steels (SASS) can be chosen for applications with higher corrosion resistance requirements. However, both of them present low hardness and wear resistance that has limited their use for mechanical parts fabrication. Plasma nitriding is a very effective surface treatment for producing harder and wear resistant surface layers on these steel grades, without harming their corrosion resistance if low processing temperatures are employed. In this work UNS S31600 and UNS S31254 SASS samples were plasma nitrided in temperatures from 400 °C to 500 °C for 5 h with 80% H 2-20% N2 atmosphere at 600Pa. Nitrided layers were analyzed by optical (OM) and transmission electron microscopy (TEM), x-ray diffraction (XRD), and Vickers microhardness testing. Observations made by optical microscopy showed that N-rich layers were uniform but their thicknesses increased with higher nitriding temperatures. XRD analyses showed that lower temperature layers are mainly composed by expanded austenite, a metastable nitrogen supersaturated phase with excellent corrosion and tribological properties. Samples nitrided at 400 °C produced a 5 μm thick expanded austenite layer. The nitrided layer reached 25 lm in specimens treated at 500 °C. There are indications that other phases are formed during higher temperature nitriding but XRD analysis was not able to determine that phases are iron and/or chromium nitrides, which are responsible for increasing hardness from 850 up to 1100 HV. In fact, observations made by TEM have indicated that formation of fine nitrides, virtually not identified by XRD technique, can begin at lower temperatures and their growth is affected by both thermodynamical and kinetics reasons. Copyright © 2012 by ASTM International.