Toward an understanding of intermediate- and short-range defects in ZnO single crystals. A combined experimental and theoretical study

A joint use of experimental and theoretical techniques allows us to understand the key role of intermediate- and short-range defects in the structural and electronic properties of ZnO single crystals obtained by means of both conventional hydrothermal and microwave-hydrothermal synthesis methods. X-ray diffraction, Raman spectra, photoluminescence, scanning electronic and transmission electron microscopies were used to characterize the thermal properties, crystalline and optical features of the obtained nano and microwires ZnO structures. In addition, these properties were further investigated by means of two periodic models, crystalline and disordered ZnO wurtzite structure, and first principles calculations based on density functional theory at the B3LYP level. The theoretical results indicate that the key factor controlling the electronic behavior can be associated with a symmetry breaking process, creating localized electronic levels above the valence band.

Crystallization and preliminary diffraction data of BaP1, a haemorrhagic metalloproteinase from Bothrops asper snake venom

BaP1 is a metalloproteinase isolated from the venom of the Central American snake Bothrops asper (terciopelo). It is a 24 kDa protein consisting of a single chain which includes the metalloproteinase domain only, therefore being classified as a class P-I snake-venom metalloproteinase. BaP1 induces prominent local tissue damage, such as haemorrhage, myonecrosis, blistering, dermonecrosis and oedema. In order to elucidate its structure, BaP1 was crystallized by the hanging-drop vapour-diffusion technique in 0.1 M bicine pH 9.0, 10% PEG 20 000 and 2%(v/v) dioxane. Diffraction data were observed to a resolution of 2.7 Angstrom. Crystals belong to space group P2(1)2(1)2(1), with unit-cell parameters a = 38.22, b = 60.17, c = 86.09 Angstrom.

Crystallization and preliminary diffraction data of a platelet-aggregation inhibitor from the venom of Agkistrodon piscivorus piscivorus (North American water moccasin)

Applaggin (Agkistrodon piscivorus piscivorus platelet-aggregation inhibitor) is a potent inhibitor of blood platelet aggregation derived from the venom of the North American water moccasin, the protein consists of 71 amino acids, is rich in cysteines, contains the sequence-recognition site of adhesion proteins at positions 50-52 (Arg-Gly-Asp) and shares high sequence homology with other snake-venom disintegrins such as echistatin, kistrin and trigramin, Single crystals of applaggin have been grown and X-ray diffraction data have been collected to a resolution of 3.2 Angstrom. The crystals belong to space group P4(1)2(1)2 (or its enantiomorph), with unit-cell dimensions a = b = 63.35, c = 74.18 Angstrom and two molecules per asymmetric unit. Molecular replacement using models constructed from the NMR structures of echistatin and kistrin has not been successful in producing a trial structure for applaggin.

Laüe back-reflection method for crystallographic orientation of a martensitic Cu-Zn-Al single crystal of the monoclinic system

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

Development of metal - SiO2 nanocomposites in a single-step process by the polymerizable complex method

This work presents the synthesis and characterization of SiO2:metal (Ni, Co, Ag, and Fe) nanocomposites processed by the polymerizable complex method. The polymeric precursor solutions obtained were characterized by means of FT-Raman and C-13 NMR spectroscopy. The results show the formation of a hybrid polymer with carbon and silicon in the macromolecule chain and the transition metal cation arrested within this polymeric chain. The nanocomposites are formed during the controlled polymeric precursor pyrolysis. The reduction of the metal cation is promoted by the CO/CO2 atmosphere resulting from the pyrolysis of the organic material. Microstructural characterization, performed by TEM and X-ray diffraction (XRD), showed that the nanocomposites are formed by metal nanoparticles embedded in a amorphous matrix formed by SiO2 and carbon. In the SiO2:Fe system, Fe3C was also detected by XRD.

Grazing incidence X-ray diffraction and atomic force microscopy analysis of BaBi2Ta2O9 thin films

Thin films of BaBi2Ta2O9 (BBT) composition were prepared through the metal organic decomposition method. The crystallinity, phase formation, crystallite size and morphology of the thin films were measured as a function of the type of substrate, stoichiometry of solution and process variables such as thickness and temperature. The thin films were investigated by grazing incidence X-ray diffractometry and atomic force microscopy (AFM) techniques. For the sample without excess of bismuth, diffraction peaks other than that of the BBT phase were observed. A well crystallized BBT single phase was observed for films prepared from a solution with 10% excess of bismuth, deposited on Si/Pt substrate, with a thickness up to 150 nm and sintered at temperatures of 700 degreesC. The thin BBT phase films heat-treated at 600 degreesC presented a diffraction pattern characteristic of samples with lower degree of crystallinity whereas for the thin films heat-treated at 800 degreesC, we observed the presence of other phases than the BBT. For the thin film deposited on the Sin+ substrate, we observe that the peaks corresponding to the BBT phase are broader than that observed on the samples deposited on the Pt and Si/Pt substrates. No variation of average crystallite size was observed as the excess of Bi increased from 10 to 20%. AFM images for the samples showed that the increasing the amount of bismuth promotes grain growth. The average surface roughness measured was in the range of 16-22 nm showing that the bismuth amount had no or little effect on the roughness of films. (C) 2002 Elsevier B.V. B.V. All rights reserved.

DIFFRACTION AND THE GLUON MASS

We recently proposed a QCD Pomeron described by the exchange of two nonperturbative gluons characterized by a dynamically generated gluon mass. It is shown here that data on elastic scattering, exclusive rho production in deep inelastic scattering, and the J/psi-nucleon total cross section can be successfully described in terms of a single gluon mass m(g) congruent-to 0.37 GeV. We observe that the total cross sections of hadrons with small radii, such as J/psi, have a marked dependence on the effective gluon mass.

Crystallization and preliminary X-ray diffraction analysis of a novel Arg49 phospholipase A(2) homologue from Zhaoermia mangshanensis venom

Zhaoermiatoxin, an Arg49 phospholipase A(2) homologue from Zhaoermia mangshanensis (formerly Trimeresurus mangshanensis, Ermia mangshanensis) venom is a novel member of the PLA(2)-homologue family that possesses an arginine residue at position 49, probably arising from a secondary Lys49 -> Arg substitution that does not alter the catalytic inactivity towards phospholipids. Like other Lys49 PLA(2) homologues, zhaoermiatoxin induces oedema and strong myonecrosis without detectable PLA(2) catalytic activity. A single crystal with maximum dimensions of 0.2 x 0.2 x 0.5 mm was used for X-ray diffraction data collection to a resolution of 2.05 angstrom using synchrotron radiation and the diffraction pattern was indexed in the hexagonal space group P6(4), with unit-cell parameters a = 72.9, b = 72.9, c = 93.9 angstrom.

Structural, microstructural, and transport properties of highly oriented LaNiO3 thin films deposited on SrTiO3(100) single crystal

Electrical conductive textured LaNiO3/SrTiO3 (100) thin films were successfully produced by the polymeric precursor method. A comparison between features of these films of LaNiO3 (LNO) when heat treated in a conventional furnace (CF) and in a domestic microwave (MW) oven is presented. The x-ray diffraction data indicated good crystallinity and a structural orientation along the (h00) direction for both films. The surface images obtained by atomic force microscopy revealed similar roughness values, whereas films LNO-MW present slightly smaller average grain size (similar to 80 nm) than those observed for LNO-CF (60-150 nm). These grain size values were in good agreement with those evaluated from the x-ray data. The transport properties have been studied by temperature dependence of the electrical resistivity rho(T) which revealed for both films a metallic behavior in the entire temperature range studied. The behavior of rho(T) was investigated, allowing to a discussion of the transport mechanisms in these films. (C) 2007 American Institute of Physics.

Low-temperature synthesis of single-phase Co7Sb2O12

Polycrystalline Co7Sb2O12 compounds have been synthesized by a chemical route, which is based on a modified polymeric precursor method. In order to study the physical properties of the samples, X-ray diffraction (XRD), thermal analyses (TG and DSC), infrared spectroscopy (IR), specific surface area (BET), and magnetization measurements were performed on these materials. Characterization through XRD revealed that the samples are single-phase after a heat-treatment at 1100degreesC for 2h, while the X-ray patterns of the samples heat-treated at lower temperatures revealed the presence of additional Bragg reflections belonging to the Co6Sb2O6 phase. These data were analyzed by means of Rietveld refinement and further analyze showed that Co7Sb2O12 displays an inverse spinel crystalline structure. In this structure, the Co2+ ions occupy the eight tetrahedral positions, and the sixteen octahedral positions are randomly occupied by the Sb5+ and Co2+ ions. IR studies disclosed two strong absorption bands, v(1) and v(2), in the expected spectral range for a spinel-type binary oxide with space group Fd3m. Exploratory studies concerning the magnetic properties indicated that this sample presents a spin-glass transition at T-f similar to 64 K. (C) 2004 Elsevier B.V. All rights reserved.

Differential scanning calorimetry, x-ray diffraction and F-19 nuclear magnetic resonance investigations of the crystallization of InF3-based glasses

Results of differential scanning calometry (DSC), x-ray diffraction (XRD), and F-19 nuclear magnetic resonance (NMR) of InF3-based glasses, treated at different temperatures, ranging from glass transition temperature (T-g) to crystallization temperature (T-c), are reported. The main features of the experimental results are as follows. DSC analysis emphasizes several steps in the crystallization process. Heat treatment at temperatures above T-g enhances the nucleation of the first growing phases but has little influence on the following ones. XRD results show that several crystalline phases are formed, with solid state transitions when heated above 680 K, the F-19 NMR results show that the spin-lattice relaxation, for the glass samples heat treated above 638 K, is described by two time constants. For samples treated below this temperature a single time constant T-1 was observed. Measurements of the F-19 spin-lattice relaxation time (T-1), as a function of temperature,made possible the identification of the mobile fluoride ions. The activation energy, for the ionic motion, in samples treated at crystallization temperature was found to be 0.18 +/- 0.01 eV. (C) 1998 American Institute of Physics.

Purification, Characterization, and Preliminary X-Ray Diffraction Analysis of a Lactose-Specific Lectin from Cymbosema roseum Seeds

The unique carbohydrate-binding property of lectins makes them invaluable tools in biomedical research. Here, we report the purification, partial primary structure, carbohydrate affinity characterization, crystallization, and preliminary X-ray diffraction analysis of a lactose-specific lectin from Cymbosema roseum seeds (CRLII). Isolation and purification of CRLII was performed by a single step using a Sepharose-4B-lactose affinity chromatography column. The carbohydrate affinity characterization was carried using assays for hemagglutination activity and inhibition. CRLII showed hemagglutinating activity toward rabbit erythrocytes. O-glycoproteins from mucine mucopolysaccharides showed the most potent inhibition capacity at a minimum concentration of 1.2 A mu g mL(-1). Protein sequencing by mass spectrometry was obtained by the digestion of CRLII with trypsin, Glu-C, and AspN. CRLII partial protein sequence exhibits 46% similarity with the ConA-like alpha chain precursor. Suitable protein crystals were obtained with the hanging-drop vapor-diffusion method with 8% ethylene glycol, 0.1 M Tris-HCl pH 8.5, and 11% PEG 8,000. The monoclinic crystals belong to space group P2(1) with unit cell parameters a = 49.4, b = 89.6, and c = 100.8 A....

Signal and backgrounds for the single production of scalar and vector leptoquarks at the CERN LHC

We perform a detailed analysis of the potentiality of the CERN Large Hadron Collider to study the single production of leptoquarks via pp→e±q→ leptoquark →e± q, with e± generated by the splitting of photons radiated by the protons. Working with the most general SU(2)L⊗U( 1 )Y invariant effective Lagrangian for scalar and vector leptoquarks, we analyze in detail the leptoquark signals and backgrounds that lead to a final state containing an e± and a hard jet with approximately balanced transverse momenta. Our results indicate that the LHC will be able to discover leptoquarks with masses up to 2-3 TeV, depending on their type, for Yukawa couplings of the order of the electromagnetic one.

Influence of Nd:YAG Laser on the Bond Strength of Self-etching and Conventional Adhesive Systems to Dental Hard Tissues

Purpose: The aim of this study was to investigate the influence of Nd:YAG laser on the shear bond strength to enamel and dentin of total and self-etch adhesives when the laser was applied over the adhesives, before they were photopolymerized, in an attempt to create a new bonding layer by dentin-adhesive melting.Material and Methods: One-hundred twenty bovine incisors were ground to obtain flat surfaces. Specimens were divided into two substrate groups (n=60): substrate E (enamel) and substrate D (dentin). Each substrate group was subdivided into four groups (n=15), according to the surface treatment accomplished: X (Xeno III self-etching adhesive, control), XL (Xeno III + laser Nd:YAG irradiation at 140 mJ/10 Hz for 60 seconds + photopolymerization, experimental), S (acid etching + Single Bond conventional adhesive, Control), and SL (acid etching + Single Bond + laser Nd:YAG at 140 mJ/10 Hz for 60 seconds + photopolymerization, experimental). The bonding area was delimited with 3-mm-diameter adhesive tape for the bonding procedures. Cylinders of composite were fabricated on the bonding area using a Teflon matrix. The teeth were stored in water at 37 degrees C/48 h and submitted to shear testing at a crosshead speed of 0.5 mm/min in a universal testing machine. Results were analyzed with three-way analysis of variance (ANOVA; substrate, adhesive, and treatment) and Tukey tests (alpha=0.05). ANOVA revealed significant differences for the substrate, adhesive system, and type of treatment: lased or unlased (p<0.05). The mean shear bond strength values (MPa) for the enamel groups were X=20.2 +/- 5.61, XL=23.6 +/- 4.92, S=20.8 +/- 4.55, SL=22.1 +/- 5.14 and for the dentin groups were X=14.1 +/- 7.51, XL=22.2 +/- 6.45, S=11.2 +/- 5.77, SL=15.9 +/- 3.61. For dentin, Xeno III self-etch adhesive showed significantly higher shear bond strength compared with Single Bond total-etch adhesive; Nd:YAG laser irradiation showed significantly higher shear bond strength compared with control (unlased).Conclusion: Nd:YAG laser application prior to photopolymerization of adhesive systems significantly increased the bond strength to dentin.

Hard X-ray photoemission study of the Fabre salts (TMTTF)(2)X (X = SbF6 and PF6)

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