913 resultados para all-solid-state


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High amylose was cross-linked with sodium trimetaphosphate (STMP) using 2% and 4% solutions of NaOH at room temperature with reaction contact times of 0.5, 1, 2 and 4 h. The different polymers obtained were analyzed by FT IR, C-13 and P-31 solid state NMR, SEM and C, H and P elemental analysis. The results were used to propose a two-stage mechanism for phosphate incorporation, the first being kinetically controlled. (C) 2008 Elsevier Ltd. All rights reserved.

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We present the structural, electronic structure and magnetic studies of Ni doped SmFeO3. The X-ray diffraction (XRD) studies confirm the single phase nature of the samples having orthorhombic Pbnm structure and the unit-cell volume is decreasing with the increase of Ni concentration. X-ray absorption spectroscopy (XAS) studies on O K. Fe L-3.2, Ni L-3.2 and Sm M-5.4 edges of SmFe1-xNixO3 (x <= 0.5) samples along with the reference compounds revealed the homo-valence state of Fe and Ni in these materials. From magnetization studies it has been observed the materials exhibit ferromagnetic and anti-ferromagnetic sub-lattices, which are strongly dependent on the thermo-magnetic state of the system. (C) 2010 Elsevier B.V. All rights reserved.

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

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Foram sintetizados compostos Ln-L no estado sólido, onde Ln significa os lantanídeos leves trivalentes e L é o piruvato. Estes compostos foram caracterizados e estudados utilizando-se a Termogravimetria e Termogravimetria derivada (TG/DTG), calorimetria exploratória diferencial (DSC) difratometria de raios X pelo método do pó, espectroscopia na região do infravermelho, análise elementar e complexometria. Os resultados permitiram obter informações com respeito a composição, desidratação, sitio de coordenação, comportamento térmico e a decomposição térmica destes compotos.

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Solid-state compounds of general formula Ln(2)L(3)center dot nH(2)O, where L represents 1,4-bis(3-carboxy-3-oxo-prop-1-enyl)benzene and Ln = La, Ce, Pr, Nd, Sm, were synthesized. Complexometric titrations with EDTA, thermogravimetry (TG), differential thermal analysis (DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, elemental analysis and infrared spectroscopy have been employed to characterize and to study the thermal behavior of these compounds in dynamic air atmosphere. The results led to information about the composition, dehydration, crystallinity, and thermal decomposition of the synthesized compounds.

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This work was performed to verify the chemical structure, mechanical and hydrophilic properties of amorphous hydrogenated carbon films prepared by plasma enhanced chemical vapor deposition, using acetylene/argon mixture as monomer. Films were prepared in a cylindrical quartz reactor, fed by 13.56 MHz radiofrequency. The films were grown during 5 min, for power varying from 25 to 125 W at a fixed pressure of 9.5 Pa. After deposition, all samples were treated by SF(6) plasma with the aim of changing their hydrophilic character. Film chemical structure investigated by Raman spectroscopy, revealed the increase of sp(3) hybridized carbon bonds as the plasma power increases. Hardness measurements performed by the nanoindentation technique showed an improvement from 5 GPa to 14 GPa following the increase discharge power. The untreated films presented a hydrophilic character, which slightly diminished after SF(6) plasma treatment.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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A method for the attachment of 2-mercaptothiazoline (MTZ) to modified silica gel has been developed. In the first step, a new silylant agent was synthesized, named SiMTZ, by the reaction between MTZ molecule and chloropropyltrimethoxysilane (SiCl). SiMTZ and tetraethylortosilicate were co-condensed in the presence of n-dodecylamine, a neutral surfactant template, to produce a modified ordered hexagonal mesoporous silica named HMTZ. The modified material contained 0.89 +/- 0.03 mmol of 2-mercaptothiazoline per gram of silica. FT-IR, FT-Raman, Si-29- and C-13-NMR spectra were in agreement with the proposed structure of the modified mesoporous silica in the solid state. HMTZ material has been used for divalent mercury adsorption from aqueous solution at 298 I K. The series of adsorption isotherms were adjusted to a modified Langmuir equation. The maximum number of moles of mercury adsorbed gave 2.34 +/- 0.09 mmol/g of material. The same interaction was followed by calorimetric titration on an isoperibol calorimeter. The HMTZ presented a high capacity for the removal of the contaminant mercury from water. The Delta H and Delta G values for the interaction were determined to be -56.34 +/- 1.07 and -2.14 +/- 0.11 kJ mol(-1). This interaction process was accompanied by a decrease of entropy value (- 182 J mol(-1) K-1). Thus, the interaction between mercury and HMTZ resulted in a spontaneous thermodynamic system with a high favorable exothermic enthalpic effect. (c) 2007 Elsevier B.V. All rights reserved.

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This dissertation describes the igneous suites of the Japi granitoid pluton, intrusive in the Paleoproterozoic gneiss-migmatite complex of the eastern domain of the Seridó Belt, northeastern Brazil. Field relations show that the pluton is affected by strong deformation associated to the Brasiliano orogeny (known as the D3 phase) , with a NW-trending extensionalleft-hand senestral shear zone (the Japi Shear Zone, JSZ) bordering the intrusive body to the west. Four plutonic suites are found in the main pluton and as satellyte intrusions, besides Iate pegmatite and pink leucogranites. An alkaline granitoid suite, dominated by syenogranites bearing sodic augite (and subordinate hornblende), define a main elliptical intrusion. In its northern part, this intrusion is made up by concentric sheets, contrasting with a smaller rounded stock to the south. These granites display a pervasive solid-state S>L fabric developed under high T conditions, characterized by plastic deformation of quartz and feldspar. It is especially, developed along the border of the pluton, with inward dips. A regular magmatic layering is present sometimes, parallel to the tectonic foliation. The syntectonic emplacement as regards to the Brasiliano (D3) event is indicated by the common occurrence of dykes and sheets along transtensional or extensional sites of the major structure. Field relations attest to the early emplacement of the alkaline granites as regards to the other suites. A basic-to-intermediate suite occurs as a western satellyte body and occupying the southern tail of the main alkaline pluton. It comprises a wide variety of compositional terms, including primitive gabbros and gabbro-norites, differentiated to monzonitic intermediate facies containing amphibole and biotite as their main mafic phases. These rocks display transitional high-K calc-alkaline to shoshonitic affinities. Porphyritic monzogranite suítes commonly occur as dykes and minor intrusives, isolated or associated with the basic-tointermediate rocks. In the latter case, magma mingling and mixing features attest that these are contemporaneous igneous suites. These granites show K-feldspar phenocrysts and a hornblende+biotite+titanite assemblage, displaying subalkaline/monzonitic geochemical affinities. Both suites exhibit SL magmatic fabrics overprinting or transitional to solid-state D3 deformation related to the JSI. Chemical data clearly show that they are related to different parental magmas. Finally, a microgranite suite occurs along a few topographic ridges paralell to the JSI. It comprises dominantly granodiorites with a mineralogy similar to the one of the porphyritic granitoids. However, discriminant diagrams show their distinct calc-alkaline affinity. The granodiorites display an essencially magmatic fabric, even though an incipient D3 solid-state structure may be developed along the JSI. Intrusion relationships with the previous suites, as well as regards to the D3 structures, point to their Iate emplacement. All these suites are intrusive in a Paleoproterozoic, high-grade gneiss-migmatite complex affected by two previous deformation phases (D1, D2). The fabrics associated with these earlier events are folded and overprinted by the younger D3 structures along the JSZ. The younger deformation is characterized by NE-dipping foliations and N/NE-plunging stretching lineations. In the JSZ northern termination the foliation acquires an ENE orientation, containing a stretching lineation plunging to the south. Symmetric kinematic cri teria developed at this site confirms the transpressional termination of the JSZ, as also shown by orthorrombic quartz c-axis patterns. E-W-trending d extra I shear zones developed in the central part of the JSZ are interpreted as antithetic structures associated to the transtensional deformation along the JSZ. This is consistent with its extensional-transcurrent kinematics and a flat-and-ramp geometry at depth, as shown by gravimetric data. The lateral displacement of the negative residual Bouguer anomalies, as regards to the main outcropping alkaline pluton, may be modelized by other deeper-seated granite bodies. Based on numerical modelling it was possible to infer two distinct intrusion styles for the alkaline pluton. The calculated model values are consistent with an emplacement by sheeting for the northern body, as already suggested by satellyte imagery and field mapping. On the other hand, the results point to a transition towards a diapir-related style associated to the smaller. southern stock. This difference in intrusion styles may relate to intensity variations and transtensional sites of the shear deformation along the JSZ. Trace element and Sr and Nd isotopes of the alkaline granites are compatible with their derivation trom a more basic crustal source, as compared to the presently outcropping highgrade gneisses, with participation (or alternatively dominated by) of an enriched lithospheric mantle component. Like other igneous suites in the Seridó Belt, the high LlL contents and fractionated REE patterns of the basic rocks also point to an enriched mantle as the source for this kind of magmatism. Geochemical and isotope data are compatible with a lower crustal origin for the porphyritic granites. On the basis of the strong control of the JSZ on the emplacement of lower crustal (porphyritic and alkaline granites) or lithospheric mantle (basic rocks, alkaline granites or a component of them) magmas, one may infer a deep root for this structure, bearing an important role in magma extraction, transport and emplacement in the Japi region, eastern domain of the Seridó Belt