121 resultados para Powder morphology

em Indian Institute of Science - Bangalore - Índia


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A new series of substituted perovskites of the type LaCr1−xMxO3−δ, where M=Cu or Mg have been synthesised by the citrate gel process and characterized by means of powder X-ray diffraction, infrared spectroscopy, selected area diffraction and also by electron paramagnetic resonance spectroscopy. The general powder morphology was also observed using scanning electron microscopy. 40 mole percent substitution of Cr3+ by Cu2+ or Mg2+ have shown to result in single phase perovskite structure. Beyond x=0.5, a new phase has been identified in a narrow compositional range. Effect of Cu and Mg substitution on the sinterability of pure LaCrO3 has also been studied. It is possible to get near theoretically dense materials at a temperature as low as 1200°C in air by copper substitution.

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α-Manganese dioxide is synthesized in a microemulsion medium by a redox reaction between KMnO4 and MnSO4 in presence of sodium dodecyl sulphate as a surface active agent. The morphology of MnO2 resembles nanopetals, which are spread parallel to the field. The material is further characterized by powder X-ray diffraction, energy dispersive analysis of X-ray, and Brunauer–Emmett–Teller surface area. Supercapacitance property of α-MnO2 nanopetals is studied by cyclic voltammetry and galvanostatic charge–discharge cycling. High values of specific capacitance are obtained.

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Efficient ZnO:Eu3+ (1-11 mol%) nanophosphors were prepared for the first time by green synthesis route using Euphorbia tirucalli plant latex. The final products were well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), etc. The average particle size of ZnO:Eu3+ (7 mol%) was found to be in the range 27-47 nm. With increase of plant latex, the particle size was reduced and porous structure was converted to spherical shaped particles. Photoluminescence (PL) spectra indicated that the peaks situated at similar to 590, 615, 648 and 702 nm were attributed to the D-5(0) -> F-7(j(j=1,2,3,4)) transitions of Eu3+ ions. The highest PL intensity was recorded for 7 mol% with Eu3+ ions and 26 ml plant latex concentration. The PL intensity increases with increase of plant latex concentration up to 30 ml and there after it decreases. The phosphor prepared by this method show spherical shaped particles, excellent chromaticity co-ordinates in the white light region which was highly useful for WLED's. Further, present method was reliable, environmentally friendly and alternative to economical routes. (c) 2013 Elsevier B.V. All rights reserved.

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Here we present digestive ripening facilitated interatomic diffusion for the phase controlled synthesis of homogeneous intermetallic nanocrystals of Au-Sn system. Au and Sn metal nanoparticles synthesized by a solvated metal atom dispersion (SMAD) method are employed as precursors for the fabrication of AuSn and Au5Sn which are Au-rich Au-Sn intermetallic nanocrystals. By optimizing the stoichiometry of Au and Sn in the reaction mixture, and by employing growth directing agents, the formation of phase pure intermetallic AuSn and Au5Sn nanocrystals could be realized. The as-prepared Au and Sn colloidal nanoparticles and the resulting intermetallic nanocrystals are thoroughly characterized by powder X-ray diffraction, transmission electron microscopy (TEM and STEM-EDS), and optical spectroscopy. The results obtained here demonstrate the potential of solution chemistry which allows synthesizing phase pure Au-Sn intermetallics with tailored morphology.

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The formation of the helical morphology in monolayers and bilayers of chiral amphiphilic assemblies is believed to be driven at least partly by the interactions at the chiral centers of the amphiphiles. However, a detailed microscopic understanding of these interactions and their relation with the helix formation is still not clear. In this article a study of the molecular origin of the chirality-driven helix formation is presented by calculating, for the first time, the effective pair potential between a pair of chiral molecules. This effective potential depends on the relative sizes of the groups attached to the two chiral centers, on the orientation of the amphiphile molecules, and also on the distance between them. We find that for the mirror-image isomers (in the racemic modification) the minimum energy conformation is a nearly parallel alignment of the molecules. On the other hand, the same for a pair of molecules of one kind of enantiomer favors a tilt angle between them, thus leading to the formation of a helical morphology of the aggregate. The tilt angle is determined by the size of the groups attached to the chiral centers of the pair of molecules considered and in many cases predicted it to be close to 45 degrees. The present study, therefore, provides a molecular origin of the intrinsic bending force, suggested by Helfrich (J. Chem. Phys. 1986, 85, 1085-1087), to be responsible for the formation of helical structure. This effective potential may explain many of the existing experimental results, such as the size and the concentration dependence of the formation of helical morphology. It is further found that the elastic forces can significantly modify the pitch predicted by the chiral interactions alone and that the modified real pitch is close to the experimentally observed value. The present study is expected to provide a starting point for future microscopic studies.

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We report the growth of one-dimensional ZnO nanostructures with different morphologies such as nanoneedles, nanorods, nanobelts from Zn powder/granule. The growth process is different from the conventional vapor-solid mechanism. The advantage of this method is that neither a catalyst nor any gas flow is required for the synthesis of nanostructures. Depending upon the Zn powder or Zn granules as the starting material different nanostructures have been synthesized which demonstrates the versatility of the technique.

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A series of dual-phase (DP) steels containing finely dispersed martensite with different volume fractions of martensite (V-m) were produced by intermediate quenching of a boron- and vanadium-containing microalloyed steel. The volume fraction of martensite was varied from 0.3 to 0.8 by changing the intercritical annealing temperature. The tensile and impact properties of these steels were studied and compared to those of step-quenched steels, which showed banded microstructures. The experimental results show that DP steels with finely dispersed microstructures have excellent mechanical properties, including high impact toughness values, with an optimum in properties obtained at similar to 0.55 V-m. A further increase in V-m was found to decrease the yield and tensile strengths as well as the impact properties. It was shown that models developed on the basis of a rule of mixtures are inadequate in capturing the tensile properties of DP steels with V-m > 0.55. Jaoul-Crussard analyses of the work-hardening behavior of the high-martensite volume fraction DP steels show three distinct stages of plastic deformation.

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Electrochemical capacity retention of nearly X-ray amorphous nanostructured manganese oxide (nanoMnO2) synthesized by mixing directly KMnO4 with ethylene glycol under ambient conditions for supercapacitor studies is enhanced significantly. Although X-ray diffraction (XRD) pattern of nanoMnO2 shows poor crystallinity, it is found that by Mn K-edge X-ray absorption near edge structure (XANES) measurement that the nanoMnO2 obtained is locally arranged in a δ-MnO2-type layered structure composed of edge-shared network of MnO6 octahedra. Field emission scanning electron microscopy and XANES measurements show that nanoMnO2 contains nearly spherical shaped morphology with δ-MnO2 structure, and 1D nanorods of α-MnO2 type structure (powder XRD) in the annealed (600 °C) sample. Volumetric nitrogen adsorption−desorption isotherms, inductively coupled plasma analysis, and thermal analysis are carried out to obtain physicochemical properties such as surface area (230 m2 g−1), porosity of nanoMnO2 (secondary mesopores of diameter 14.5 nm), water content, composition, etc., which lead to the promising electrochemical properties as an electrode for supercapacitor. The nanoMnO2 shows a very high stability even after 1200 cycles with capacity retention of about 250 F g−1.

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Carbon-supported Pt-TiO2 (Pt-TiO2/C) catalysts with varying at. wt ratios of Pt to Ti, namely, 1:1, 2:1, and 3:1, are prepared by the sol-gel method. The electrocatalytic activity of the catalysts toward oxygen reduction reaction (ORR), both in the presence and absence of methanol, is evaluated for application in direct methanol fuel cells (DMFCs). The optimum at. wt ratio of Pt to Ti in Pt-TiO2/C is established by fuel cell polarization, linear sweep voltammetry, and cyclic voltammetry studies. Pt-TiO2/C heattreated at 750 degrees C with Pt and Ti in an at. wt ratio of 2:1 shows enhanced methanol tolerance, while maintaining high catalytic activity toward ORR. The DMFC with a Pt-TiO2/C cathode catalyst exhibits an enhanced peak power density of 180 mW/cm(2) in contrast to the 80 mW/cm(2) achieved from the DMFC with carbon-supported Pt catalyst while operating under identical conditions. Complementary data on the influence of TiO2 on the crystallinity of Pt, surface morphology, and particle size, surface oxidation states of individual constituents, and bulk and surface compositions are also obtained by powder X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, energy dispersive analysis by X-ray, and inductively coupled plasm optical emission spectrometry.

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Nanoparticles of trivalent Eu3+-doped Nd2O3 phosphors have been prepared using a low-temperature solution combustion method with metal nitrate as precursor and oxalyldihydrazide as a fuel at a fairly low temperature (<500 degrees C) and in a very short time (<5 min). A powder X-ray diffraction pattern reveals that cubic Nd2O3 : Eu3+ crystallites are directly obtained without the requirement of further calcinations. The crystallite size, evaluated from Scherer's formula, was found to be in the range of 20-30 nm. The microstructure and morphology were studied by scanning electron microscopy, which showed the phosphor to be foamy and fluffy in nature. Thermoluminescence characteristics of the Nd2O3 : Eu3+ have been studied using gamma irradiation. These demonstrate that the phosphor is suitable for use as a dosimeter.

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Sr2SbMnO6 (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li2SO4-0.365 Na2SO4 (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 degrees C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with similar to 60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95 +/- 5 kJ mol(-1). The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties.

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Microstructure and microtexture evolution during static annealing of a hot-extruded AZ21 magnesium alloy was studied. Apart from fine recrystallized equiaxed grains and large elongated deformed grains, a new third kind of abnormal grains that are stacked one after the other in a row parallel to the extrusion direction were observed. The crystallographic misorientation inside these grains was similar to that of the fine recrystallized grains. The large elongated grains exhibited significant in-grain misorientation. A self-consistent mechanistic model was developed to describe the formation of these grain morphologies during dynamic recrystallization (DRX). The texture of pre-extruded material, although lost in DRX, leaves a unique signature which manifests itself in the form of these grain morphologies. The origin of abnormal stacked grains was associated with slow nucleation in pre-extruded grains of a certain orientation. Further annealing resulted in large secondary recrystallized grains with occasional extension twins. (c) 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

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Nanostructured MnO2 was synthesized at ambient condition by reduction of potassium permanganate with aniline. Powder X-ray diffraction, thermal analysis (thermogravimetric and differential thermal analysis), Brunauer-Emmett-Teller surface area, and infrared spectroscopy studies were carried out for physical and chemical characterization. The as-prepared MnO2 was amorphous and contained particles of 5-10 nm diameter. Upon annealing at temperatures >400°C, the amorphous MnO2 attained crystalline α-phase with a concomitant change in morphology. A gradual conversion of nanoparticles to nanorods is evident from scanning electron microscopy and transmission electron microscopy (TEM) studies. High-resolution TEM images suggested that nanoparticles and nanorods grow in different crystallographic planes. Capacitance behavior was studied by cyclic voltammetry and galvanostatic charge-discharge cycling in a potential range from -0.2 to 1.0 V vs SCE in 0.1 M sodium sulfate solution. Specific capacitance of about 250 F g-1 was obtained at a current density of 0.5 mA cm-2(0.8 A g-1).

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The enzyme UDP-galactose-4-epimerase (GAL10) catalyzes a key step in galactose metabolism converting UDP-galactose to UDPglucose which then can get metabolized through glycolysis and TCA cycle thus allowing the cell to use galactose as a carbon and energy source. As in many fungi, a functional homolog of GAL10 exists in Candida albicans. The domainal organization of the homologs from Saccharomyces cerevisiae and C albicans show high degree of homology having both mutarotase and an epimerase domain. The former is responsible for the conversion of beta-D-galactose to alpha-D-galactose and the hitter for epimerization of UDP-galactose to UDP-glucose. Absence of C albicans GAL10 (CaGAL10) affects cell-wall organization, oxidative stress response, biofilm formation and filamentation. Cagal10 mutant cells tend to flocculate extensively as compared to the wild-type cells. The excessive filamentation in this mutant is reflected in its irregular and wrinkled colony morphology. Cagal10 strain is more susceptible to oxidative stress when tested in presence of H2O2. While the S. cerevsiae GAL10 (ScGAL10), essential for survival in the presence of galactose, has not been reported to have defects in the absence of galactose, the C albicans homolog shows these phenotypes during growth in the absence of galactose. Thus a functional CaGal10 is required not only for galactose metabolism but also for normal hyphal morphogenesis, colony morphology, maintenance of cell-wall integrity and for resistance to oxidative stress even in the absence of galactose. (c) 2006 Elsevier Inc. All rights reserved.

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The ignition behaviour of boron powder, prepared through electrowinning process, was studied by using thermogravimetry coupled with simultaneous differential thermal analysis (TG-SDTA). The dependence of the inception of the ignition reaction on the partial pressure of oxygen, particle size of the boron powder and heating rate was investigated. It was observed that all these factors affect the ignition temperature. Boron powder with a mean particle size of about 10 mu m was found to be susceptible to ignition in oxygen even at 783K. In general, the susceptibility to ignition was found to vary inversely with the degree of crystallinity. Presence of carbon was found to retard the oxidation of boron and raise the ignition temperature. These results are useful in safe handling and storage of finely divided boron powder and in the subsequent production of boron carbide from it. (C) 2009 Elsevier B.V. All rights reserved.