176 resultados para SIZE-CONTROLLED SYNTHESIS


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ZnAl2O4:Dy3+ (1-9 mol%) nanophosphors were synthesized by a simple, cost effective and environmental friendly route using Euphorbia tirucalli plant latex. The structural properties and morphological features of the phosphors were well studied by PXRD, FTIR, SEM and TEM measurements. The luminescent properties of ZnAl2O4:Dy3+ (1-9 mol%) nanophosphors were investigated from the excitation and emission spectra. The phosphor performance was evaluated by color co-ordinates. The values were well located in the near white region as a result it was highly useful for the fabrication of green component in WLEDs. The average particle size was found to be similar to 9-18 nm and same was confirmed by TEM and Scherrer's method. The highest photoluminescence (PL) and thermoluminescence (TL) intensity was obtained to be similar to 7 mol% Dy3+ concentration. A single TL glow peak was recorded at 172 degrees C at a warming rate of 2.5 degrees Cs (1). The intensity at 172 degrees C peak increases linearly up to 1 kGy and after that it diminishes. PL intensity was studied with different plant latex concentration (2-8 ml) and highest PL intensity was recorded for similar to 8 ml. The optimized phosphor showed good reusability, low fading and wide range of linearity with gamma-dose hence the phosphor was quite useful in radiation dosimetry. (C) 2013 Elsevier B.V. All rights reserved.

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In the present work, Co1-xMnxFe2O4 nanoparticles were synthesized by the low-temperature auto-combustion method. The thermal decomposition process was investigated by means of differential and thermal gravimetric analysis (TG-DTA) that showed the precursor yield the final product above 450 degrees C. The phase purity and crystal lattice symmetry were estimated from X-ray diffraction (XRD). Microstructural features observed by scanning electron microscopy (SEM) demonstrates that the fine clustered particles were formed with an increase in average grain size with Mn2+ content. Fourier transform infrared spectroscopy (FTIR) study confirms the formation of spinel ferrite. Room temperature magnetization measurements showed that the magnetization M-s increases from 29 to 60 emu/g and H-c increases from 13 to 28 Oe with increase in Mn2+ content, which implies that these materials may be applicable for magnetic data storage and recording media. (C) 2013 Elsevier B.V. All rights reserved.

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Pure cubic zirconia (ZrO2) nanopowder is prepared for the first time by simple low temperature solution combustion method without calcination. The product is characterized by Powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Fourier Transform Infra Red spectroscopy (FTIR) and Ultraviolet-Visible spectroscopy (UV-Vis). The PXRD showed the formation of pure stable cubic ZrO2 nanopowders with average crystallite size ranging from 6 to 12 nm. The lattice parameters were calculated from Rietveld refinement method. SEM micrograph shows fluffy, mesoporous, agglomerated particles with large number of voids. TEM micrograph shows honey comb like arrangement of particles with particle size similar to 10 nm. The PL emission spectrum excited at 210 nm and 240 nm consists of intense bands centered at similar to 365 and similar to 390 nm. Both the samples show shoulder peak at 420 nm, along with four weak emission bands at similar to 484, similar to 528, similar to 614 and similar to 726 nm. TL studies were carried out pre-irradiating samples with gamma-rays ranging from 1 to 5 KGy at room temperature. A well resolved glow peak at 377 degrees C is recorded which can be ascribed to deep traps. With increase in gamma radiation there is linear increase in TL intensity which shows the possible use of ZrO2 as dosimetric material. (C) 2013 Elsevier B.V. All rights reserved.

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The Cobalt ferrite (CoFe2O4) powders were synthesized by Co-precipitation method. The as prepared ferrite powders were incorporated into a polyaniline matrix at various volumetric ratios. The as prepared composites of ferrite and polyaniline powders were characterized using X-ray diffraction (XRD), transmission electron microscope (TEM). The particle size of CoFe2O4 is found to be 20 nm. The saturation magnetization (M-s) of all the composites was found to be decreasing with decrease of ferrite content, while coercivity (H-c) remained at the value corresponding to pure cobalt ferrite nanopowders. The complex permittivity (epsilon' and epsilon `') and permeability (mu' and mu `') of composite samples were measured in the range of 1 MHz to 1.1 GHz. The value of epsilon' and mu' found to be increased with ferrite volume concentration.

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Cobalt ferrite (CoFe2O4) is an engineering material which is used for applications such as magnetic cores, magnetic switches, hyperthermia based tumor treatment, and as contrast agents for magnetic resonance imaging. Utility of ferrites nanoparticles hinges on its size, dispersibility in solutions, and synthetic control over its coercivity. In this work, we establish correlations between room temperature co-precipitation conditions, and these crucial materials parameters. Furthermore, post-synthesis annealing conditions are correlated with morphology, changes in crystal structure and magnetic properties. We disclose the synthesis and process conditions helpful in obtaining easily sinterable CoFe2O4 nanoparticles with coercive magnetic flux density (H-c) in the range 5.5-31.9 kA/m and M-s in the range 47.9-84.9 A.m(2)Kg(-1). At a grain size of similar to 54 +/- 2 nm (corresponding to 1073 K sintering temperature), multi-domain behavior sets in, which is indicated by a decrease in H-c. In addition, we observe an increase in lattice constant with respect to grain size, which is the inverse of what is expected of in ferrites. Our results suggest that oxygen deficiency plays a crucial role in explaining this inverse trend. We expect the method disclosed here to be a viable and scalable alternative to thermal decomposition based CoFe2O4 synthesis. The magnetic trends reported will aid in the optimization of functional CoFe2O4 nanoparticles

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We report a simple hydrothermal synthesis of highly reproducible carbon nanoparticles in a size range between 2 and 7 nmfroma single precursor sucrose without either surface passivating agents or acids and bases. The carbon nanoparticles can be used as white light phosphors, especially for ultraviolet light emitting diodes and metal-free catalyst for the reduction of nitrophenol.

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Geopolymers are an alternative binder to portland cement in the manufacture of mortars and concrete, as its three-dimensional aluminosilicate network imparts excellent mechanical properties. Use of geopolymers in place of ordinary portland cement is favored owing to the possible energy and carbon dioxide savings. River sand is another construction industry material that needs development of a sustainable alternate in India. Geopolymerization of fly ash amorphous silica mixtures is employed to produce fine aggregates as a possible replacement to river sand. Geopolymerization of fly ash amorphous silica mixtures in 10M NaOH solution at 100 degrees C for 7days produced fine aggregates termed fly ash geopolymer sand (FAPS)] that had comparable grain size distribution, specific gravity, and improved frictional resistance with river sand. The FAPS particles exhibited more alkaline pH (12.5) and higher total dissolved solids (TDS) concentration (TDS=747 mg/L) in comparison to the river sand specimen (pH=7.9 and TDS=32.5 mg/L). However, when used as fine aggregate in mortar, FAPS-mortar specimens develop similar pH, lower TDS, similar compressive strength, and modulus in relation to river sand-mortar specimens. The experimental results suggest that FAPS particles have the potential to replace river sand in the manufacture of mortar and concrete.

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This work explores the preparation of nanocrystalline Cr3+ (1-5 mol%) doped CaSiO3 phosphors by solution combustion process and study of its photoluminescence (PL) behavior. The nanopowders are well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infra-red (FTIR) spectroscopy. PXRD results confirm monoclinic phase upon calcination at 950 degrees C for 3 h. SEM micrographs indicates that the powder is highly porous and agglomerated. The TEM images show the powder to consist of spherical shaped particles of size similar to 30-60 nm. Upon 323 nm excitation, the emission profile of CaSiO3:Cr3+ exhibits a narrow red emission peak at 641 nm due to E-2 -> (4)A(2) transition and broad band at 722 nm due to T-4(2g) -> (4)A(2g). It is observed that PL intensity increases with increase in Cr3+ concentration and highest PL intensity is observed for 3 mol% doped sample. The PL intensity decreases with further increase in Cr3+ doping. This decrease in PL intensity beyond 3 mol% is ascribed to concentration quenching. Racah parameters are calculated to describe the effects of electron-electron repulsion within the crystal lattice. The parameters show 21% reduction in the Racah parameter of free ion and the complex, indicating the moderate nephelauxetic effect in the lattice. (C) 2014 Elsevier B.V. All rights reserved.

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Gd1.96-xYxEu0.04O3 (x = 0.0, 0.49, 0.98, 1.47, 1.96 mol%) nanophosphors were synthesized by propellant combustion method at low temperature (400 degrees C). The powder X-ray diffraction patterns of as formed Gd1.96Eu0.04O3 showed monoclinic phase, however with the addition of yttria it transforms from monoclinic to pure cubic phase. The porous nature increases with increase of yttria content. The particle size was estimated from Scherrer's and W-H plots which was found to be in the range 30-40 nm. These results were in well agreement with transmission electron microscopy studies. The optical band gap energies estimated were found to be in the range 5.32-5.49 eV. PL emission was recorded under 305 nm excitation show an intense emission peak at 611 nm along with other emission peaks at 582, 641 nm. These emission peaks were attributed to the transition of D-5(0) —> F-7(J) (J = 0, 1, 2, 3) of Eu3+ ions. It was observed that PL intensity increases with increase of Y content up to x = 0.98 and thereafter intensity decreases. CIE color co-ordinates indicates that at x = 1.47 an intense red bright color can be achieved, which could find a promising application in flat panel displays. The cubic and monoclinic phases show different thermoluminescence glow peak values measured under identical conditions. The response of the cubic phase to the applied dose showed good linearity, negligible fading, and simple glow curve structure than monoclinic phase indicating that suitability of this phosphor in dosimetric applications. (C) 2014 Elsevier B.V. All rights reserved.

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CaTiO3:Sm3+ (1-11 mol%) nanophosphors were successfully synthesized by a low temperature solution combustion method LCS]. The structural and morphological properties of the phosphors were studied by using Powder X-ray diffractometer (PXRD), Fourier transform infrared (FTIR), X-ray photo electron spectroscopy (XPS), scanning electron microscope (SEM) and transmission electron microscopy (TEM). TEM studies indicate that the size of the phosphor is similar to 20-35 nm. Photoluminescence (PL) properties of Sm3+ (1-11 mol%) doped CaTiO3 for NUV excitation (407 nm) was studied in order to investigate the possibility of its use in White light emitting diode (WLED) applications. The emission spectra consists of intra 4f transitions of Sm3+, such as (4)G(5/2) -> H-6(5/2) (561 nm), (4)G(5/2) -> H-6(7/2) (601-611 nm), (4)G(5/2) -> H-6(9/2) (648 nm) and (4)G(5/2) -> H-6(11/2) (703 nm) respectively. Further, the emission at 601-611 nm show strong orange-red emission and can be applied to the orange-red emission of phosphor for the application for near ultra violet (NUV) excitation. Thermoluminescence (TL) of the samples irradiated with gamma source in the dose range 100-500 Gy was recorded at a heating rate of 5 degrees C s(-1). Two well resolved glow peaks at 164 degrees C and 214 degrees C along with shouldered peak at 186 degrees C were recorded. TL intensity increases up to 300 Gy and thereafter, it decreases with further increase of dose. The kinetic parameters namely activation energy (E), frequency factor (s) and order of kinetics were estimated and results were discussed in detail. (C) 2014 Elsevier B.V. All rights reserved.

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An efficient and scalable total synthesis of the architecturally challenging sesquiterpenoid (+/-)-penifulvin A has been accomplished via a 12-step sequence with an overall yield of 16%. For the construction of this structurally complex tetracyclic molecule, the key steps used included 1,4-conjugate addition, a Pd(0) catalyzed cross-coupling reaction between an enol phosphate and trimethyl aluminum, Claisen rearrangement using the Johnson orthoester protocol, Ti(III)-mediated reductive epoxide opening-cyclization, Lewis acid catalyzed epoxy-aldehyde rearrangement, and finally a substrate controlled oxidative cascade lactonization process.

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Differential mobility analyzers (DMAs) are commonly used to generate monodisperse nanoparticle aerosols. Commercial DMAs operate at quasi-atmospheric pressures and are therefore not designed to be vacuum-tight. In certain particle synthesis methods, the use of a vacuum-compatible DMA is a requirement as a process step for producing high-purity metallic particles. A vacuum-tight radial DMA (RDMA) has been developed and tested at low pressures. Its performance has been evaluated by using a commercial NANO-DMA as the reference. The performance of this low-pressure RDMA (LP-RDMA) in terms of the width of its transfer function is found to be comparable with that of other NANO-DMAs at atmospheric pressure and is almost independent of the pressure down to 30 mbar. It is shown that LP-RDMA can be used for the classification of nanometer-sized particles (5-20 nm) under low pressure condition (30 mbar) and has been successfully applied to nanoparticles produced by ablating FeNi at low pressures.

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The investigation involves preparation and photoluminescence properties of CeO2:Eu3+ (1-11 mol%) nano phosphors by eco-friendly green combustion route using Euphorbia tirucalli plant latex as fuel. The final product was characterized by powder X-ray diffraction (PXRD), Scanning electron microcopy (SEM) and Transmission electron microscopy (TEM). The PXRD and SEM results reveals cubic fluorite phase with flaky structure. The crystallite size obtained from TEM was found to be similar to 20-25 nm, which was comparable to W-H plots and Scherrer's method. Photoluminescence (PL) emission of all the Eu3+ doped samples shows characteristic bands arising from the transitions of D-5(0) -> F-5(J) (J = 0, 1, 2, 3, 4) manifolds under excitation at 373 and 467 nm excitation. The D-5(0) -> F-7(2) (613 nm) transition often dominate the emission spectra, indicating that the Eu3+ cations occupy a site without inversion center. The highest PL intensity was recorded for 9 mol% Eu3+ ions with 5 ml latex. PL quenching was observed upon further increase in Eu3+ concentration. The international commission on illumination (CIE) chromaticity co-ordinates were calculated from emission spectra, the values (x, y) were very close to national television system committee (NTSC) standard values of pure red emission. The results demonstrate that the synthesized phosphor material could be very useful for display applications. Further, the phosphor material prepared by this method was found to be non toxic, environmental friendly and could be a potential alternative to economical routes. (C) 2014 Elsevier B.V. All rights reserved.

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GdAlO3, GdAlO3:Eu3+ and GdAlO3:Eu3+:Bi3+ nanophosphors were synthesised by solution combustion technique. Pure orthorhombic phase was obtained from powder X-ray diffraction (PXRD) studies. Scanning electron microscopy (SEM) micrographs showed the porous, agglomerated and irregular shaped particles. The particle size obtained by transmission electron microscopy (TEM) measurement was in good agreement with the values obtained by Debye Scherrer's and W-H plots. The selected area electron diffraction (SAED) pattern show single crystalline nature of the sample. Photoluminescence (PL) measurements were carried out for GdAlO3:Eu3+ and GdAlO3:Eu3+:Bi3+ phosphors excited at a wavelength of 274 nm. The characteristic emission peaks of Eu3+ ions were recorded at 590, 614, 655 and 695 nm corresponding to D-5(0) -> F-7(J) (J = 1, 2, 3, 4) transitions respectively. However, with addition of Bi3+ ions in GdAlO3:Eu3+, PL intensity drastically enhanced. Orange red color was tuned to deep red color with the addition of Bi3+ ions in GdAlO3:Eu3+ phosphor. Therefore, the phosphor was highly useful as red component in WLEDs. A single well resoled glow peak at 225 degrees C was recorded in GdAlO3 and GdAlO3:Eu3+. Further, with addition of Bi3+ ions, an additional peak at 300 degrees C was recorded. TL glow curves of different UV-exposed GdAlO3:Eu3+:Bi3+ show two TL peaks at 207 and 300 degrees C respectively. The 207 degrees C peak show simple glow peak structure and its intensity increases linearly up to 25 mm and after that it decrease. (C) 2014 Elsevier B.V. All rights reserved.

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Digestive ripening, a postsynthetic treatment of colloidal nanoparticles, is a versatile method to produce monodisperse nanoparticles and to prepare various bimetallic nanostructures. The mechanism of this process is largely unknown. Herein, we present a systematic study conducted using Au nanoparticles prepared by a solvated metal atom dispersion method to probe the mechanistic aspects of digestive ripening. In our study, experimental conditions such as concentration of capping agent, reaction time, and temperature, were found to influence the course of the digestive ripening process. Here it is shown that, during digestive ripening under reflux, nanoparticles within an optimum size window are conserved, and surface etching facilitated mass transfer resulted in monodisperse nanoparticles. Overall, digestive ripening can be considered as a kinetically controlled thermodynamic process.