Effect of different surfactants on the shape, growth and photoluminescence behavior of MnWO4 crystals synthesized by the microwave-hydrothermal method

In this communication, we report the effect of different surfactants [cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and sodium bis(2-ethylhexyl)sulfosuccinate (AOT)] on the shape, growth and photoluminescence (PL) behavior of manganese tungstate (MnWO4) crystals synthesized by the microwave-hydrothermal (MH) method at 413 K for 45 min. These crystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), ultraviolet-visible (UV-vis) absorption spectroscopy and PL measurements. XRD patterns proved that these crystals have a monoclinic structure. FE-SEM images showed that MnWO4 crystals exhibit different shapes and growth mechanisms depending on the surfactant employed. The CTAB cationic surfactant promotes the hindrance of small nuclei that leads to the formation of flake-like nanocrystals, while SDS and AOT anionic surfactants promote a growth of crystals to plate-like and leaf-like crystals due to considerable size effect of counter-ions (RSO4- and RSO2O-) and an increase in Na+ ion remnants. UV-vis absorption spectroscopy revealed different optical band gap values due to modifications in the shape, surface and crystal size. Finally, the effect of surfactants on the crystal shapes and average crystal size distribution causing changes in the PL behavior of MnWO4 crystals was explained. (C) 2011 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.

Structural refinement, growth process, photoluminescence and photocatalytic properties of (Ba1-xPr2x/3)WO4 crystals synthesized by the coprecipitation method

Barium praseodymium tungstate (Ba1-xPr2x/3)WO4 crystals with (x = 0, 0.01, and 0.02) were prepared by the coprecipitation method. These crystals were structurally characterized by X-ray diffraction (XRD), Rietveld refinements, Fourier-transform Raman (FT-Raman) and Fourier-transform infrared (FT-IR) spectroscopies. The shape and size of these crystals were observed by field emission scanning electron microcopy (FE-SEM). Their optical properties were investigated by ultraviolet visible (UV-vis) absorption and photoluminescence (PL) measurements. Moreover, we have studied the photocatalytic (PC) activity of crystals for degradation of rhodamine B (RhB) dye. XRD patterns, Rietveld refinements data, FT-Raman and FT-IR spectroscopies indicate that all crystals exhibit a tetragonal structure without deleterious phases. FT-Raman spectra exhibited 13 Raman-active modes in a range from 50 to 1000 cm(-1), while FT-IR spectra have 8 infrared active modes in a range from 200 to 1050 cm(-1). FE-SEM images showed different shapes (bonbon-, spindle-, rice-and flake-like) as well as a reduction in the crystal size with an increase in Pr3+ ions. A possible growth process was proposed for these crystals. UV-vis absorption measurements revealed a decrease in optical band gap values with an increase of Pr3+ into the matrix. An intense green PL emission was noted for (Ba1-xPr2x/3)WO4 crystals (x = 0), while crystals with (x = 0.01 and 0.02) produced a reduction in the wide band PL emission and the narrow band PL emission which is related to f-f transitions from Pr3+ ions. High photocatalytic efficiency was verified for the bonbon-like BaWO4 crystals as a catalyst in the degradation of the RhB dye after 25 min under UV-light. Finally, we discuss possible mechanisms for PL and PC properties of these crystals.

Ultrasound-assisted synthesis of aliphatic acid esters at room temperature

This work describes the ultrasound-assisted synthesis of saturated aliphatic esters from synthetic aliphatic acids and either methanol or ethanol. The products were isolated in good yields after short reaction times under mild conditions. (C) 2011 Elsevier BM. All rights reserved.

Synthesis of supported metal nanoparticle catalysts using ligand assisted methods

The synthesis and characterization methods of metal nanoparticles (NPs) have advanced greatly in the last few decades, allowing an increasing understanding of structure-property-performance relationships. However, the role played by the ligands used as stabilizers for metal NPs synthesis or for NPs immobilization on solid supports has been underestimated. Here, we highlight some recent progress in the preparation of supported metal NPs with the assistance of ligands in solution or grafted on solid supports, a modified deposition-reduction method, with special attention to the effects on NPs size, metal-support interactions and, more importantly, catalytic activities. After presenting the general strategies in metal NP synthesis assisted by ligands grafted on solid supports, we highlight some recent progress in the deposition of pre-formed colloidal NPs on functionalized solids. Another important aspect that will be reviewed is related to the separation and recovery of NPs. Finally, we will outline our personal understanding and perspectives on the use of supported metal NPs prepared through ligand-assisted methods.

Structural evolution of Eu-doped hydroxyapatite nanorods monitored by photoluminescence emission

This paper reports the synthesis of Eu-doped hydroxyapatite (HA:Eu) resulting in particles with nanorod diameters from 9 to 26 nm using the microwave hydrothermal method (HTMW). Eu3+ ions were used as a marker in the HA network by basic hydrolysis followed by the HTMW treatment. The crystalline HA:Eu nanorod nature in a short-range order was detected by photoluminescence (PL) measurements from Eu3+ emission into the HA matrix. Thus, was possible to verify that HA crystallization is favored in a short structural order when the HTMW treatment time was increased from 0 to 40 min and that the Eu3+ substitution in the HA lattice is site-selective. (C) 2012 Elsevier B.V. All rights reserved.

Synthesis of 1,2,3-triazolylpyranosides through click chemistry reaction

We have developed an efficient method for the synthesis of functionalized C-glycosyl 1,2,3-triazoles through a Cu(1)-promoted azide-alkyne 1,3-dipolar cycloaddition between a TMS-protected C-alkynyl-glycoside and organic azides. The reaction was accelerated by ultrasound irradiation and the addition of a base was not necessary to obtain the 1,2,3-triazole product. Moreover, further manipulation of the products led to chiral molecules with a C-glycoside linkage. (C) 2012 Elsevier Ltd. All rights reserved.

Synthesis Methodology Applied to a Tunable Patch Filter With Independent Frequency and Bandwidth Control

A new methodology for the synthesis of tunable patch filters is presented. The methodology helps the designer to perform a theoretical analysis of the filter through a coupling matrix that includes the effect of the tuning elements used to tune the filter. This general methodology accounts for any tuning parameter desired and was applied to the design of a tunable dual-mode patch filter with independent control of center frequency and bandwidth (BW). The bandpass filter uses a single triangular resonator with two etched slots that split the fundamental degenerate modes and form the filter passband. Varactor diodes assembled across the slots are used to vary the frequency of each degenerate fundamental mode independently, which is feasible due to the nature of the coupling scheme of the filter. The varactor diode model used in simulations, their assembling, the dc bias configuration, and measured results are presented. The theory results are compared to the simulations and to measurements showing a very good agreement and validating the proposed methodology. The fabricated filter presents an elliptic response with 20% of center frequency tuning range around 3.2 GHz and a fractional BW variation from 4% to 12% with low insertion loss and high power handling with a 1-dB compression point higher than +14.5 dB.

One-Pot, Three-Step Reaction of 5-[(Trimethylsilyl)ethynyl]pyrrolidin-2-one with Azides Catalyzed by Cu-I: Synthesis of a Novel Class of 1,4-Disubstituted 1,2,3-Triazoles

A very fast, easy and efficient synthesis is described for a novel and biologically important class of 1,4-disubstituted-4-(5-pyrrolidin-2-one)-1,2,3-triazoles by an ultrasound-assisted one-pot, three-step click reaction sequence of 5-[(trimethylsilyl)ethynyl]pyrrolidin-2-one with organic azides mediated by catalytic Cu-I salts.