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.

Urea-Based Synthesis of Zinc Oxide Nanostructures at Low Temperature

The preparation of nanometer-sized structures of zinc oxide (ZnO) from zinc acetate and urea as raw materials was performed using conventional water bath heating and a microwave hydrothermal (MH) method in an aqueous solution. The oxide formation is controlled by decomposition of the added urea in the sealed autoclave. The influence of urea and the synthesis method on the final product formation are discussed. Broadband photoluminescence (PL) behavior in visible-range spectra was observed with a maximum peak centered in the green region which was attributed to different defects and the structural changes involved with ZnO crystals which were produced during the nucleation process.

Effect of partial preferential orientation and distortions in octahedral clusters on the photoluminescence properties of FeWO4 nanocrystals

This communication is a report of our initial research to obtain iron tungstate (FeWO4) nanocrystals by the microwave-hydrothermal method at 170 degrees C for 45 min. X-ray diffraction patterns showed that the FeWO4 nanocrystals prepared with polyethylene glycol-200 have a partial preferential orientation in the (011) plane in relation to other nanocrystals prepared with sodium bis(2-ethylhexyl) sulfosuccinate and water. Rietveld refinement data indicates that all nanocrystals are monophasic with wolframite-type monoclinic structures and exhibit different distortions on octahedral [FeO6]/[WO6] clusters. High resolution transmission electron microcopy revealed an oriented attachment mechanism for the growth of aggregated FeWO4 nanocrystals. Finally, we observed that the photoluminescence properties of these nanocrystals are affected by partial preferential orientation in the (011) plane and distortions on [FeO6]/[WO6] clusters.

Sintesi e caratterizzazione di nanopolveri composite allumina-zirconia

Il presente lavoro di tesi riguarda la sintesi di nanopolveri allumina-zirconia, seguendo tre differenti metodologie (sintesi per coprecipitazione, sintesi con il metodo dei citrati, sintesi idrotermale assistita da microonde) e il trattamento termico (calcinazione) delle polveri ottenute, mediante tecniche di riscaldamento convenzionali ed alternative (microonde). Lo scopo del lavoro è consistito nell’individuare, tra le tecniche esaminate, quella più idonea e conveniente, per la preparazione di nanopolveri cristalline 95 mol% Al2O3 – 5 mol% ZrO2 e nell’esaminare gli effetti che la calcinazione condotta con le microonde, ha sulle caratteristiche finali delle polveri, rispetto ai trattamenti termici convenzionali. I risultati ottenuti al termine del lavoro hanno evidenziato che, tra le tecniche di sintesi esaminate, la sintesi idrotermale assistita da microonde, risulta il metodo più indicato e che, il trattamento termico eseguito con le microonde, risulta di gran lunga vantaggioso rispetto a quello convenzionale. La sintesi idrotermale assistita da microonde consente di ottenere polveri nano cristalline poco agglomerate, che possono essere facilmente disaggregate e con caratteristiche microstrutturali del tutto peculiari. L’utilizzo di tale tecnica permette, già dopo la sintesi a 200°C/2ore, di avere ossido di zirconio, mentre per ottenere gli ossidi di alluminio, è sufficiente un ulteriore trattamento termico a basse temperature e di breve durata (400°C/ 5 min). Si è osservato, inoltre, che il trattamento termico condotto con le microonde comporta la formazione delle fasi cristalline desiderate (ossidi di alluminio e zirconio), impiegando (come per la sintesi) tempi e temperature significativamente ridotti. L’esposizione delle polveri per tempi ridotti e a temperature più basse consente di evitare la formazione di aggregati duri nelle nanopolveri finali e di contrastare il manifestarsi di fenomeni di accrescimento di grani, preservando così la “nanostruttura” delle polveri e le sue caratteristiche proprietà.

Microwave-assisted hydrothermal synthesis of hydroxy-sodalite zeolite membrane

A high quality pure hydroxy-sodalite zeolite membrane was successfully synthesized on an alpha-Al2O3 support by a novel microwave-assisted hydrothermal synthesis (MARS) method. Influence of synthesis conditions, such as synthesis time, synthesis procedure, etc., on the formation of hydroxy-sodalite zeolite membrane by MAHS method was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and gas permeation measurements. The synthesis of hydroxy-sodalite zeolite membrane by MAHS method only needed 45 min and synthesis was more than 8 times faster than by the conventional hydrothermal synthesis (CHS) method. A pure hydroxy-sodalite zeolite membrane was easily synthesized by MAHS method, while a zeolite membrane, which consisted of NaX zeolite, NaA zeolite and hydroxy-sodalite zeolite, was usually synthesized by CHS method. The effect of preparation procedures had a dramatic impact on the formation of hydroxy-sodalite zeolite membrane and a single-stage synthesis procedure produced a pure hydroxy-sodalite zeolite membrane. The pure hydroxy-sodalite zeolite membrane synthesized by MARS method was found to be well inter-grown and the thickness of the membrane was 6-7 mum. Gas permeation results showed that the hydrogen/n-butane permselectivity of the hydroxy-sodalite zeolite membrane was larger than 1000. (C) 2004 Elsevier Inc. All rights reserved.

Morphological and Structural changes of CaxSr1-xTiO3 Powders Obtained by the Microwave-Assisted Hydrothermal Method

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

Photoluminescence of barium-calcium titanates obtained by the microwave-assisted hydrothermal method (MAH)

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

Structural and optical properties of CaTiO3 perovskite-based materials obtained by microwave-assisted hydrothermal synthesis: An experimental and theoretical insight

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Hydrothermal Microwave: A New Route to Obtain Photoluminescent Crystalline BaTiO3 Nanoparticles

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis of KNbO3 nanostructures by a microwave assisted hydrothermal method

One-dimensional nanostructures of KNbO3 have attracted a great interest in the scientific community, mainly because of their promising application as nanoelectromechanical systems (NEMS). However, the synthesis of KNbO3 structures becomes complex due to the natural tendency to form non-stoichiometric potassium niobates. In this context, we report on the crystallization of one-dimensional KNbO3 nanostructures through the reaction between Nb2O5 and KOH under microwave-assisted hydrothermal synthesis (M-H). The use of this synthesis method made possible a very fast synthesis of singlecrystalline powders. Based on SEM, TEM and XRD characterizations, the influence of the synthesis time and the reactants concentration in the structure and morphology of the resultant KNbO3 was established. The conditions that favor the crystallization of nanofingers were determined to be small amounts of Nb2O5 and short reaction times. (C) 2008 Elsevier B.V. All rights reserved.

Microwave-assisted hydrothermal synthesis of structurally and morphologically controlled sodium niobates by using niobic acid as a precursor

There are many advantages to using a microwave as a source of heat in hydrothermal reactions. Because it is a quick and homogeneous way to crystallize ceramic powders, it was used in this work for the production of antiferroelectric sodium mobate (NaNbO3) in a cubic-like form and its intermediary phase, disodium diniobate hydrate (Na2Nb2O6 center dot H2O), with a fiber morphology. The syntheses were carried out by treating niobic acid (Nb2O5 center dot nH(2)O) with NaOH. By changing the reaction time and the concentration of the reactants, particles with different structures and different morphologies could be obtained. The structural evolution of the products of this reaction was elucidated on the basis of the arrangement of the NbO6 octahedral units. Conclusive results were obtained with morphological and structural characterizations through XRD, TEM, MEV, and NMR and Raman spectroscopy. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008).

Synthesis of Fine Micro-sized BaZrO3 Powders Based on a Decaoctahedron Shape by the Microwave-Assisted Hydrothermal Method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Efficient microwave-assisted hydrothermal synthesis of CuO sea urchin-like architectures via a mesoscale self-assembly

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

Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained. (c) 2007 Elsevier B.V. All rights reserved.