Stable colloidal suspensions of nanostructured zirconium oxide synthesized by hydrothermal process

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

Preparation and characterization of ceria nanospheres by microwave-hydrothermal method

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

2-methoxybenzylidenepyruvate with heavier trivalent lanthanides and yttrium(III) - Synthesis and characterization

Solid-state Ln(2-MeO-BP) compounds, where Ln stands for trivalent Eu to Lu and Y(III) and 2-MeO-BP (which is 2-methoxybenzylidenepyruvate) have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffraction, infrared spectroscopy and other methods of analysis were used to characterize and to study these compounds. on the base of the obtained results an Ln(2MeO-BP)(3)center dot H2O general formula can be established.

Hydrothermal treatment of gadolinium oxide in presence of silica

Hydrothermal and solvothermal (isopropanol) treatments of gadolinium oxide and silica were investigated under different pressure and temperature conditions. Products were examined by infrared vibrational spectroscopy (IR), x-ray powder diffraction (XRD) and thermal analysis (DTA, TG). Hexagonal gadolinium hydroxide was obtained in hydrothermal conditions, even in presence of silica, while no change was observed from isopropanolic medium treatment. Hydrothermally treated samples are more reactive as precursors for solid state reactions in inorganic synthesis.

Preparation and characterization of uniform, spherical particles of Y2O2S and Y2O2S:Eu

The preparation of spherical Y2O2S and Y2O2S:Eu particles using a solid-gas reaction of monodispersed precursors with elemental sulfur vapor under an argon atmosphere has been investigated. The precursors, undoped and doped yttrium basic carbonates, are synthesized by aging a stock solution containing the respective cation chloride and urea at 82-84 °C. Y2O2S and Y2O2S:Eu were characterized in terms of their composition, crystallinity and morphology by chemical analysis, X-ray powder diffraction (XRD), IR spectroscopy, and scanning electron microscopy (SEM). The Eu-doped oxysulfide was also characterized by atomic absorption spectrophotometry and luminescence spectroscopy. The spherical morphology of oxysulfide products and of basic carbonate precursors suggests a topotatic inter-relationship between both compounds.

Preparation and thermal decomposition of solid-state cinnamates of lighter trivalent lanthanides

Some new compounds of cinnamic acid with lighter trivalent lanthanides were prepared in the solid state. The compounds have general formula ML3·H2O, where L is cinnamate (C6H5-CH=CH-COO-) and M is La, Ce, Pr, Nd or Sm. Thermogravimetry, derivative thermogravimetry, differential scanning calorimetry, infrared absorption spectra and X-ray diffraction powder patterns were used to characterize and to study the thermal stability and thermal decomposition of these compounds.

Microstructural characteristics and electrochemical behavior of Co3O4 sintered electrodes

Co3O4 can be used as electrocatalyst for oxygen evolution reaction. The macro and microstructure of the oxide, obtained by compacting and sintering lithium-doped Co3O4 powder in atmosphere of dry air and in conditions of controlled temperature and time was analyzed by metallographic techniques. The porous material was characterized by XRD, SEM and EDS combined techniques. For working temperatures up to 1200°C, the pellet was consituted of particles with varying sizes over a wide range of particle size and, at higher temperatures CoO is formed and polymorphic transformation was observed. The materials were also characterized electrochemically in alkaline media by open circuit potential and potentiodynamic I/E measurements. The results were compared to those previously prepared by others by thermal deposition.

Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with some bivalent transition metal ions

Solid-state M-4-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds. © 2005 Akadémiai Kiadó, Budapest.

Heating rate and temperature effects on the BaTiO3 formation by thermal decomposition of (Ba,Ti) organic precursors during the Pechini process

Different thermal treatments for the synthesis of BaTiO3 powder obtained through the Pechini method were studied. The synthesis of BaTiO3 starts at 150 °C by the thermal dehydration of organic precursors. The usual inevitable formation of barium carbonate during the thermal decomposition of the precursor could be retarded at lower calcination temperatures and optimized heating rates. The organic precursors were treated at temperatures between 200 and 400 °C. Then, the samples were calcined at 700 and 800 °C for 4 and 2 h, respectively. The resulting ceramic powders were characterized by gravimetric and differential thermal analyses, X-ray powder diffraction and infrared spectroscopy. It was found that depending on the heating rate and final temperature of the thermal treatment, high amounts of BaCO3 and TiO2 could be present due to the high concentration of organics in the final calcination step. © 2007 Elsevier B.V. All rights reserved.

CdMoO 4 synthesized by a microwave-assisted hydrothermal method and their photoluminescence and photocatality properties

In this work CdMoO 4 nanoparticles were obtained under hydrothermal conditions using microwave radiation (2.45 GHz) (MH) at 100°C for different times. These powders were analyzed by X-ray diffraction (XRD), Field-emisson gum scanning electron microscopy (FEG-SEM), Ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD pattern confirmed that the pure CdMoO 4 phases were obtained. FEG-SEM powders present large-scale and homogeneous particles with microspheres-like morphology. UV-vis results were employed to determine the optical band gap these materials. Also, it showed existence of photoluminescence (PL) emission in the green wavelength range of 540-546 nm. Photocatalytic activity of CdMoO 4 nanocrystals was examined by monitoring the degradation of rhodamine B dye.

Microwave-assisted hydrothermal synthesis of ZnO powders with different reagents

In this work, zinc oxide powders were synthesized by microwave-assisted hydrothermal method in basic medium. These powders were analyzed by X-ray diffraction (XRD), Field-emisson gum scanning electron microscopy (FEG-SEM), Ultraviolet-visible (UV-vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD pattern confirmed that the pure ZnO phases were obtained after MH processing performed at 130°C/ 1h. FEG-SEM micrographs reveals that these nanostructures are made up of ZnO plates. UV-vis results were employed to determine the optical band gap these materials. Also, it showed existence of photoluminescence (PL) in the different zinc powders. An orange PL emission when excited by 350 nm wavelength at room temperature was observad in the different powders.

Strongly luminescent, highly ionic europium in a lanthanum diphenylphosphinate matrix

A series of insoluble, chemically inert and thermally stable compounds La1-xEux(DPP)3 (x = 0.50, 0.20, 0.10, and 0.050; DPP = diphenylphosphinate) was synthesized and characterized by elemental and thermogravimetric analysis, FT Infrared spectroscopy and X-ray powder diffraction. Luminescence spectroscopy at both 77 and 298 K showed changes in the intensity of the hypersensitive transition 5D 0 → 7F2 of Eu3+ which are dependent of the excitation wavelength, suggesting that the europium occupies two different sites in the compounds. The large quantum efficiency and quantum yield, as well as the long radiative lifetime of the 5D0 Eu3+ level of the series of compounds, which are desirable qualities for light-conversion molecular devices, are discussed in terms of the interactions and the energy transfer process between the ligands and the metal ion. © 2012 Elsevier B.V. All rights reserved.

Synthesis, structural characterization and photophysical properties of highly photoluminescent crystals of Eu(III), Tb(III) and Dy(III) with 2,5-thiophenedicarboxylate

Lanthanide compounds of general formula [Ln2(2,5-tdc) 3(dmf)2(H2O)2] ·2dmf·H2O (Ln = Eu(III) (1), Tb(III) (2), Gd(III) (3) and Dy(III) (4), dmf = N,N′-dimethylformamide and 2,5-tdc2- = 2,5-thiophedicarboxylate anion) were synthesized and characterized by elemental analysis, X-ray powder diffraction patterns, thermogravimetric analysis and infrared spectroscopy. Phosphorescence data of Gd(III) complex showed that the triplet states (T1) of 2,5-tdc2- ligand have higher energy than the main emitting states of Eu(III), Tb(III) and Dy(III), indicating that 2,5-tdc2- ligand can act as intramolecular energy donor for these metal ions. An energy level diagram was used to establish the most relevant channels involved in the ligand-to-metal energy transfer. The high value of experimental intensity parameter Ω2 for the Eu(III) complex indicate that the europium ion is in a highly polarizable chemical environment. The emission quantum efficiency (η) of the 5D0 emitting level of Eu(III) was also determined. The complexes act as possible light conversion molecular devices (LCMDs). © 2013 Elsevier B.V. All rights reserved.

Development and characterization of a new bio-nanocomposite (bio-NCP) for diagnosis and treatment of breast cancer

Breast cancer is a public health problem throughout the world. Moreover, breast cancer cells have a great affinity for hydroxyapatite, leading to a high occurrence of bone metastasis. In this work we developed a bio-nanocomposite (bio-NCP) in order to use such affinity in the diagnosis and treatment of breast cancer. The bio-NCP consists of magnetic nanoparticles of Mn and Zn ferrite inside a polymeric coating (chitosan) modified with nanocrystals of apatite. The materials were characterized with synchrotron X-ray Powder Diffraction (XPD), Time-of-Flight Neutron Powder Diffraction (NPD), Fourier Transformed Infra-red Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and magnetic measurement with a Physical Property Measurement System (PPMS). We obtained ferrite nanoparticles with a high inversion degree of the spinel structure regarding the Fe and Mn, but with all the Zn in the A site. The coating of such nanoparticles with chitosan had no notable effects to the ferrite microstructure. In addition, the polymeric surface can be easily modified with apatite nanocrystals since the hydration of the bio-NCP during synthesis can be controlled. The resulting bio-NCP presents a spherical shape with a narrow size distribution and high magnetic response at room temperature and is a very promising material for early diagnosis of breast cancer and its treatment. © 2013 Elsevier B.V.

Estudo termoanalítico e caracterização no estado sólido dos anti-hipertensivos: atenolol, besilato de anlodipino e maleato de enalapril

Pós-graduação em Ciência e Tecnologia de Materiais - FC