RESUMO Este trabalho relata nanopartículas de prata estabilizadas com citrato (AgNPs) sintetizadas pela redução química do íon nitrato com boro-hidreto de sódio, em diferentes pHs (2-9). As AgNPs sintetizadas por este método apresentaram distribuição de tamanho de 5 a 249 nm dependente do pH, conforme determinado por espalhamento dinâmico de luz, além de morfologia esférica, conforme determinado por microscopia eletrônica de transmissão. Na faixa de pH de 3 a 7 ocorreu a agregação das nanopartículas. A distribuição de tamanho, dependendo do pH, foi determinada por espalhamento dinâmico de luz. O potencial Zeta foi determinado e a estabilidade coloidal foi correlacionada com a agregação de nanopartículas em diferentes pHs. A atividade antimicrobiana dependente do tamanho foi avaliada para duas soluções, em que ambas as amostras exibiram atividade antimicrobiana, embora as menores AgNPs sem aglomeração apresentaram propriedades antimicrobianas melhores.

ABSTRACT This paper reports citrate-stabilized silver nanoparticles (AgNPs) synthesized by nitrate ion chemical reduction with sodium borohydride, at different pHs (2–9). The AgNPs synthesized by this method exhibited size distribution from 5 to 249 nm, depending on pH, as determined by dynamic light scattering, and morphology spherical, as determined by transmission electron microscopy. In pH range 3–7 occurred aggregation of the nanoparticles. The size distribution depending on pH was determined by dynamic light scattering. The zeta potential was determined, and the colloidal stability was correlated with nanoparticles aggregation at different pHs. The size-dependent antimicrobial activity was evaluated for two solutions, wherein both samples exhibited antimicrobial activity, although the smallest AgNPs without agglomeration have enhanced antimicrobial properties.

This work reports a simple and reproducible method for silica-coated multiwalled carbon nanotubes (MWCNTs) nanostructures by the sol-gel method using tetraethoxysilane and 3-aminopropyltriethoxysilane as organosilicon precursors of silica. The synthetic method is based on a noncovalent functionalization of the MWCNTs by the adsorption of the monolayers of different polyelectrolytes, such as poly(allylamine hydrochloride) and poly(sodium 4-styrene sulfonate), which are positively and negatively charged, respectively. The role of these polyelectrolytes is the dispersion and interaction with both the nanotubes and the silicon precursors, influencing directly the silica shell growth. Two different morphology types of the silica-coated multiwalled carbon nanotubes composites were obtained on multiwalled carbon nanotubes. In both case the samples displayed uniformity in the silica layer. Finally, the investigation of the photoluminescence spectra of the samples suggested the presence of some incorrect oxygen bond, or vacancy of oxygen or even presence of nitrogen in the network, which is a typical feature of materials prepared by the sol-gel process at room temperature.

In this work, the glass forming ability was studied in potassium phosphate glasses with increasing amounts of TiO2 in order to obtain a glass-ceramic with photocatalytic properties. The first studied series has been the binary system (100-x) KPO3-xTiO2. Homogeneous and transparent glasses could be obtained with x varying from 10 to 30 mole%. Since the photocatalytic anatase phase could not be precipitated in this system, the ternary system KPO3-TiO2-Nb2O5 was investigated in order to incorporate higher TiO2 contents without spontaneous crystallization under cooling. Thermal properties of all glass samples were investigated by DSC and allowed identifying an increase of glass transition temperatures with increasing TiO2. For all compositions, exothermic events related with crystallization were also observed and suitable heat-treatments resulted in specific crystalline phases identified by X-ray diffraction. Selective precipitation of the anatase titanium oxide was successfully obtained from the glass compostion 35KPO3-25Nb2O5-40TiO2 (KN25T40) after heat treatment at 720°C for 2 h, suggesting the possibility of obtaining a glass-ceramic for photocatalytic applications. Structural investigations by Raman were also performed on glasses and glass-ceramics and allowed to point out the glass intermediary behavior of TiO2 in the phosphate vitreous network where TiO4 and TiO6 octahedra are inserted inside the phosphate network with TiO6 clusters identified at higher TiO2 contents. Raman analysis also identified anatase TiO2 in the KN25T40 glass-ceramic.

In this work a colloidal approach to synthesize water-soluble CdSe quantum dots (QDs) bearing a surface ligand, such as thioglycolic acid (TGA), 3-mercaptopropionic acid (MPA), glutathione (GSH), or thioglycerol (TGH) was applied. The synthesized material was characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), UV-visible spectroscopy (UV-Vis), and fluorescence spectroscopy (PL). Additionally, a comparative study of the optical properties of different CdSe QDs was performed, demonstrating how the surface ligand affected crystal growth. The particles sizes were calculated from a polynomial function that correlates the particle size with the maximum fluorescence position. Curve resolution methods (EFA and MCR-ALS) were employed to decompose a series of fluorescence spectra to investigate the CdSe QDs size distribution and determine the number of fraction with different particle size. The results for the MPA-capped CdSe sample showed only two main fraction with different particle sizes with maximum emission at 642 and 686 nm. The calculated diameters from these maximum emission were, respectively, 2.74 and 3.05 nm.

New glass compositions were investigated in the binary system KPO3-Nb2O5. The glass forming domain was determined by melt-quenching of the starting nominal compositions and it has been experimentally observed that glass samples can be obtained between the molar compositions 95KPO3-5Nb2O5 and 50KPO3-50Nb2O5. Chemically stable compositions from 80KPO3-20Nb2O5 to 50KPO3-50Nb2O5 were characterized by DSC for determination of characteristic temperatures Tg, Tx, Tp and Tf. Glass transition temperatures strongly increase with Nb2O5 content whereas thermal stability against devitrification progressively decreases. Thermal data were used to suggest a structural model in which NbOx polyhedra are inserted inside the phosphate chains of PO4 units. For higher Nb2O5 contents, NbOx units progressively link together to form amorphous NbOx clusters, responsible for the yellow color and lower thermal stability against devitrification. For the composition 50KPO3-50Nb2O5, it has been found that the first crystallization peak is related with precipitation of hexagonal Nb2O5 in the glass matrix whereas the high temperature exothermic peak is due to both phase transition of hexagonal niobium oxide to monoclinic niobium oxide and precipitation of niobium potassium phosphate K2Nb6P4O26.

Este trabalho trata da obtenção de SrC2O4, Ce2(C2O4)3, e SrC2O4 dopado com diferentes porcentagens de Ce3+ como precursores do luminóforo azul Sr2CeO4. Os precursores preparados foram estudados por TG e DTA. Uma mistura contendo SrC2O4 e Ce2(C2O4)3 na relação 4:1 respectivamente e SrC2O4 dopado com diferentes porcentagens de Ce3+, foram tratadas termicamente à 1100ºC, 12 horas. Os produtos foram analisados por XRD e espectroscopia de luminescência e apresentam mistura das fases SrCeO3, Sr2CeO4 e SrCO3. Os produtos contendo a fase Sr2CeO4 apresentam luminescência azul de banda larga, com exceção daquele obtido a partir de SrC2O4 dopado com 50% de Ce3+. Neste caso a fase predominante é SrCeO3. Pela curva DTA observa-se um pico endotérmico em torno de 1000ºC para todas as amostras, com exceção da amostra dopada em 50%, evidenciando a temperatura de formação da fase Sr2CeO4. A fase luminescente Sr2CeO4 é preferencialmente obtida partindo-se de SrC2O4:Ce3+ 25% e de misturas mecânicas na proporção de 4:1 de oxalatos de estrôncio e de oxalato de cério.

This work reports on the preparation of SrC2O4, Ce2(C2O4)3, and SrC2O4 doped with different percentages of Ce3+, as precursors for the new blue phosphor Sr2CeO4. Precursors were studied by using TG and DTA curves. A mixture containing SrC2O4 and Ce2(C2O4)3, in 4:1 ratio as well as SrC2O4 doped with different percentages of Ce3+, were heated under 1100ºC, 12 hours and the resulting products were analyzed by XRD and luminescence spectroscopy. All products prepared under 1100ºC, 12 hours were identified as a mixture of SrCeO3, Sr2CeO4 and SrCO3 phases. All products which Sr2CeO4 phase is detected, present blue wide band luminescence, except the one from SrC2O4 doped with 50% of Ce3+. In this case, the majority phase is SrCeO3 one. All samples DTA curves present endothermic peak ca 1000°C except the 50% doped one indicating the Sr2CeO4 phase formation. Therefore, the blue phosphor Sr2CeO4 is better prepared from SrC2O4:Ce3+ 25% or from SrC2O4 and Ce2(C2O4)3 mixtures.