Influence of water flow rate on shear bond strength of resin composite to Er : YAG cavity preparation

Purpose: To evaluate in vitro the influence of water flow rate on shear bond strength of a resin composite to enamel and dentin after Er:YAG cavity preparation. Methods: Ten bovine incisors were selected and roots removed. Crowns were sectioned in four pieces, resulting in 40 samples that were individually embedded in polyester resin (n=10), and ground to plane the enamel and expose the dentin. The bonding site was delimited and samples were randomly assigned according to cavity preparation: (1) Er:YAG/1.0 mL/minute; (2) Er:YAG/1.5 mL/minute; (3) Er:YAG/2.0 mL/minute and (4) High speed handpiece/bur (control group). Samples were fixed to a metallic device, where composite resin cylinders were prepared. Subsequently, they were stored for 24 hours and subjected to a shear bond strength test (500N at 0.5 mm/minute). Results: Means (MPa) were: enamel: 1: 12.8; 2: 16.8; 3: 17.5; 4: 36.0 and Dentin: 1: 13.6; 2: 18.7; 3: 12.1; 4: 21.3. Data were submitted to ANOVA and Tukey`s test. Adhesion to enamel was more efficient than for dentin. The cavities prepared with conventional bur (control) presented higher statistically significant bond strength values (P<0.05) than for Er:YAG laser for both enamel and dentin. No significant differences were observed between water flow rates employed during enamel ablation. For dentin, the shear bond strength of 2.0 mL/minute water flow rate was lower than for 1.5 mL/minute and 1.0 mL/minute rates. The Er:YAG laser adversely affected shear bond strength of resin composite to both enamel and dentin, regardless of the water flow rate used.

The Ability of Different Nickel-Titanium Rotary Instruments To Induce Dentinal Damage During Canal Preparation

The purpose of this study was to compare the incidence of dentinal defects (fractures and craze lines) after canal preparation with different nickel-titanium rotary files. Two hundred sixty mandibular premolars were selected. Forty teeth were left unprepared (n = 40). The other teeth were prepared either with manual Flexofiles (n = 20) or with different rotary files systems: ProTaper (Dentsply-Maillefer, Ballaigues, Switzerland), ProFile (Dentsply-Maillefer), SystemGT (Dentsply-Maillefer), or S-ApeX (FKG Dentaire, La Chaux-de-Fonds, Switzerland) (n = 50 each). Roots were then sectioned 3, 6, and 9 mm from the apex and observed under a microscope. The presence of dentinal defects was noted. There was a significant difference in the appearance of defects between the groups (p < 0.05). No defects were found in the unprepared roots and those prepared with hand files and S-ApeX. ProTaper, ProFile, and GT preparations resulted in dentinal defects in 16%, 8%, and 4% of teeth, respectively. Some endodontic preparation methods might damage the root and induce dentinal defects. (J Endod 2009;35:236-238)

Tin oxide nanoparticle formation using a surface modifying agent

This work presents results concerning the preparation of redispersible tin oxide nanoparticles achieved by using Tiron molecule ((OH)(2)C(6)H(2) (SO(3)Na)(2)) as surface modifying agent. The adsorption isotherm measurements show that an amount of 10 wt.% of Tiron is need to recover the SnO(2) nanoparticles surface with a monolayer. These nanoparticles can be easily redispersed in tetramethyl ammonium hydroxide at pH greater than or equal to11 until a powder concentration of 12 vol.% of tin. Under these conditions, hydrodynamic particle size is about 7 nm and increases until 52 nm at pH 6 due to the aggregation phenomenon. The time evolution of the viscoelastic properties indicates that the suspensions at pH 12.5, containing 12 vol.% tin oxide and 10 wt.% of surface modifier are kinetically stable. After thermal treatment at different temperature the powder characterisation evidences that the presence of Tiron monolayer at the nanoparticles surface increases the thermal stability of the porous texture and prevent the micropore size growth. This set of results contributes to satisfy the demand for more controlled synthesis of nanoparticles with high thermal stability as required for fabrication of ultrafiltration ceramic membranes. (C) 2004 Elsevier Ltd. All rights reserved.

New strategies in the preparation of exfoliated thermoplastic starch-montmorillonite nanocomposites

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

Influence of mineralizer agents on the growth of crystalline CeO 2 nanospheres by the microwave-hydrothermal method

Cystalline ceria (CeO2) nanoparticles have been synthesized by a simple and fast microwave-assisted hydrothermal (MAH) under NaOH, KOH, and NH4OH mineralizers added to a cerium ammonium nitrate aqueous solution. The products were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transformed-IR and Raman spectroscopies. Rietveld refinement reveals a cubic structure with a space group Fm3m while infrared data showed few traces of nitrates. Field emission scanning microcopy (FEG-SEM) revealed a homogeneous size distribution of nanometric CeO2 nanoparticles. The MAH process in KOH and NaOH showed most effective to dehydrate the adsorbed water and decrease the hydrogen bonding effect leaving a weakly agglomerated powder of hydrated ceria. TEM micrographs of CeO2 synthesized under MAH conditions reveal particles well-dispersed and homogeneously distributed. The MAH enabled cerium oxide to be synthesized at 100 °C for 8 min. © 2012 Elsevier B.V. All rights reserved.

Synthesis of PTSH-modified CeO2 nanoparticles: Effect of the modifier on structure, optical properties, and dispersibility

CeO2 nanoparticles were synthesized by the precipitation method and modified with para-toluene sulfonic acid (PTSH), either in situ or post-synthesis. The presence of PTSH in the samples was confirmed by FTIR. PXRD and FTIR analyses showed that the post-synthesis PTSH modification altered the CeO2 structure, whereas the in situ modification maintained intact the crystalline structure and UV-vis absorbance properties. For both in situ and post-synthesis modifications, TEM images revealed the presence of nanoparticles that were 5nm in size. The dispersibility of the in situ PTSH-modified material in a hydrophilic ureasil-poly(ethylene oxide) matrix was investigated using SAXS measurements, which indicated that CeO2 nanoparticles modified with PTSH in situ were less aggregated within the matrix, compared to unmodified CeO2 nanoparticles. © 2013 Elsevier B.V.

Degradation of dipyrone via advanced oxidation processes using a cerium nanostructured electrocatalyst material

This work studied the degradation of dipyrone, via electrochemical processes and via electro-Fenton reaction using a 4% CeO2/C gas diffusion electrode (GDE) prepared via modified polymeric precursor method. This material was used to electrochemically generate H2O2 through oxygen reduction. The mean crystallite sizes estimated by the Scherrer equation for 4% CeO2/C were 4 nm for CeO2-x (0 4 4) and 5 nm for CeO2 (1 1 1) while using transmission electron microscopy (TEM) the mean nanoparticle size was 5.4 nm. X-ray photoelectron spectroscopy (XPS) measurements revealed nearly equal concentrations of Ce(III) and Ce(IV) species on carbon, which contained high oxygenated acid species like CO and OCO. Electrochemical degradation using Vulcan XC 72R carbon showed that the dipyrone was not removed during the two hour electrolysis in all applied potentials by electro-degradation. Besides, when the Fenton process was employed the degradation was much similar when using cerium catalysts but the mineralization reaches just to 50% at -1.1 V. However, using the CeO2/C GDE, in 20 min all of the dipyrone was degraded with 26% mineralization at -1.3 V and when the Fenton process was employed, all of the dipyrone was removed after 5 min with 57% mineralization at -1.1 V. Relative to Vulcan XC72R, ceria acts as an oxygen buffer leading to an increase in the local oxygen concentration, facilitating H2O2 formation and consequently improving the dipyrone degradation © 2013 Elsevier B.V. All rights reserved.

Low tungsten content of nanostructured material supported on carbon for the degradation of phenol

A comparative study using different mass proportions of WO3/C (1%, 5%, 10% and 15%) for H2O2 electrogeneration and subsequent phenol degradation was performed. To include the influence of the carbon substrate and the preparation methods, all synthesis parameters were evaluated. The WO3/C materials were prepared by a modified polymeric precursor method (PPM) and the sol-gel method (SGM) on Vulcan XC 72R and Printex L6 carbon supports, verifying the most efficient metal/carbon proportion. The materials were physically characterized by X-ray diffraction (XRD) and by X-ray photoelectron spectroscopy (XPS) techniques. The XRD and the XPS techniques identified just one phase containing WO3 and elevated oxygen concentration on carbon with the presence of WO3. The oxygen reduction reaction (ORR), studied by the rotating ring-disk electrode technique, showed that WO3/C material with the lowest tungsten content (1% WO3/C), supported on Vulcan XC 72R and prepared by SGM, was the most promising electrocatalyst for H2O2 electrogeneration. This material was then analyzed using a gas diffusion electrode (GDE) and 585mgL-1 of H2O2 was produced in acid media. This GDE was employed as a working electrode in an electrochemical cell to promote phenol degradation by an advanced oxidative process. The most efficient method applied was the photo-electro-Fenton; this method allowed for 65% degradation and 11% mineralization of phenol during a 2-h period. Following 12h of exhaustive electrolysis using the photo-electro-Fenton method, the total degradation of phenol was observed after 4h and the mineralization of phenol approached 75% after 12h. © 2013 Elsevier B.V.

Síntese e aplicação de catalisadores à base de óxidos de cério, tungstênio e HZSM-5 para a produção do biodiesel

This work presents a study on the production of biodiesel by esterification reaction of oleic acid with methanol using batch reactor and different catalysts based on CeO2 and WO3 and HZSM-5. Acid treatment was performed in order to increase the catalytic activity. Different characterization techniques were performed, among them X-ray diffraction (XRD), Thermogravimetric analysis TGA/DTA, Spectroscopy in the Region in Fourier Transform Infrared (FTIR) and X-ray fluorescence (XRF). The effects of independent variables: temperature, molar ratio of oil: alcohol and the amount of catalyst and their interactions on the dependent variable (conversion of oleic acid to the corresponding ester). Overall, through the results obtained in the characterization was observed that the applied treatments were efficient, however the XRF technique, indicated that tungsten oxide leaching could occur during the preparation of the materials. The treatments performed on HZSM-5 caused no significant changes in the structure indicating that the zeolite was quite resistant to the treatments used. It was evaluated using complete 23 factorial design. For the catalysts investigated, the best reaction conditions were obtained when using higher levels of the independent variables temperature and amount of catalyst. However, for the variable molar ratio the lowest level showed significant yields for most of the synthesized catalyst, obtaining maximum conversion to the OC (67.97%), OW (74.37%), HZSM-5 (61.16%) OC-OW 1 (75.93%), OC-OW 2 (82.57%), OC-OW 3 (79.15%), S/OC-OW 1 (86.90%), S/OC-OW 2 (91.04%), S/OC-OW 3 (88.60%), S/OC-OW/H 1 (92.34%), S/OC-OW/H 2 (100%) and S/OC-OW/H 3 (98.16%). According to the experimental design, the temperature has the biggest influence on the reaction variable for all the synthesized catalysts. Among the catalysts investigated S/OC-OW/H 2 e S/OC-OW/H 3 were more effective. Reuse tests showed that the catalyst activity decreased after each cycle, indicating that the regeneration process was effective. The leaching test indicated that the catalysts are heterogeneous in the evaluated operating range. The catalysts investigated showed themselves promising for the production of biodiesel.

Estudo do crescimento de nanofitas de céria dopada com gadolínio por sistema de aquecimento por micro-ondas

O óxido de cério (céria) tem atraído atenção devido às suas importantes aplicações, como em células a combustível de óxido sólido, catalisadores de gases de exaustão de automóveis, catalisadores para a obtenção de hidrogênio, bloqueadores de raios ultravioleta, biomateriais, entre outros. Controlar os métodos de síntese da céria é de grande importância para explicar ou prever essas propriedades. Desta forma, o objetivo deste trabalho foi estudar o crescimento de nanofitas de óxido de cério em um sistema hidrotérmico assistido por micro-ondas, no qual 8 min foram obtidas nanofitas com comprimentos próximos a 330 nm, em 130 ºC e pressão de 3 atm. Os resultados colaboram para pesquisas em reformadores para obtenção de etanol e/ou anodos de células combustíveis de óxido sólido.

Estudo do potencial de associações de ZnO com os produtos naturais ácido cafeico e ferúlico como filtros solares híbridos: [recurso eletrônico]

In this work were studied associations of ZnO with the natural products caffeic and feluric acids. Two preparation methods were used, that is, the sol-gel and a reflux procedure. In the sol-gel method, ZnO is produced by the basics hydrolysis of precursors in the presence of the organic filters (caffeic and feluric acids), which results in 30 nm (or less) ZnO particles with the organic filters (in dissociated form) bonded to the surface of ZnO. In the reflux method, a dispersion of ZnO in a water/ethanol mixture was kept under reflux (50oC/4h) in the presence of the organic acids. The ZnO particles used in the reflux method have a higher diameter than sol-gel ZnO particles, but the prepared associated product ZnO/Organic acids were similar. Despite of the difference in relation to crystallinity between the products, the preparation methods resulted in analogous associations with respect to the interaction of the organic filters with the ZnO surface. The caffeic/ZnO associations presented low photostability, which lead to the degradation of the organic filter. The other associations (feluric acid/ZnO) presented satisfactory results. The FT-IR spectroscopy confirmed the formation of the association, and the nature of the bond formed compared with the Zn-O bond in Zn2+/Felutic acid complexes. The isolated organic and inorganic filters, along with the associations were analyzed by diffuse reflectance spectroscopy and Uv-vis spectroscopy. The absorption edges and the critical wavelengths were analyzed and the effects of Zn-O bonds in feluric acid/ZnO associations described as a function of the relative position of the π/π* system of the organic filter. Finally the performance of the hybrid filters were investigated in terms of the absorption of UVA and UVB radiations, with the UVA/UVB ratio, an efficiency parameter largely used in the description of solar filters, sunscreen and suncare products

Influence of the preparation route on the structural, morphological and spectroscopic properties of SrTiO3 and SrTiO3:eu3+ powders

This research shows the influence of the synthesis route in the structural and morphological characteristics as well as in the luminescent properties of doped with europium and pure SrTiO3 (STO) powders prepared by microwave assisted hydrothermal synthesis, MWH, and by the polymeric precursor method, PPM. The XRD at room temperature of the STO powders nominally pure obtained by PPM at 700°C for 3 hours, as well as by the MWH at 190°C by 30 minutes present all the reflection peaks for the cubic perovskite structure (JCPDS-ICDD 35-734). The morphology varies according to the synthesis route. The particles of pure STO obtained by PPM presents morphology in the form of plates and the morphology of the particles synthesized by MWH is spherical with approximately 150 nm. The photoluminescent analysis shows for pure STO wide bands associated with the transition of charge transfer from the titanates group (TiO3)2- that are centered on 450 nm. In both preparation methods the emission bands obtained in the composites spectra were found to be asymmetric and low intense. However, in the case of the STO prepared by the PPM a bigger FWHM of the band can be observed. The excitation of the samples was done using a laser (Coherent Innova) with wavelength of 350 nm.

Catalisadores de cobre suportados em óxidos de zircônio hierarquicamente estruturados para a reação de desidrogenação de etanol

Pós-graduação em Química - IQ

Organokompatible Zinnoxid-Nanopartikel

In der vorliegenden Arbeit werden verschiedene Methoden der Synthese von Zinn(IV)oxid Nanopartikeln, deren Stabilisierung durch unterschiedliche Surfactants und der Einbau der Nanomaterialien in PMMA beschrieben und die erhaltenen Materialien charakterisiert. Die Darstellung der Zinnoxid Nanopartikel wurde über drei verschiedene Synthesewege durchgeführt: a) Polymeric Precursor Methode, b) Solvothermal-Synthese und c) säurekatalysierte Fällungsreaktion. Im Rahmen von a) konnte neben der thermodynamisch stabilen Phase von Zinn(IV)oxid ebenfalls die metastabile orthorhombische Phase synthetisiert werden. Durch eine Analyse der Pyrolysebedingungen konnte der Kristallisationsmechanismus des Zinnoxids ausgehend vom Precursor bis zur tetragonalen Phase des Zinn(IV)oxid diskutiert werden. Die Synthesemethoden b) und c) boten sich zur Darstellung von oberflächenmodifizierten Zinnoxid Nanopartikeln an. Als Surfactant benutzte man unter anderem Alkylphosphonsäuren, da eine hydrophobe Oberfläche die Dispersion in MMA ermöglichte. Abschließend wurde eine radikalische in situ-Polymerisation von MMA in Gegenwart von oberflächenmodifizierten Partikeln durchgeführt. Der erhaltene Verbundwerkstoff zeichnete sich durch eine erhöhte thermische Stabilität aufgrund weniger Strukturdefekte des Polymers aus. Durch eine Untersuchung des Polymerisationsmechanismus konnte die Wirkung der oberflächenmodifizierten Nanopartikel auf die Polymerisation veranschaulicht werden. Aufgrund der nicht homogenen Verteilung der Nanopartikel im Verbundwerkstoff konnte jedoch keine Charakterisierung der optischen Eigenschaften durchgeführt werden.

Hydrophobe und hydrophile Beladung polymerer Vesikel

Polymere Vesikel, gebildet durch Selbstorganisation des amphiphilen Blockcopolymers Polybutadien-b-Polyethylenoxid in Wasser, wurden in der vorliegenden Arbeit erfolgreich mit hydrophoben und hydrophilen Substraten beladen und detailliert charakterisiert. Über verschiedene Präparationsmethoden sind unilamellare PB130-PEO66-Vesikel unterschiedlicher Größen und Verteilungsbreiten zugänglich, die aber alle eine konstante hydrophobe Schalendicke von etwa 15nm aufweisen, wie aus TEM-Messungen hervorgeht. Die hydrophoben Farbstoffe Oil Red EGN, Oil Blue N, Nilrot sowie ein Perylen-Derivat wurden in diese hydrophobe Schale eingelagert. Durch Absorptions-, Emissions-, (cryo)TEM- und Fluoreszenzmikroskopie-Messungen konnte gezeigt werden, dass die selbstorganisierte Struktur durch die Einlagerung der hydrophoben Farbstoffe in die Schale nicht beeinflusst wird. Als zusätzliche hydrophobe Modell-Substrate wurden Halbleiter-Nanokristalle, sogenannte Quantum Dots (QDs, d=5.7nm), erfolgreich in die polymere Vesikelschale eingelagert und durch Fluoreszenz-Korrelations-Spektroskopie (FCS) in Kombination mit dynamischer Lichtstreuung (DLS) nachgewiesen. Die Position der QDs in der Mitte der polymeren Doppelmembran konnte durch cryogene TEM-Abbildungen aufgezeigt werden. Darüber hinaus wurde die hydrophile Beladung des Vesikelkerns mit dem wasserlöslichen Farbstoff Phloxin B erfolgreich realisiert.