Influência da superfície do titânio nitretado a plasma em diferentes atmosferas na ativação de plaquetas sanguíneas

This study aimed to analyze the biological response of titanium surfaces modified by plasma Ar + N2 + H2. Titanium disks grade II received different surface treatments Ar + N2 + H2 plasma, constituting seven groups including only polished samples used as standard. Before and after treatment the samples were evaluated in terms of topography, crystal structure and wettability, using atomic force microscopy, X-ray diffraction, Raman spectroscopy and testing of the sessile drop, respectively. Rich plasma (PRP) was applied to the surfaces modified in culture plates. Images obtained by scanning electron microscopy of the adhered platelets were analyzed to verify the behavior of platelets in the different experimental conditions. We verified that the adition of H2 on plasma atmosphere resulted in more rough surfaces, with round tops. These surfaces, in contrast to that surfaces treated with high concentration of N2, are less propense to platelet aggregation and, consequently, to the formation of thrombus when applied in biomedical devices.

Alquilação de tolueno com propeno, através de complexo ferro (II) ᵦ- diimina homogêneo e heterogeneizado em MCM-41, Al-MCM-41 e SBA-15

This work describes the synthesis and aplication of homogeneous and heterogenized iron catalysts in the alkylation reaction of toluene with propene, empolying experimental design. The homogenous complex was obtained trough the synthesis of the organic ligand folowed by the complexation of the iron(II) chloride. As to the heterogenized complexes, first were synthetized the inorganic supports (SBA-15, MCM-41 and Al-MCM-41). Then, it was synthetized the ligand again, that through funcionalization with chloropropyltrimethoxysilane (CPTMS), was anchored on the support previously calcinated. To these anchored ligands, was complexed the iron(II) chloride, previously solubilizated in tetrahydrofuran (THF). The organic ligand characterization was accomplished trough nuclear magnetic resonance (NMR) and Infrared spectroscopy (IV). The supports were characterized with x-ray diffraction (DRX), texture analysis with nitrogen adsorption/desorption (before and after the anchoring), termogravimetric analysis (TG) and infrared (IV). The metalic content was quantified trough the atomic absorption spectrophotometry (AAS). The complexes were tested in catalytic reactions emolying ethylaluminium sesquichloride (EASC) as co-catalyst in steel reactor, under mecanic stirring. The reaction conditions ranged from 4 to 36 ◦C, with many aluminum/iron ratios. The catalysts were actives in homogeneous and heterogenized ways. The homogenous catalytic complex showed a maximum turnover frequency (TOF) of 8.63 ×103 · h −1 , while, in some conditions, the anchored complexes showed better results, with TOF of until 8.08 ×103 · h −1 . Aditionally, it was possible to determine an equation, to the homogenous catalyst, that describes the product quantity in function of reacional temperature and aluminum/iron ratio.

Compósitos NiO-CGO obtidos pelo método de síntese em uma etapa

Composite NiO-C0.9Gd0.1O1.95 (NiO-GDC), one of the materials most used for the manufacture of anodes of Cells Solid Oxide Fuel (SOFC) currently, were obtained by a chemical route which consists in mixing the precursor solution of NiO and CGO phases obtained previously by the Pechini method. The nanopowders as-obtained were characterized by thermal analysis techniques (thermogravimetry and Differential Scanning Calorimetry) and calcined materials were evaluated by X-ray diffraction (XRD). Samples sintered between 1400 and 1500 ° C for 4 h were characterized by Archimedes method. The effects of the composition on the microstructure and electrical properties (conductivity and activation energy) of the composites sintered at 1500 ° C were investigated by electron microscopy and impedance spectroscopy (between 300 and 650 ° C in air). The refinement of the XRD data indicated that the powders are ultrafine and the crystallite size of the CGO phase decreases with increasing content of NiO. Similarly, the crystallite of the NiO phase tends to decrease with increasing concentration of CGO, especially above 50 wt % CGO. Analysis by Archimedes shows a variation in relative density due to the NiO content. Densities above 95% were obtained in samples containing from 50 wt % NiO and sintered between 1450 and 1500 °C. The results of microscopy and impedance spectroscopy indicate that from 30-40 wt.% NiO there is an increase in the number of contacts NiO - NiO, activating the electronic conduction mechanism which governs the process of conducting at low temperatures (300 - 500 °C). On the other hand, with increasing the measuring temperature the mobility of oxygen vacancies becomes larger than that of the electronic holes of NiO, as a result, the high temperature conductivity (500-650 ° C) in composites containing up to 30-40 wt.% of NiO is lower than that of CGO. Variations in activation energy confirm change of conduction mechanism with the increase of the NiO content. The composite containing 50 wt. % of each phase shows conductivity of 19 mS/cm at 650 °C (slightly higher than 13 mS/cm found for CGO) and activation energy of 0.49 eV.

Aplicação da perlita expandida modificada com ortofenantrolina na remoção do negro de eriocromo T em águas residuais geradas em laboratórios de ensino de química

In this study, we carried out the study of Eriochrome black T removal using expanded perlite modified orthophenanthroline by adsorption technique. The study of the adsorption process was performed by investigating the effect of the initial dye concentration, contact time and pH range of the solution (acidic and alkaline) in the adsorption process, for a so-called synthetic effluent (aqueous solution of black eriochrome T) and a real effluent (generated from the test for determining the water hardness, by complexation titration). The materials were characterized by Thermogravimetry / Differential Thermal Analysis (TG / DTA), absorption spectroscopy in the infrared (IR), X-ray Diffraction (XRD) and scanning electron microscopy (SEM). By analysis of XRD observed thinking on orthophenanthroline the modified expanded perlite. And by IR analysis showed an increase in intensity and a detailed enlargement of the absorption band related to the axial deformation of the OH bond of silanol groups of perlite (Si-OH). In the equilibration time of the study, in the evaluated time range (5-230 min) was not possible to observe the existence of a balance of time, probably attributed to the type of interaction between the Eriochrome black-T and the expanded perlite modified orthophenanthroline, being an interaction of surface origin. In the study effect of the initial concentration of the adsorbate in the case 2,0x10-4 mol / L natural pH (pH 5) gave the highest removal percentage value of eriochrome T black color with 63.74 % removal in 20 minutes of contact. In evaluating the effect of varying the pH of Eriochrome black T solution in the adsorption process, it was found that the more acidic the environment, the greater the percentage stain removal, being a result of acid-base interaction between the adsorbate and the adsorbent. In T Eriochrome black removal study in real effluent we used the optimized conditions by studying with synthetic sewage. The dye removal at pH 10, natural pH of the effluent was no significant reaching the maximum amount of color removal percentage of 8.12%, obtained already at pH 3 with maximum color removal 100.00% of color, once more proving that eriochrome black T and effectively interact better with the adsorbent at acid pH values (pH 5 or 3), and most efficiently at pH 3. thus one can mention that the perlite expanded (an amorphous aluminosilicate naturally acid) modified with orthophenanthroline (one Bronsted base) consists of a master and effective removal of coloring material in the acid-type aqueous solution, the conditions expressed in this study, can be applied as an adsorbent of this dye also mums real effluent.

Estudo da deposição de filmes finos de BaTi(1-X)Zr(X)O3 por meio de planejamento Box-Behnken

Ferroelectric ceramics with perovskite structure (ABO3) are widely used in solid state memories (FeRAM’s and DRAM's) as well as multilayered capacitors, especially as a thin films. When doped with zirconium ions, BaTiO3-based materials form a solid solution known as barium zirconate titanate (BaTi1-xZrxO3). Also called BZT, this material can undergo significant changes in their electrical properties for a small variation of zirconium content in the crystal lattice. The present work is the study of the effects of deposition parameters of BaTi0,75Zr0,25O3 thin films by spin-coating method on their morphology and physical properties, through an experimental design of the Box-Behnken type. The resin used in the process has been synthesized by the polymeric precursor method (Pechini) and subsequently split into three portions each of which has its viscosity adjusted to 10, 20 and 30 mPa∙s by means of a rotary viscometer. The resins were then deposited on Pt/Ti/SiO2/Si substrates by spin-coating method on 15 different combinations of viscosity, spin speed (3000, 5500 and 8000 rpm) and the number of deposited layers (5, 8 and 11 layers) and then calcined at 800 ° C for 1 h. The phase composition of the films was analyzed by X-ray diffraction (XRD) and indexed with the JCPDS 36-0019. Surface morphology and grain size were observed by atomic force microscopy (AFM) indicating uniform films and average grain size around 40 nm. Images of the cross section of the films were obtained by scanning electron microscopy field emission (SEM-FEG), indicating very uniform thicknesses ranging from 140-700 nm between samples. Capacitance measurements were performed at room temperature using an impedance analyzer. The films presented dielectric constant values of 55-305 at 100kHz and low dielectric loss. The design indicated no significant interaction effects between the deposition parameters on the thickness of the films. The response surface methodology enabled better observes the simultaneous effect of variables.

Síntese, estrutura e propriedades de polímeros de coordenação à base de íons lantanídeos e ácidos benzenodicarboxílicos

Metal Organic Frameworks (MOFs) are hybrids materials, often crystalline, consisting of metal or metal clusters, connected by polytopic organic ligands repetitively, leading to structures, usually porous. In this work, MOFs based on lanthanide ions (La3+ and Gd3+) and dicarboxylate type of ligands (isophthalic and terephthalic acids), were synthesized by hydrothermal, solvothermal and hydro(solvo)thermal methods. The effects of the synthetic route as well as the type of heating, conventional or by microwave, on the structure and properties of MOFs were studied. The powder samples obtained were characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. The results suggest that the addition of an organic or inorganic base is needed to promote the deprotonation of the ligand, since in the samples prepared by the hydrothermal method, without the use of a base, no formation of the metalorganic framework was observed. On the other hand, the presence of DMF as solvent or cosolvent, afforded the deprotonation of the ligand with the consequent formation of MOFs. At least two different crystalline structures were identified for the samples prepared with terephthalic acid. These samples are isostructural with those reported for phases Eu(1,3-BDC)DMF, Eu2(1,4-BDC)3 (DMF)2 and Tb(1,4-BDC)H2O. The presence of water in the reaction medium in the hydro(solvo)thermal method, provoked the growth of the structure different from that observed in the absence of water. This can be explained by the difference in the coordination mode of water and DMF to lanthanide ions. Although not identified by XRD, the samples prepared with isophthalic acid, also present metalorganic structures, which was confirmed by the presence of the characteristic displacement of the carbonyl group band in their infrared spectra, compared to the spectrum of the pure ligand. This shift was also observed in the samples prepared with terephthalic acid. Thermal analisys shows that the metal organic frameworks do not collapse occurs at a temperature below 430°C.The analysis of scanning electron microscopy suggests that the morphology of powders is highly dependent on the type of heating used, conventional or by microwave.

Ordenamento de cargas e propriedades magnéticas de ortoferritas de lantânio dopadas com estrôncio

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Ordenamento de cargas e propriedades magnéticas de ortoferritas de lantânio dopadas com estrôncio

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese e caracterização de complexos de Co(II) e Ni(II) com l-dopa, carbidopa e benzimidazol

Were synthesized in this work in the following aqueous solution coordination compounds: [Ni(LDP)(H2O)2Cl2].2H2O, [Co(LDP)Cl2].3H2O, [Ni(CDP)Cl2].4H2O, [Co(CDP)Cl2].4H2O, [Ni(BDZ)2Cl2].4H2O and [Co(BDZ)2Cl2(H2O)2]. These complexes were synthesized by stoichiometric addition of the binder in the respective metal chloride solutions. Precipitation occurred after drying the solvent at room temperature. The characterization and proposed structures were made using conventional analysis methods such as elemental analysis (CHN), absorption spectroscopy in the infrared Fourier transform spectroscopy (FTIR), X-ray diffraction by the powder method and Technical thermoanalytical TG / DTG (thermogravimetry / derivative thermogravimetry) and DSC (differential scanning calorimetry). These techniques provided information on dehydration, coordination modes, thermal performance, composition and structure of the synthesized compounds. The results of the TG curve, it was possible to establish the general formula of each compound synthesized. The analysis of X-ray diffraction was observed that four of the synthesized complex crystal structure which does not exhibit the complex was obtained from Ldopa and carbidopa and the complex obtained from benzimidazole was obtained crystal structures. The observations of the spectra in the infrared region suggested a monodentate ligand coordination to metal centers through its amine group for all complexes. The TG-DTG and DSC curves provide important information and on the behavior and thermal decomposition of the synthesized compounds. The molar conductivity data indicated that the solutions of the complexes formed behave as a nonelectrolyte, which implies that chlorine is coordinated to the central atom in the complex.

Síntese e caracterização de complexos de Co(II) e Ni(II) com l-dopa, carbidopa e benzimidazol

Were synthesized in this work in the following aqueous solution coordination compounds: [Ni(LDP)(H2O)2Cl2].2H2O, [Co(LDP)Cl2].3H2O, [Ni(CDP)Cl2].4H2O, [Co(CDP)Cl2].4H2O, [Ni(BDZ)2Cl2].4H2O and [Co(BDZ)2Cl2(H2O)2]. These complexes were synthesized by stoichiometric addition of the binder in the respective metal chloride solutions. Precipitation occurred after drying the solvent at room temperature. The characterization and proposed structures were made using conventional analysis methods such as elemental analysis (CHN), absorption spectroscopy in the infrared Fourier transform spectroscopy (FTIR), X-ray diffraction by the powder method and Technical thermoanalytical TG / DTG (thermogravimetry / derivative thermogravimetry) and DSC (differential scanning calorimetry). These techniques provided information on dehydration, coordination modes, thermal performance, composition and structure of the synthesized compounds. The results of the TG curve, it was possible to establish the general formula of each compound synthesized. The analysis of X-ray diffraction was observed that four of the synthesized complex crystal structure which does not exhibit the complex was obtained from Ldopa and carbidopa and the complex obtained from benzimidazole was obtained crystal structures. The observations of the spectra in the infrared region suggested a monodentate ligand coordination to metal centers through its amine group for all complexes. The TG-DTG and DSC curves provide important information and on the behavior and thermal decomposition of the synthesized compounds. The molar conductivity data indicated that the solutions of the complexes formed behave as a nonelectrolyte, which implies that chlorine is coordinated to the central atom in the complex.

Catalisadores bifuncionais à base de silicoaluminofosfato e fosfatos de nióbio para emprego em reações de hidroisomerização e hidrocraqueamento do n-hexadecano

Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.

Catalisadores bifuncionais à base de silicoaluminofosfato e fosfatos de nióbio para emprego em reações de hidroisomerização e hidrocraqueamento do n-hexadecano

Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.

Caracterização e avaliação da atividade fotocatalítica de catalisadores baseados no TiO2, sintetizados mediante hidrólise em uma mistura de solventes

This study involved the synthesis of photocatalysts based on titanium dioxide (TiO2). The photocatalysts were synthesized by the sol-gel method using three different proportions of acetone (25%, 50% and 75% v/v) in water/acetone mixtures, in order to control the hydrolysis of the precursor of titanium (titanium tetraisopropoxide). Aiming to investigate the structural, morphological and electronic changes provoked by the use of the solvent mixtures, different methodologies were used to characterize the oxides, such as X-ray diffraction (XRD), RAMAN spectroscopy, UV-Vis diffuse reflectance spectroscopy, and measurements of specific surface area (BET). XRD combined to RAMAN analyses revealed that the products are two-phase highly crystalline oxides involving anatase as main phase and brookite. Besides, the refined XRD using the method of Rietveld demonstrated that the presence of acetone during the synthesis influenced in the composition of the crystalline phases, increasing the proportion of the brookite phase between 13 and 22%. The band gap energy of these oxides practically did not suffer changes as function of the synthesis conditions. As shown by the isotherm, these photocatalysts are mesoporous materials with mean diameter of pores of 7 nm and approximately 20% of porosity. The surface area of the oxides prepared by hydrolysis in presence of acetone was 12% higher compared to the bare oxide. After characterized, these oxides had their photocatalytic activities evaluated by photodegradation of the azo dyes Ponceau 4R (P4R), Tartrazine (TTZ) and Reactive Red 120 (RR120), and also by the ability to mediate the photocatalytic production of hydrogen. Using the most efficient photocatalyst, the mineralization achieved for the dyes P4R, RR120 and TTZ was of respectively 83%, 79% and 56% in 120 minutes of reaction, while the discoloration of P4R e RR120 reached 100% and 94% for TTZ. In addition, the same photocatalyst in the presence of 0.5% w/w of Platinum and suspended in a 5:1 v/v water/methanol mixture, produced 56 mmol of gaseous hydrogen in five hours of experiment, corresponding to a specific rate of hydrogen production of 139.5 mmol h-1 g-1.

Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Sensibilidade à mudança de trajetória de deformação no aço TWIP980

Resultante dos avanços tecnológicos, conseguiu-se obter um aço que elimina o paradigma de se aliar alta ductilidade e resistência mecânica. Assim foi desenvolvido durante a última década o aço TWIP, deformação induzida por maclação, tendo como principal mecanismo de deformação a maclação. Este presente trabalho teve como principal objetivo caraterizar o aço TWIP980 em três temáticas diferentes: química, mecânica e microestrutura. Na primeira temática, a química, esta teve como objetivo encontrar a designação do aço TWIP em estudo. Sendo apenas conhecida a direção de laminação, RD, e a empresa que forneceu as chapas, a POSCO, o objetivo era obter a sua designação. Através da comparação das curvas de tração encontradas para o material em estudo, e conjuntamente, com as diversas curvas de tração de vários aços TWIP da empresa POSCO, realizou-se a comparação. Visto ter-se ficado reduzido a dois possíveis aços TWIP, foi através de uma análise à composição química, EDS - Espectroscopia da energia dispersa por raios-X, que se concluiu que o aço em estudo era o TWIP980. Na caraterização mecânica, e através de ensaios de tração, foram estudadas propriedades como: o módulo de elasticidade, tensão limite elástico, ductilidade, anisotropia, coeficiente de encruamento e Poisson. Estas propriedades foram estudas para três mudanças na trajetória de deformação e quatro pré-deformações em estudo. Assim estudou-se a alteração de trajetória para os ângulos a 0º, 45º e 90º em relação a RD, para as deformações de engenharia de 0%, 10%, 20% e 30%. Por último, na análise à microestrutura, esta teve como objetivo obter valores para o tamanho de grão e de macla bem como as suas orientações cristalográficas. Também a densidade de deslocações e maclação para cada uma das 4 pré-deformações esteve em estudo. Estes parâmetros foram obtidos através de microscopia ótica, eletrónica de varrimento, MEV e eletrónica de transmissão, MET.