Obtenção e caracterização de nanopartículas de argilominerais

Natural nanoclays are of great interest particularly for the production of polymer-based nanocomposites. In this work, kaolinite clays from two natural deposits in the State of the Rio Grande do Norte and Paraiba were purified with thermal treatment and chemical treatments, and characterized. Front to the gotten data, had been proposals methodologies for elimination or reduction of coarse particle texts, oxide of iron and organic substance. These methodologies had consisted of the combination of operations with thermal treatments, carried through in electric oven, and acid chemical attacks with and hydrogen peroxide. The Analyzers Thermogravimetric was used to examine the thermal stability of the nanoclays. The analysis indicated weight losses at temperatures under 110 ºC and over the temperature range of 350 to 550 ºC. Based on the thermal analysis data, the samples were submitted to a thermal treatment at 500 °C, for 8 h, to remove organic components. The X-ray diffraction patterns indicated that thermal treatment under 500 °C affect the basic structure of kaolinite. The BET surface area measurements ranged from 32 to 38 m2/g for clay samples with thermal treatment and from 36 to 53 m2/g for chemically treated samples. Thus, although the thermal treatment increased the surface area, through the removal of organic components, the effect was not significant and chemical treatment is more efficient, not affect the basic structure of kaolinite, to improve particle dispersion. SEM analysis confirms that the clay is agglomerated forming micron-size particles

Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Avaliação espectrofotométrica do manchamento de resinas odontológicas contendo nanopartículas

Composite resins have been subjected to structural modifications aiming at improved optical and mechanical properties. The present study consisted in an in vitro evaluation of the staining behavior of two nanohybrid resins (NH1 and NH2), a nanoparticulated resin (NP) and a microhybrid resin (MH). Samples of these materials were prepared and immersed in commonly ingested drinks, i.e., coffee, red wine and acai berry for periods of time varying from 1 to 60 days. Cylindrical samples of each resin were shaped using a metallic die and polymerized during 30 s both on the bottom and top of its disk. All samples were polished and immersed in the staining solutions. After 24 hours, three samples of each resin immersed in each solution were removed and placed in a spectrofotome ter for analysis. To that end, the samples were previously diluted in HCl at 50%. Tukey tests were carried out in the statistical analysis of the results. The results revealed that there was a clear difference in the staining behavior of each material. The nanoparticulated resin did not show better color stability compared to the microhybrid resin. Moreover, all resins stained with time. The degree of staining decreased in the sequence nanoparticulated, microhybrid, nanohybrid MH2 and MH1. Wine was the most aggressive drink followed by coffee and acai berry. SEM and image analysis revealed significant porosity on the surface of MH resin and relatively large pores on a NP sample. The NH2 resin was characterized by homogeneous dispersion of particles and limited porosity. Finally, the NH1 resin depicted the lowest porosity level. The results revealed that staining is likely related to the concentration of inorganic pa rticles and surface porosity

Adição de nanopartículas de Ti em matriz de Fe através da deposição por magnetron sputtering

Microalloyed steels constitute a specific class of steel with low amount of carbon and microalloying elements such as Vanadium (V), Niobium (Nb) and Titanium (Ti). The development and application of microalloyed steels and steels in general are limited to the handling of powders with particles of submicron or nanometer dimensions. Therefore, this work presents an alternative in order to construction of microalloyed steels utilizing the deposition by magnetron sputtering technique as a microalloying element addiction in which Ti nanoparticles are dispersed in an iron matrix. The advantage of that technique in relation to the conventional metallurgical processes is the possibility of uniformly disperse the microalloying elements in the iron matrix. It was carried out deposition of Ti onto Fe powder in high CH4, H2, Ar plasma atmosphere, with two deposition times. After the deposition, the iron powder with nanoparticles of Ti dispersed distributed, were compacted and sintered at 1120 ° C in resistive furnace. Characterization techniques utilized in the samples of powder before and after deposition of Ti were Granulometry, Scanning Electron Microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (DRX). In the case of sintered samples, it was carried out characterization by SEM and Vickers Microhardness assays. The results show which the deposition technique by magnetron sputtering is practicable in the dispersion of particles in iron matrix. The EDX microanalysis detected higher percentages of Ti when the deposition were carried out with the inert gas and when the deposition process was carried out with reactive gas. The presence of titanium in iron matrix was also evidenced by the results of X-ray diffraction peaks that showed shifts in the network matrix. Given these results it can be said that the technique of magnetron sputtering deposition is feasible in the dispersion of nanoparticles of iron matrix in Ti.

Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface

Desenvolvimento de filtros cerâmicos impregnados com nanopartículas de prata para desinfecção de água potável

Brazil has vast amounts of hydric resources, whose quality has been deteriorating due to pollutant dumping. Household waste disposal is one of the main sources of water pollution, stimulating bacteria proliferation and introducing microorganisms, including those from fecal matter. Conventional water disinfection methods are a solution, but on the downside, they lead to the formation byproducts hazardous to human health. In this study, aiming to develop bactericidal filters for the disinfection of drinking water; silver nanoparticles were deposited on alumina foams through three routes: sputtering DC, dip coating and in situ chemical reduction of silver nitrate. The depositions were characterized through X-ray diffraction, scanning electron microscopy and EDS element mapping. The influence of the depositions on permeability and mechanical properties of the ceramic foams was assessed and, in sequence, a preliminary antibacterial efficiency analysis was carried out. Characterization results indicate that the chemical reduction routes were efficient in depositing homogeneously distributed silver particles and that the concentration of the metallic precursor salt affects size and morphology of the particles. The antibacterial efficiency analysis indicates that the chemical reduction filters have potential for water disinfection

Aplicação de nanopartículas de quitosana com potencial de adjuvante na produção de soro contra o venneno do escorpião Tityus serrulatus

In Brazil, several species of scorpions are known to cause accidents which can lead to death, which are mainly belonging to the genus Tityus. The scorpion Tityus serrulatus is the main responsible for more severe cases. Anti-scorpion serums are routinely produced by various institutions, despite their effectiveness, quality and action depends on how quickly treatment is started. Studies have been developed in the search for appropriate technologies to encapsulate and release recombinant or natives proteins capable of inducing antibody production. In this context, chitosan copolymer which can be obtained from the partial deacetylation of chitin or in some microorganisms and it is biocompatible and biodegradable has been widely used for this purpose. This study aimed to search for a system release from chitosan nanoparticles for peptide / protein of the venom of the scorpion T. serrulatus, able to provide a new model of immunization in animals, in order to obtain a potential novel polyclonal serum, anti-venom T. serrulatus. The chitosan nanoparticles were prepared by ionic gelation with polyanion tripolyphosphate (TPP). After standardizing the concentrations of TPP and chitosan was evaluated the efficiency of incorporation of bovine serum albumin (BSA) and scorpion venom, showed particle size compatible with the intended purpose. The particles showed adequate size around 200nm. The crosslinking was confirmed by absorption spectroscopy in the infrared. After verified the high encapsulation efficiency (EE) for acid bicinconínico method (BCA) protein assay and the particle size distribution, the success of the technique was proven and the potential for in vivo application of nanoparticles. The experimental animals were vaccinated and the antibodies measured by ELISA

Desenvolvimento e caracterização de nanocompósito de resina epóxi com nanopartículas de sílica para revestimento de dutos para transporte de petróleo

The use of polymer based coatings is a promising approach to reduce the corrosion problem in carbon steel pipes used for the transport of oil and gas in the oil industry. However, conventional polymer coatings offer limited properties, which often cannot meet design requirements for this type of application, particularly in regard to use temperature and wear resistance. Polymer nanocomposites are known to exhibit superior properties and, therefore, offer great potential for this type of application. Nevertheless, the degree of enhancement of a particular property is greatly dependent upon the matrix/nanoparticle material system used, the matrix/nanoparticle interfacial bonding and also the state of dispersion of the nanoparticle in the polymer matrix. The objective of the present research is to develop and characterize polymer based nanocomposites to be used as coatings in metallic pipelines for the transportation of oil and natural gas. Epoxy/SiO2 nanocomposites with nanoparticle contents of 2, 4, and 8 wt % were processed using a high-energy mill. Modifications of the SiO2 nanoparticles‟ surfaces with two different silane agents were carried out and their effect on the material properties were investigated. The state of dispersion of the materials processed was studied using Scanning and Transmission Electron Microscopy (SEM and TEM) micrographs. Thermogravimetric analysis (TG) were also conducted to determine the thermal stability of the nanocomposites. In addition, the processed nanocomposites were characterized by dynamic mechanical analysis (DMA) to investigate the effect of nanoparticles content and silane treatment on the viscoelastic properties and on the glass transition temperature. Finally, wear tests of the pin-on-disc type were carried out to determine the effects of the nanoparticles and the silane treatments studied. According to the results, the addition of SiO2 nanoparticles treated with silane increased the thermal stability, the storage modulus and Tg of the epoxy resin and decreased wear rate. This confirms that the interaction between the nanoparticles and the polymer chains plays a critical role on the properties of the nanocomposites

Estudo tribológico de biolubrificantes com adição de nanopartículas de óxidos (zinco e cobre)

Currently, vegetable oils have been studied for bio-lubricants base that fits the new environmental standards. Since, in a world full of finite natural resources, mineral oils bring consequences to the environment due to its low biodegradability and toxicity, also it is important to consider that synthetic oils have a high cost The aim of this work is to obtain a biolubricant additived with oxide nanoparticles (ZnO and CuO) for better resistance to friction and wear, which is not toxic to the environment and have better adherence under boundary lubrication. The methodology consisted in the synthesis of bio-lubricants (soybean and sunflower base) by epoxidation reaction. Then, some physical-chemical analysis in bio-lubricants are made to characterize theses lubricants, such as, density, acidity, iodine value, viscosity, viscosity index. Later, the lubricants were additive with nanoparticles. The tribological performance was evaluated by the equipment HFRR (High Frequency Reciprocating Rig) consisting of a wear test ball-plan type. The characterization of wear analysis was performed by SEM / EDS. The results show that bio-lubricants may be synthesized by reaction of epoxidation with good conversion. Tribological point of view, the epoxidized oils are more effective than lubricant additived with the oxide nanoparticles, they had lower coefficients of friction and better rate of film formation in the study. However, because they are environmentally friendly, bio-lubricants gain the relevant importance in tribological field

Propriedades magnéticas de nanopartículas de ferro em substratos antiferromagnéticos

The effect of finite size on the magnetic properties of ferromagnetic particles systems is a recurrent subject. One of the aspects wide investigated is the superparamagnetic limit where the temperature destroys the magnetic order of ferromagnetic small particles. Above the block temperature the thermal value of the magnetic moment of the particle vanishes, due to thermal fluctuations. The value of the blocking temperature diminishes when the size of the particle is reduced, reflecting the reduction of the anisotropy energy barrier between the uniform states along the uniaxial axis. The increasing demand for high density magnetic media has recently attracted great research interest in periodic arrangements of nanometric ferromagnetics particles, approach in the superparamagnetic limit. An interesting conjecture is the possibility of stabilization of the magnetic order of small ferromagnetic particles (F) by interface coupling with antiferromagnetic (AF) substrate. These F/AF systems may also help to elucidate some details of the effect of exchange bias, because the effect of interface roughness and the paper of domain walls, either in the substrate or the particle, are significantly reduced. We investigate the magnetic phases of small ferromagnetic particles on a antiferromagnetic substrate. We use a self-consistent local field method, incorporating the interface field and the dipole interaction between the spins of the ferromagnetic particle. Our results indicate that increasing the area of the interface favors the formation of the uniform state. Howere above a critical height value appears a state non-uniform is formed where the spins of in the particle s free surface are rotated with respect to the interface spins direction. We discuss the impact of the competition between the dipolar and interface field on the magnetic charge, that controls the field of flux leakage of the particle, and on the format of the hysteresis curves. Our results indicate that the liquid magnetic charge is not a monotonically increasing function of the height of the particle. The exchange bias may display anomalous features, induced for the dipolar field of the spins near the F/AF interface

Obtenção e caracterização de nanopartículas de quitosana

Chitosan nanoparticles have been used in several systems for the controlled release of drugs. The aim of this study was to obtain and characterize chitosan nanoparticles prepared by the method of coacervation / precipitation using sodium sulfate at different concentrations as the crosslinking agent. The characterization was done using zeta potential and small angle Xray scattering, SAXS. The dispersions of chitosan were obtained at pH 1 and pH = 3. The results of zeta potential at pH = 1 ranged from +64.8 to +29.27 mV and for pH = 3 they varied from +72.4 to +23.48 mV, indicating that the chain of chitosan is positively charged in acidic pH and the behavior of nanoparticles in terms of surface charge was independent of pH. However, the results indicated a dependence of particle size in relation to pH. This difference in behavior was explained by the influence of enthalpic and entropic components

Encapsulação de nanopartículas de magnetita em matriz de poli(metacrilato de metilacoácido metacrílico) por processo de polimerização em miniemulsão

Magnetic particles are systems with potential use in drug delivery systems, ferrofluids, and effluent treatment. In many situations, such as in biomedical applications, it is necessary to cover magnetic particles with an organic material, as polymers. In this work, magnetic particles were obtained through covering magnetite particles with poly(methyl methacrylate‐comethacrylic acid) via miniemulsion polymerization process. The resultant materials were characterized X‐ray diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), zeta potential (��) measurements and vibrating sample magnetometry (VSM). XRD results showed magnetite as the predominant cristalline phase in all samples and that cristallites had nanometric dimensions. Thermogravimetric analysis revealed an increase in polymer thermal stability as a result of magnetite encapsulation. TGA results showed also that the encapsulation efficiency was directly related to nanoparticles s hidrofobicity degree. VSM measurements showed that magnetic polymeric particles were superparamagnetic, so that they may be potentially used for magnetic (bio)separation

Síntese e imobilização de nanopartículas de ouro em fibras regeneradas via exaustão para potencial aplicação biomédica

The advancement of nanotechnology in the synthesis and characterisation of nanoparticles (NP's) has played an important role in the development of new technologies for various applications of nano-scale materials that have unique properties. The scientific development in the last decades in the field of nanotechnology has sought ceaselessly, the discovery of new materials for the most diverse applications, such as biomedical areas, chemical, optical, mechanical and textiles. The high bactericidal efficiency of metallic nanoparticles (Au and Ag), among other metals is well known, due to its ability to act in the DNA of fungi, viruses and bacteria, interrupting the process of cellular respiration, making them important means of study, in addition to its ability to protect UVA and UVB. The present work has as its main objective the implementation of an innovative method in the impregnation of nanoparticles of gold in textile substrate, functionalized with chitosan, by a dyeing process by exhaustion, with the control of temperature, time and velocity, thus obtaining microbial characteristics and UV protection. The exhausted substrates with colloidal solutions of NPAu's presented the colours, lilac and red (soybean knits) due to their surface plasmon peak around 520-540 nm. The NPAu's were synthesized chemically, using sodium citrate as a reducing agent and stabilizer. The material was previously cationised with chitosan, a natural polyelectrolyte, with the purpose of functionalising it to enhance the adsorption of colloid, at concentrations of 5, 7, 10 and 20 % of the bonding agent on the weight of the material (OWM). It was also observed, through an experimental design 23 , with 3 central points, which was the best process of exhaustion of the substrates, using the following factors: Time (min.), temperature (OC) and concentration of the colloid (%), having as a response to variable K/S (ABSORBÂNCIA/ Kubelka-Munk) of the fibres. Furthermore, it was evidenced as the best response, the following parameters: concentration 100%, temperature 70 ºC and time 30 minutes. The substrate with NPAu was characterised by XRD; thermal analysis using TGA; microstructural study using SEM/EDS and STEM, thus showing the NP on the surface of the substrate confirming the presence of the metal. The substrates showed higher washing fastness, antibacterial properties and UV radiation protection.

Micropartículas contendo nanopartículas de quitosana usando sulfato e genipina para liberação modificada da triancinolona: obtenção, caracterização e estudo em células tumorais

Chitosan is a polymer biocompatibility and biodegradability widely used in drug delivery systems. The co-crosslinking of chitosan with sodium sulfate and genipin, to form particulate systems is related of making them more resistant to acidic pH and to modulate the release kinetics for the oral route. Triamcinolone is a glucocorticoid with anti-inflammatory and immunosuppressive actions. The nanoparticles were prepared by co-crosslinking and characterized for particle size, PDI, zeta potential, crosslinking degree, encapsulation rate, morphology, infrared spectroscopy, thermal analysis, release kinetics and cells studies. The nanoparticles were prepared initially without genipin with sodium sulphate and the particles parameters were monitored in function of different ratio of drug / polymer, different concentrations of sodium sulfate and polysorbate 80 and the drip mode of crosslinkers on polymers. After optimizing conditions, the chosen system parameters without genipin included mean diameter of 312.20 ± 5.70 nm, PDI 0.342 ± 0.013 and zeta potential of 20.18 ± 2.28 mV. The genipin was introduced into the system analyzing different concentrations (0.5, 1.0 and 2.0 mM) and crosslinking times (3, 6, 12 and 24 h). Evaluating crosslinking time with genipin (0.5 mM) it was showed that varying the genipin reaction time the systems size ranged from 235.1 to 334.4 nm, the PDI from 0.321 to 0.392 and zeta potential 20.92 to 30.39 mV. The crosslinking degree that coud vary from 14 to 30 %. Nanoparticles without genipina, 6 h and 24 h crosslinking time were dried by spray-drying method. Analysis by scanning electron micrograph (SEM) revealed that the microparticles showed spherical morphology. The encapsulation rate was 75 ± 2.3 % using validated HPLC methodology. The infrared analysis showed chemical interactions between the components of the formulation. Thermal analysis showed that systems with a higher degree of crosslinking had a higher thermal stability. On release kinetics, increasing the degree of crosslinking was able to decrease the concentration and rate of release of triamcinolone. In studies with liver cancer cells (HepG2) and colon (HT-29), the microparticulate prepared with triamcinolone and 24 h of crosslinking with genipin showed a potential for antitumor activity in hepatic cell line HepG2. Therefore, a new delivery system for triamcinolone on polymeric nanoparticles of chitosan cocrosslinked with genipin and sodium sulfate was obtained with hepatic antitumor potential.

Síntese e caracterização de nanopartículas magnéticas de Co e Ni com aplicação em magneto hipertermia

Nanoparticles are importante for the study of new phenomena and for the development of new applications. Metallic magnetic nanoparticles like Cobalt and Nickel are important for their applications in nanoscience and nanotechnology. In this work, we report on the synthesis and characterization of Ni and Co nanoparticles. The nanoparticles were prepared by the modi- ed sol-gel method and were formed in the pore-network of the biopolymer quitosan. The reduction occurred in absence of H2 ux. The metallic particles and their monoxides have a face-centered- cubic structure. The metallic particles sizes ranged from 59 to 77 nm and from 19 to 50 nm for Ni and Co, respectively. Their monoxides chemically passivated the metallic cores, and after several weeks we have not observed further increase in oxidation. The synthesis method was tuned to obtain mainly the ferromagnetic phase. The system behaves like a core/shell structure with a ferromagnetic core and an antiferromagnetic shell. Exchange bias e ect was observed at temperatures below the Néel temperature. Both systems were submitted to an alternated magnetic eld and the heat released by the particles increased the temperature to 140°C in an interval of 5 min. Similar studies in samples dispersed in water increased the temperatures to 40-59°C, these results suggest that these materials are candidates for magnetic hyperthermia.