Local drug delivery systems used in dental implants need to have uniform pore size distribution, adequate wettability, chemical composition, and biocompatibility. In the present work, titanium was treated by pulsed plasma electrolytic oxidation (PPEO), using 0.025 M sodium dihydrogen phosphate and 0.25 M calcium acetate as electrolytes, aiming at use in drug delivery systems. Pulse with Ton/Toff (width pulse/repetition time) of 50 μs/100 μs or 100 μs/50 μs, duty cycle 0,33, and 0.67, respectively, were used. After treatment, Ca/P ratio, wettability, crystalline phase, pore size and distribution were determined. The average pore size ranged from 1.5 μm to 2.3 μm according to the increase of energy supplied to the system. Pore distributions with lower dispersion were verified for the Ton/Toff condition of 50 μs /100 μs, using a current density of 30 mA/dm2. On the other hand, the 100 μs/50 μs conditions produce larger pores, but with greater dispersion. In general, conditions with lower currents (30 mA/dm2 and 38 mA/dm2) and Ton/Toff ratio = 50/100 were the most appropriate for use in drug delivery systems, due to their size and distribution of uniform pores, greater hydrophilicity, and Ca/P ratio close to desirable (1.67) was obtained.

RESUMO Cera de carnaúba é utilizada, com sucesso, em revestimento de frutos por formar uma barreira contra a perda de umidade, troca de gases e ação antimicrobiana. No presente trabalho, pretende-se melhorar esta última propriedade através do tratamento por plasma. Plasma produzido por descarga de barreira dielétrica (DBD), usando pulsos de voltagem de 45 kV, repetidos na frequência de 405 Hz, durante 9 min, foi aplicado diretamente sobre esporos de fungo Colletotrichum brevisporum (4x104 conidia.cm-1) ou sobre superfície dos revestimentos de cera. Verificou-se que o revestimento, após tratado por plasma, apresentou resistência antifúngica equivalente àquela existente quando aplicada diretamente sobre os fungos. Este resultado foi justificado com base na literatura, em que o tratamento com plasma em lipídios estimula a oxidação das cadeias lipídicas, resultando na formação de compostos carboxílicos, que possuem propriedades antimicrobianas.

ABSTRACT Carnauba wax is successfully used in fruit coating to produce a barrier against moisture loss, gas exchange and microbial action. The present study aims to improve this latter property by plasma treatment. Plasma produced by dielectric barrier discharge (DBD), using voltage pulses of 45 kV, repeated at the frequency of 405 Hz, for 9 min, was applied directly to spores of the fungus Colletotrichum brevisporum (4x104 conidia.cm-1) or on the surface of wax coatings. It was found that the coating, after being treated by plasma, presented antifungal resistance equivalent to that existing when applied directly to the fungi. This result was justified based on the literature, in which plasma treatment with lipids stimulates the oxidation of lipid chains, resulting in the formation of carboxylic compounds, which have antimicrobial properties.

RESUMO Sob condições ainda desconhecidas, cristais denominados de flor de sal, ou fleur de sel, como é comumente conhecido, pode ser formado na superfície de uma salmoura supersaturada durante a evaporação da água do mar nas salinas. Visando produzir flor de sal de uma maneira controlada e fazer melhor uso da solução residual de salinas, denominada de água-mãe, o presente trabalho foi proposto. O mecanismo de crescimento, morfologia, microestrutura e composição química dos sais obtidos foram estudados durante a evaporação da água-mãe, cuja densidade variou de 1,230 g/cm³ para 1,244 g/cm³, mantendo fixos o gradiente térmico e umidade relativa do ar. Análises quimicas, microestruturais e morfológicas foram usadas para caracterização. Cristais cúbicos ocos foram obtidos cujas concentrações iônicas foram dependents da densidade da solução. O tamanho e massa dos cristais também foram dependentes da densidade da solução. As amostras apresentaram fases contendo sulfatos como NaK3(SO4)2, Mg (SO4). (H2O) e K2SO4, cuja porcentagem aumentou levemente com o aumento da densidade. Mesmo assim, as porcentagens de NaCl foram acima de 90% para todas as amostras, mostrando que é possível extrair flor de sal de alta pureza a partir de uma solução residual hipersalina.

Abstract Up to now, plasma electrolytic oxidation (PEO) has been either produced direct current or ultra-low frequency (< 1 kHz) pulsed discharge using high concentration alkaline-silicate electrolytic (Na2SiO3 > 8 g.L-1 with presence of KOH). In order to contribute to these studies, the effect of current pulse width and time duration was investigated using diluted silicate electrolytic (Na2SiO3 2 g.L-1) and high pulse frequencies (> 1 kHz). The PEO process was performed on pure aluminum to try to explain how the phases composing the coatings are formed and distributed over the treatment time. For this, was made in situ monitoring using optical emission spectroscopy (OES) coupled with CCD camera. The crystalline phases evolution in the sample surface was investigated using grazing incidence X-ray diffraction (GIXRD). Regarding the evolution of ceramic phases, it is possible to verify that, internally, the predominant phase is rhombohedral α-Al2O3 but, superficially, the predominant phase is cubic γ-Al2O3. It was verified the presence of Si on the borders of the pores or in proximity to cracks, especially in the treatments with higher pulse width. SEM analysis shows a reduction of the superficial porosity and an increase in coating thickness with pulse width and treatment time.

ABSTRACT Direct current (DC) plasma nitriding offers some disadvantages, especially in parts with complex geometries, where the presence of edges is significant, such as gears, molds, and needle punched parts are strongly affected by this effect, leading to irregular formation of nitrided layers and high variation in surface hardness. To solve these problems two techniques were developed as alternatives, namely: pulsed plasma nitriding and cathodic cage nitriding. In this work, these three nitriding techniques were compared using AISI 1045 steel as substrate. Steel discs were nitrided with the purpose of evaluating the influence of these different plasma configurations on the characteristics of the nitrided layer. The treatments in the three techniques were carried out at the same pressure, temperature, time and gas atmosphere. The samples were characterized for the microstructure, microhardness and crystalline phases present. X-ray diffraction with grazing incidence was used to verify the order of the nitrites formed and to estimate the thickness of the single-phase layers. Differences between the configurations with respect to the occurrence of restriction rings, total thickness (xε +xγ') and relative (xε/xγ') compound layers were observed.

Electrical discharges in liquids are currently used to synthesize nanoparticles. The plasma-liquid interaction is complex, where parameters such as electric field, ion charges and other species present are important. In order to understand the mechanism of crystallization, mother liquor (saturated solution of NaCl, MgCl2 and KCl) was used to study the effectiveness and selectivity of the crystallization caused by the application of plasma. Discharge was applied with the solution at room temperature or during cooling. X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and chemical analysis was used to evaluate the structure and composition effects on crystal structure and composition. It was observed that the discharge induces selectively crystallization, and when compared to crystals obtained conventionally by cooling, were smaller and more uniform. We therefore confirm that plasma in liquid can also be used to selectively crystallize materials in atmospheric pressure, where the sizes of the crystals must be dependent on the parameters used.

High performance solar collectors are those with high selectivity surfaces, high solar radiation absorption and that do not thermally reemit to the external environment. Strategies to enhance this performance might involve surface porosity modification. In this work, a plasma treatment technique called plasma electrolytic oxidation (PEO) has been tested to produce porosity on aluminium surfaces in a controlled manner. The porosity control was made by varying the intensity, frequency and duty cycle of the applied voltage pulses. The aluminium sample was placed in a solution of 1 g/L Na2SiO3. Voltage of 500 V and current density of 0.17 A cm2 was applied between electrodes. Three duty cycles were used: 33.33%, 50.00% and 67.77%. After treatment, the size, number and distribution of pores were evaluated. These parameters were correlated with both surface reflectance and optical absorbance. It was possible to control the porosity by controlling the electrical parameters of the process. While the mean pore size was directly related to the duty cycle, the inverse occurred for the number of pores. Surface treated with duty cycle of 33.33% presented higher values of absorption for all wavelength range.

Titanium oxides such as rutile and anatase, are materials that stand out for exhibiting properties that act in biomedical and photocatalytic applications, among others. It is extreme importance to idealize new techniques that produce such compounds, being indispensable the improvement of characterizations for these materials. For this purpose, titanium comercially pure (CP) grade II cylindrical samples were oxidized ionically using titanium cage electric shields, oxidized at 350 ° C in 3 and 8 hours. Through Grazing Incidence X-ray Diffraction (GIXRD) analysis, was observed on the surface of the treated samples the formation of a TiO2 film with the anatase, rutile and brookite phases, the latter phase cited being difficult to produce in conventional thermochemical treatments. All samples treated showed a significant increase in wettability using distilled water. The higer value was for the sample with a 8 hours treatment time, in which this condition presented phases with greater intensity in the analysis of GIXRD

AbstractPolyester fabric samples – PET (poly (ethylene terephtalate)), were treated with oxygen plasma, in order to alter the hydrophilicity of such material. The process parameters: working pressure, current, tension and temperature were kept constant, varying only the treatment time. In order to evaluate the change caused on samples hydrophilicity, as well as the influence of the treatment time, the vertical wicking test was used. The samples were stored at standard temperature and pressure conditions, and their wettability were measured one day after the treatment and repeated after 30, 60 and 360 days, in order to check the stability of the effects produced. Scanning electron microscopy (SEM), Raman and ATR (Attenuated total reflection) spectroscopies were used to evaluate physical and chemical alterations on the samples surface. The results have shown a substantial improvement on the hydrophilicity of the treated samples compared to the non-treated sample.

Cylindrical samples of AISI 1020 steel were nitrided, using the techniques of conventional plasma nitriding and cathodic cage. In the latter, the samples are kept at floating potential, inside of a cage that works as a cathode and to shield the samples from the cathodic potential. A systematic study was conducted in order to evaluate the efficiency of this technique in the elimination of edge effect, in comparison with conventional plasma nitriding. In addition, another comparative study of the phases obtained using the conventional plasma nitriding and nitriding with cathodic cage was performed. Two metallic cages were used, one made of austenitic stainless AISI 316 and other one made of AISI 1020 steel, to prove the effect of deposition in nitriding with cathodic cage. The samples which were nitrided by this new technique had shown nitriding rates, crystalline phases, and microhardness, similar to those samples which were nitrided conventionally. However, it was possible to confirm the elimination of edge effect through the characterization by optical microscopy and by microhardness test along the samples surfaces. The samples were characterized by optical microscopy, microhardness tests and X-ray diffraction.

Objective: the main purpose of the study is to evaluate in vitro bioactivity in sodium alginate layers of hydroxyapatite disks. Methods: the hydroxyapatite disks were manufactured by successive pressing and sintering in an electric furnace. The sodium alginate layers were obtained by overpressure and a 5% sodium alginate aqueous solution. For the bioactivity assay, the study samples were soaked in simulated biological fluid. Characterization of the samples was conducted by scanning electron microscopy and energy dispersive X rays. Results: the bioactivity assay of hydroxyapatite samples with and without sodium alginate layers revealed the formation of precipitates rich in calcium and phosphorus. It was also found that an increase in the time of immersion in the simulated biological fluid brought about an increase in the size of agglomerates of apatite particles. Conclusions: experimental results show that hydroxyapatite is indeed bioactive, and that the sodium alginate layers of hydroxyapatite disks which were studied behave bioactively.

Objetivo: el propósito central de este trabajo es evaluar la bioactividad in vitro de capas de alginato de sodio en discos de hidroxiapatita. Métodos: los discos de hidroxiapatita fueron elaborados mediante procesos sucesivos de prensado y de sinterizado en un horno eléctrico. Las capas de alginato de sodio se obtuvieron empleando el método de sobrepresión y una disolución acuosa de alginato de sodio al 5 %. En el ensayo de bioactividad las muestras a estudiar fueron sumergidas en fluido biológico simulado. La caracterización de las muestras se realizó empleando microscopia electrónica de barrido y energía dispersiva de rayos X. Resultados: en las muestras de hidroxiapatita sometidas al ensayo de bioactividad, con y sin capas de alginato de sodio, se observó la formación de precipitados ricos en calcio y fósforo. Además, se determinó que con el aumento del tiempo de inmersión en el fluido biológico simulado se incrementan las dimensiones de los aglomerados formados por partículas apatíticas. Conclusiones: los resultados experimentales corroboran que la hidroxiapatita es bioactiva y demuestran que las capas estudiadas de alginato de sodio en discos de hidroxiapatita poseen un comportamiento bioactivo.

Objective: the main purpose of this study is to examine the potential use of Cuban hydroxyapatite (HA) disks as a controlled drug release system. These disks are manufactured by pressing, and sintered in electric furnaces without using pore-forming agents, with apparent porosities of 12, 20 and 40%, and doped by overpressure with a 5% sodium alginate aqueous solution and 55 ppm ceftazidime. Methods: a study was conducted of the relationship between penetration of the polymer and apparent porosity with the release of the drug. Results: it was shown that when infiltrated with the polymer encapsulating the drug, these disks may be used as a controlled release system. It was also found that apparent porosity and pore size influence polymer penetration and the mass of drug released. Conclusions: the release curves obtained show that the disks may be a potential drug-supporting material, capable of controlling the release of the remnant drug occluded by an overpressure doping method. The profile reveals that controlled release of the drug is completed in seven days.

Objetivo: el objetivo principal de este trabajo es estudiar la posibilidad de que sean empleados como sistema de liberación controlada de fármacos, discos de Hidroxiapatita (HA) cubana, fabricados por prensado y sinterizado en hornos eléctrico, sin el empleo de agentes formadores de poros, con porosidades aparentes de 12, 20 y 40%, que fueron dopados por sobre presión con una solución acuosa de alginato de sodio al 5 % y 55 ppm de ceftazidima. Métodos: se estudió la relación entre la penetración del polímero y la porosidad aparente con la liberación del fármaco. Resultados: se demostró que estos discos infiltrados con el polímero que encapsula el fármaco pueden ser utilizados como sistema de liberación controlada. Se demuestra que la porosidad aparente y el tamaño de los poros son influyentes en la penetración del polímero y la masa de fármaco liberado. Conclusiones: En las curvas de liberación obtenidas se observa que los discos pueden ser un potencial material para soportar medicamentos porque se evidencia como el material es capaz de controlar la liberación del medicamento remanente ocluido por un método de dopaje a sobre presión.El perfil indica que en un periodo de siete días se libera controladamente el medicamento.

Cathodic cage discharge was developed recently in order to eliminate phenomena as edge effect and overheating, which occurs during conventional processes. In this study, the effect of cage configuration in active species during the deposition process and optical properties of TiN film were studied. TiN compound was chosen because its optical properties are very sensitive to slight variations in microstructure and film thickness, becoming a good monitoring tool in fabrication process control. Cages were made of titanium and have different holes numbers and holes diameter. Electrical efficiency of the system and optical properties of TiN films were strongly influenced by experimental conditions. It was found that with more holes at the top of cage, deposition rate and crystallinity were higher, if compared to cages with a small number of holes at the top. On the other hand, the opposite behavior was observed when more holes were located at the sidewall of cage.