Inibição à corrosão do aço AISI 1020, em meios ácido e salino, por tensoativos e substâncias nitrogenadas microemulsionados

Corrosion inhibition efficiency of saponified coconut oil (SCO) and sodium dodecilbenzene sulfonate (DBS) surfactants in AISI 1020 carbon steel was evaluated by electrochemical methods. These surfactants were also evaluated as microemulsion systems (SCO-ME and DBS-ME), of O/W type (water-rich microemulsion), in a Winsor IV region. They were obtained according to the following composition: 15% SCO, 15% butanol (30% Co-surfactant/Surfactant C/T), 10% organic phase (FO, kerosene) and 60% aqueous phase (FA). These systems were also used to solubilize the following nitrogenated substances: Diphenylcarbazide (DC), 2,4-dinitro-phenyl-thiosemicarbazide (TSC) and the mesoionic type compound 1,3,4-triazolium-2-thiolate (MI), that were investigated with the purpose of evaluating their anticorrosive effects. Comparative studies of carbon steel corrosion inhibition efficiencies of free DBS and DBS-ME, in brine and acidic media (0.5%), showed that DBS presents better inhibition results in acidic media (free DBS, 89% and DBS-ME, 93%). However, the values obtained for DBS in salted solution (72% free DBS and 77% DBS-ME) were similar to the ones observed for the SCO surfactant in brine (63% free SCO and 74% SCO-ME). Analysis of corrosion inhibition of the nitrogenated substances that were solubilized in the SCO-ME microemulsion system by the linear polarization method in brine (0.5% NaCl) showed that such compounds are very efficient an corrosion inhibitors [DC-ME-SCO (92%), TSC-ME-SCO (93%) and MI-ME-SCO (94%)]

Estudo de titanatos nanoestruturados obtidos por tratamento hidrotérmico de óxido de titânio em meio alcalino

TiTanate NanoTubes (TTNT) were synthesized by hydrothermal alkali treatment of TiO2 anatase followed by repeated washings with distinct degrees of proton exchange. TTNT samples with different sodium contents were characterized, as synthesized and after heattreatment (200-800ºC), by X-ray diffraction, scanning and transmission electron microscopy, electron diffraction, thermal analysis, nitrogen adsorption and spectroscopic techniques like FTIR and UV-Vis diffuse reflectance. It was demonstrated that TTNTs consist of trititanate structure with general formula NaxH2−xTi3O7·nH2O, retaining interlayer water in its multiwalled structure. The removal of sodium reduces the amount of water and contracts the interlayer space leading, combined with other factors, to increased specific surface area and mesopore volume. TTNTs are mesoporous materials with two main contributions: pores smaller than 10 nm due to the inner volume of nanotubes and larger pores within 5-60 nm attributed to the interparticles space. Chemical composition and crystal structure of TTNTs do not depend on the average crystal size of the precursor TiO2-anatase, but this parameter affects significantly the morphology and textural properties of the nanostructured product. Such dependence has been rationalized using a dissolution-recrystallization mechanism, which takes into account the dissolution rate of the starting anatase and its influence on the relative rates of growth and curving of intermediate nanosheets. The thermal stability of TTNT is defined by the sodium content and in a lower extent by the crystallinity of the starting anatase. It has been demonstrated that after losing interlayer water within the range 100-200ºC, TTNT transforms, at least partially, into an intermediate hexatitanate NaxH2−xTi6O13 still retaining the nanotubular morphology. Further thermal transformation of the nanostructured tri- and hexatitanates occurs at higher or lower temperature and follows different routes depending on the sodium content in the structure. At high sodium load (water washed samples) they sinter and grow towards bigger crystals of Na2Ti3O7 and Na2Ti6O13 in the form of rods and ribbons. In contrast, protonated TTNTs evolve to nanotubes of TiO2(B), which easily convert to anatase nanorods above 400ºC. Besides hydroxyls and Lewis acidity typical of titanium oxides, TTNTs show a small contribution of protonic acidity capable of coordinating with pyridine at 150ºC, which is lost after calcination and conversion into anatase. The isoeletric point of TTNTs was measured within the range 2.5-4.0, indicating behavior of a weak acid. Despite displaying semiconductor characteristics exhibiting typical absorption in the UV-Vis spectrum with estimated bandgap energy slightly higher than that of its TiO2 precursor, TTNTs showed very low performance in the photocatalytic degradation of cationic and anionic dyes. It was concluded that the basic reason resides in its layered titanate structure, which in comparison with the TiO2 form would be more prone to the so undesired electron-hole pair recombination, thus inhibiting the photooxidation reactions. After calcination of the protonated TTNT into anatase nanorods, the photocatalytic activity improved but not to the same level as that exhibited by its precursor anatase

Degradação de compostos orgânicos voláteis usando o catalisador SBA-15 contendo titânio

The groundwater pollution arising due to fuel leaks gas stations has presented a problem aggravating. Increasingly studies related to environmental problems such accidents and seek to propose some solutions for the treatment of groundwater and soils that are contaminated by gasoline. This study evaluated the use of molecular sieve TiSBA-15 as a catalyst for the reaction of removing of volatile organic compounds, particularly benzene, toluene, ethylbenzene and xylenes, known as BTEX, one of the main pollutants found in groundwater. The catalyst was synthesized by the method post-synthesis techniques and characterized by XSD, TG/DTG, adsorption/desorption of N2, XRF-EDX, for checking the incorporation of titanium and formation of the structure of the catalyst. The reaction occurred with the presence of hydrogen peroxide, H2O2, in aqueous medium to form hydroxyl radicals, which are needed in the process of removal of BTEX compounds. The catalytic reaction was carried out for 5 hours at 60 °C, pH to 3.0, and analyzes of the compounds were made in a gas chromatograph with a flame detection means photoionization static headspace (HS-GC-PID). The catalytic tests have shown the efficacy of using this type of catalyst for the removal of these volatile organic compounds, having a removal rate of 90.60% in the range where the catalyst was studied TiSBA-15(5,0)

Estudo da eficácia do tensoativo sorbitano tween 80 veiculado em nanoemulsão contendo óleo de soja, como inibidor de corrosão

Nowadays, the use of chemicals that satisfactorily meet the needs of different sectors of the chemical industry is linked to the consumption of biodegradable materials. In this context, this work contemplated biotechnological aspects with the objective of developing a more environmentally-friendly corrosion inhibitor. In order to achieve this goal, nanoemulsion-type systems (NE) were obtained by varying the amount of Tween 80 (9 to 85 ppm) a sortitan surfactant named polyoxyethylene (20) monooleate. This NE-system was analyzed using phase diagrams in which the percentage of the oil phase (commercial soybean oil, codenamed as OS) was kept constant. By changing the amount of Tween 80, several polar NE-OS derived systems (O/W-type nanoemulsion) were obtained and characterized through light scattering, conductivity and pH, and further subjected to electrochemical studies. The interfacial behavior of these NE-OS derived systems (codenamed NE-OS1, S2, S3, S4 and S5) as corrosion inhibitors on carbon steel AISI 1020 in saline media (NaCl 3.5%) were evaluated by measurement of Open Circuit Potential (OCP), Polarization Curves (Tafel extrapolation method) and Electrochemical Impedance Spectroscopy (EIS). The analyzed NE-OS1 and NE-OS2 systems were found to be mixed inhibitors with quantitative efficacy (98.6% - 99.7%) for concentrations of Tween 80 ranging between 9 and 85 ppm. According to the EIS technique, maximum corrosion efficiency was observed for some tested NE-OS samples. Additionaly to the electrochemical studies, Analysis of Variance (ANOVA) and Principal Component Analysis (PCA) were used, characterization of the nanoemulsion tested systems and adsorption studies, respectively, which confirmed the results observed in the experimental analyses using diluted NE-OS samples in lower concentrations of Tween 80 (0.5 1.75 ppm)

Obtenção de novos sistemas nanoautoemulsificantes a partir do óleo das sementes de Azadirachta indica A Juss e suas aplicações como inibidores de corrosão

Corrosion is a natural process that causes progressive deterioration of materials, so, reducing the corrosive effects is a major objective of development of scientific studies. In this work, the efficiency of corrosion inhibition on a AISI 1018 carbon steel of the nanoemulsion system containing the oil of the seeds of Azadirachta indica A. Juss (SNEOAI) was evaluated by the techniques of linear polarization resistance (LPR) and weight loss (CPM), a instrumented cell. For that, hydroalcoholic extract of leaves of A. indica (EAI) was solubilized in a nanoemulsion system (SNEOAI) of which O/W system (rich in aqueous phase). This nanoemulsion system (tested in different concentrations) was obtained with oil from the seeds of this plant species (OAI) (oil phase), dodecylammonium chloride (DDAC) (surfactant), butanol (cosurfactant) and water, using 30 % of C/T (cosurfactant/surfactant), 0.5 % of oil phase and 69.5 % of aqueous phase, and characterized by surface tension, rheology and droplet sizes. This systems SNEOAI and SNEOAI-EAI (nanoemulsion containing hydroalcoholic extract - EAI) showed inhibition efficiencies in corrosive environment in saline (1 %), for the method of LPR with significant value of 70.58 % (300 ppm) to SNEOAI, 74.17 % (100 ppm) and 72.51 % (150 ppm) to SNEOAI-EAI. The best efficiencies inhibitions were observed for the method of CPM with 85.41 % for the SNEOAI (300 ppm) and 83.19 % SNEOAI-EAI (500 ppm). The results show that this formulation could be used commercially for use as a corrosion inhibitor, this research contributed to the biotechnological applicability of Azadirachta indica, considering the large use of this plant species rich in limonoids (tetranortriterpenoids), especially azadirachtin

Aplicação de sabões de ácidos graxos epoxidados como inibidores de corrosão em oleoduto

Corrosion usually occurs in pipelines, so that it is necessary to develop new surface treatments to control it. Surfactants have played an outstanding role in this field due to its capacity of adsorbing on metal surfaces, resulting in interfaces with structures that protect the metal at low surfactant concentrations. The appearance of new surfactants is a contribution to the area, as they increase the possibility of corrosion control at specific conditions that a particular oil field presents. The aim of this work is to synthesize the surfactants sodium 12 hydroxyocadecenoate (SAR), sodium 9,10-epoxy-12 hydroxyocadecanoate (SEAR), and sodium 9,10:12,13-diepoxy-octadecanoate (SEAL) and apply them as corrosion inhibitors, studying their action in environments with different salinities and at different temperatures. The conditions used in this work were chosen in order to reproduce oil field reality. The study of the micellization of these surfactants in the liquid-gas interface was carried out using surface tensiometry. It was observed that cmc increased as salt concentration was increased, and temperature and pH were decreased, while cmc decreased with the addition of two epoxy groups in the molecule. Using the values of cmc and the Gibbs equation, the values of Gibbs free energy of adsorption, area per adsorbed molecule, and surface excess were calculated. The surface excess increases as salt concentration and temperature decreases, increasing as pH is increased. The area per adsorbed molecule and the free energy of adsorption decrease with salt concentration, temperature, and pH increase. SAXS results showed that the addition of epoxy group in surfactant structure results in a decrease in the repulsion between the micelles, favoring the formation of more oblong micellar structures, ensuring a better efficiency of metal coverage. The increase in salt and surfactant concentrations provides an increase in micellar diameter. It was shown that the increase in temperature does not influence micellar structure, indicating thermal stability that is advantageous for use as corrosion inhibitor. The results of inhibition efficiency for the surfactants SEAR and SEAL were considered the best ones. Above cmc, adsorption occurred by the migration of micelles from the bulk of the solution to the metal surface, while at concentrations below cmc film formation must be due to the adsorption of semi-micellar and monomeric structures, certainly due to the presence of the epoxy group, which allows side interactions of the molecule with the metal surface. The metal resistance to corrosion presented values of 90% of efficiency. The application of Langmuir and Frumkin isotherms showed that the later gives a better description of adsorption because the model takes into account side interactions from the adsorbing molecules. Wettability results showed that micelle formation on the solid surface occurs at concentrations in the magnitude of 10-3 M, which isthe value found in the cmc study. This value also justifies the maximum efficiencies obtained for the measurements of corrosion resistance at this concentration. The values of contact angle as a function of time suggest that adsorption increases with time, due to the formation of micellar structures on metal surface

Obtenção e caracterização do sistema compósito alginato de sódio-dióxido de titânio em formas de pó e de membrana

The alginates are copolymers of 1→4-linked β-D-mannuronic acid (M) and α-Lguluronic acid (G) residues that are arranjed in a block structure along a linear chain. Titanium dioxide, TiO2, is a ceramic material and can exist in three distinct crystallography forms: anatase, brookite and rutile. composites of organic and inorganic materials have better properties than the components alone. Thus, this study aims to synthesize, characterize and analyze the composite NaAlg-TiO2 in the form of powder and film. The synthesis of composite powders was performed using the sol-gel process and obtain the composite film was performed using the slow evaporation process, then the composites were analyzed by infrared spectroscopy, fluorescence x ray, thermal analysis, attenuated total reflection (ATR), x ray diffraction and impedance spectroscopy. The X ray diffraction patterns of composite powders show that with increasing calcination temperature, there were no complete transition of rutile-anatase crystalline phase, since at all temperatures studied (300, 500, 700, 900 and 1100ºC) were observed peaks of anatase phase. Thermal analysis shows that at 400°C caused the decomposition of sodium alginate in sodium carbonate and above 600°C, we observe an exothermic peak related to the decomposition of sodium carbonate and in the presence of titanium dioxide becomes sodium titanate. The XRD results confirm the formation of sodium carbonate at 700ºC and the formation sodium titanate in the temperature range 900-1100ºC. The sodium titanate influenced the electrical properties of the material, because with increasing temperature there was a decrease in conductivity, probably due to the creation of Ti vacancies, since the sodium can induce the reduction of surface Ti4+ ions into Ti3+ species. The infrared spectra of the composites in the form of powder and film showed a small shift in the bands compared to the spectrum of pure alginate, indicating that these shifts, even small ones, have evidence of miscibility between the polymer and ceramic material

Modificação de superfícies de titânio tratadas por plasma de Ar + N2 + O2 visando aplicações biomédicas

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES

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.

Metodologia númerico-experimental para avaliação da espessura de filmes de nitreto de titânio obtidos por processamento a plasma

In recent decades, changes in the surface properties of materials have been used to improve their tribological characteristics. However, this improvement depends on the process, treatment time and, primarily, the thickness of this surface film layer. Physical vapor deposition (PVD) of titanium nitrate (TiN) has been used to increase the surface hardness of metallic materials. Thus, the aim of the present study was to propose a numerical-experimental method to assess the film thickness (l) of TiN deposited by PVD. To reach this objective, experimental results of hardness (H) assays were combined with a numerical simulation to study the behavior of this property as a function of maximum penetration depth of the indenter (hmax) into the film/substrate conjugate. Two methodologies were adopted to determine film thickness. The first consists of the numerical results of the H x hmax curve with the experimental curve obtained by the instrumental indentation test. This methodology was used successfully in a TiN-coated titanium (Ti) conjugate. A second strategy combined the numerical results of the Hv x hmax curve with Vickers experimental hardness data (Hv). This methodology was applied to a TiN-coated M2 tool steel conjugate. The mechanical properties of the materials studied were also determined in the present study. The thicknesses results obtained for the two conjugates were compatible with their experimental data.

Utilização do titâneo na confecção de estruturas metálicas em prótese parcial removível

Due to properties such as excellent biocompatibility, high resistance to corrosion and low specific weight, titanium has been considered a material of great interest for Dentistry. It has been widely used in implants and orthognathic surgeries. Recently, titanium has been seen as a feasible alternative for the fabrication of removable partial denture frameworks, either in pure titanium (99.75%) or in titanium alloy forms (Ti-6Al-4V; Ti-6A1-7Nb). Based on a review of the literature, this work studied the use of titanium for the fabrication of removable partial denture frameworks, focusing on its advantages and disadvantages as well as its characteristics. It was concluded that the use of titanium is a convenient option for partially edentulous arches rehabilitation with quite satisfactory and promising clinical results. However, the need for highly-equipped laboratories increases the cost, preventing its large scale use.

Utilização do titâneo na confecção de estruturas metálicas em prótese parcial removível

Due to properties such as excellent biocompatibility, high resistance to corrosion and low specific weight, titanium has been considered a material of great interest for Dentistry. It has been widely used in implants and orthognathic surgeries. Recently, titanium has been seen as a feasible alternative for the fabrication of removable partial denture frameworks, either in pure titanium (99.75%) or in titanium alloy forms (Ti-6Al-4V; Ti-6A1-7Nb). Based on a review of the literature, this work studied the use of titanium for the fabrication of removable partial denture frameworks, focusing on its advantages and disadvantages as well as its characteristics. It was concluded that the use of titanium is a convenient option for partially edentulous arches rehabilitation with quite satisfactory and promising clinical results. However, the need for highly-equipped laboratories increases the cost, preventing its large scale use.

Estudo das características físico-químicas e biológicas pela adesão de osteoblastos em superfícies de titânio modificadas pela nitretação em plasma

SILVA, J. S. P. Estudo das características físico-químicas e biológicas pela adesão de osteoblastos em superfícies de titânio modificadas pela nitretação em plasma. 2008. 119 f. Tese (Doutorado) - Faculdade de Medicina, Universidade de São Paulo. São Paulo, 2008.

Avaliação do estresse oxidativo induzido por superfícies de titânio

Commercially pure Titanium (cp Ti) is a material largely used in orthopedic and dental implants due to its biocompatibility properties. Changes in the surface of cp Ti can determine the functional response of the cells such as facilitating implant fixation and stabilization, and increased roughness of the surface has been shown to improve adhesion and cellular proliferation. Various surface modification methods have been developed to increase roughness, such as mechanical, chemical, electrochemical and plasma treatment. An argon plasma treatment generates a surface that has good mechanical proprieties without chemical composition modification. Besides the topography, biological responses to the implant contribute significantly to its success. Oxidative stress induced by the biomaterials is considered one of the major causes of implant failure. For this reason the oxidative potential of titanium surfaces subjected to plasma treatment was evaluated on this work. CHO-k1 cells were cultivated on smooth or roughed Ti disks, and after three days, the redox balance was investigated measuring reactive oxygen species (ROS) generation, total antioxidant capacity and biomarkers of ROS attack. The results showed cells grown on titanium surfaces are subjected to intracellular oxidative stress due to hydrogen peroxide generation. Titanium discs subjected to the plasma treatment induced less oxidative stress than the untreated ones, which resulted in improved cellular ability. Our data suggest that plasma treated titanium may be a more biocompatible biomaterial.

Efeito do tratamento térmico do titânio sobre a proliferação de células pré-osteoblásticas

Titanium is a biomaterial widely employed in biomedical applications (implants, prostheses, valves, stents). Several heat treatments are usually used in order to obtain physical properties required to different applications. This work studied the influence of the heat treatment on microstructure of commercial pure titanium, and their consequences in growth and proliferation of MC3T3-E1 cells. Discs of titanium were treated in different temperatures, and characterized by optical microscopy, image analysis, wettabillity, roughness, hardness and X-ray diffraction. After the heat treatment, significant modifications in these properties were observed. Pattern images of titanium, before and after the cell culture, were compared by overlapping to analyze the influence of microstructure in microstructure and preferences guidance cells. However, in general, titanium discs that showed a higher residual strength also presented an increase of cells numbers on surface