Development of amorphous carbon protective coatings on poly(vinyl)chloride

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

Characterization of a high oleic oil extracted from papaya (Carica papaya L.) seeds

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

Bioactive substance contents and antioxidant capacity of the lipid fraction of Annona crassiflora Mart. seeds

Annona crassiflora Mart. is a typical fruit of the Brazilian cerrado, considered to be a species of economic interest, mainly for its use in cooking, which is widespread among the inhabitants of that region, and can be found in many typical local dishes, especially sweets, jellies, liqueurs, soft drinks, ice creams and juices. Thus, the objective of this study was to determine the bioactive substance contents and the antioxidant capacity of the lipid fraction of A. crassiflora Mart. seeds in the interest of better identifying the quality of this raw material from the Brazilian cerrado. After the receipt of the fruits, the seeds were removed manually and, then, the lipid fraction was obtained by cold extraction with chloroform:methanol:water (2:1:0.8, v/v/v) and analyzed for the composition of phytosterols, tocopherols, fatty acids, total carotenoids, antioxidant activity and oxidative stability index. The lipid fraction showed significant quantity of bioactive substances, especially phytosterols, tocopherols and unsaturated fatty acids, as well as significant antioxidant capacity and oxidative stability, influenced by the content of phytosterols and the composition of fatty acids present in the analyzed fraction. © 2012 Elsevier B.V.

Physico-chemical characterization of seed oils extracted from oranges (Citrus sinensis)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Amorphous silicon carbonitride films modified by plasma immersion ion implantation

Amorphous silicon carbonitride (a-SiCN:H) films were deposited from hexamethyldisilazane (HMDSN) organic compounds via radio-frequency (RF) glow discharges. Afterwards the films were bombarded, from 15 to 60 min, with nitrogen ions using Plasma Immersion Ion Implantation (PIII) technique. X-ray photoelectron spectroscopy (XPS) showed that O-containing groups increased, while C-C and/or C-H groups decreased with treatment time. This result indicates chemical alterations of the polymeric films with the introduction of polar groups on the surface, which changes the surface wettability. In fact, the hydrophobic nature of a-SiCN:H films (contact angle of 100 degrees) was changed by nitrogen ion implantation and, and after aging in atmosphere air, all samples preserved the hydrophilic character (contact angle <80 degrees) independently of treatment time. The exposure of the films to oxygen plasma was performed to evaluate the etching rate, which dropped from 24% to 6% while the implantation time increased from 15 to 60 min. This data suggests that Pill increased the film structure strength, probably due to crosslinking enhancement of polymeric chains. Therefore, the treatment with nitrogen ions via Pill process was effective to modify the wettability and oxidation resistance of a-SiCN:H films. (C) 2014 Elsevier Ltd. All rights reserved.

Obtenção de compósitos nanoestruturados PSU/nanotubos de carbono pela técnica de eletrofiação

The nanostructured materials over the last decade have been increasing the variety of studies and research applications in many industries. From the understanding and manipulation of nanoscale is possible to obtain high-performance materials. One method, which has been very effective in obtaining of nanostructured composites, is the electrospinning, a technique that uses electrostatic forces to produce fibers from a polymer solution. By understanding and controlling of process conditions, such as solution viscosity, working distance, the velocity of the collector, applied voltage and others conditions, it is possible to obtain fibers in many different morphologies. This work aims to obtain nanostructured composites from polysulfone (PSU) a thermoplastic polymer with high oxidation resistance and good mechanical strength at high temperatures and carbon nanotubes (CNTs) that are excellent reinforcements for polymer materials, their mechanical resistance is greater than that of all known materials; using the electrospinning process via polymer solution. Were used polysulfone solutions, n,n-ndimetil acetamide (PSU / DMAc) and this same solution added of CNTs in order to obtain the nanofibers. In both cases were analyzed the effectiveness of the process from the analysis of fiber diameters, rheological behavior and infrared spectroscopy. The results obtained confirmed the efficiency of the electrospinning process to obtain polymeric fibers

The influence of B4C and MgB2 additions on the behavior of MgO-C bricks

Carbon-containing refractory materials have received great attention over the last years due to their importance in the steelmaking process. The oxidation of carbon present in refractory materials at temperatures above 500 degrees C is usually accompanied by the decrease of their mechanical strength and chemical resistance. Aiming to improve the oxidation resistance of carbon-oxide refractories, the use of materials known as antioxidants has been extensively studied. In this work we evaluated the performance of MgB2 and B4C antioxidants when incorporated into MgO-C bricks. We observed that the co-addition of metallic antioxidants and B4C or MgB2 leads to refractory bricks with enhanced hot modulus of rupture and resistance against oxidation and slag corrosion. However, the excessive addition of these antioxidants could impair the performance of the obtained bricks. Thus, when determining the optimum concentration of MgB2 and B4C to be added into MgO-C refractories, one must take into consideration this behavior. (c) 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Development and characterization of non-oxide ceramic composites for mechanical and tribological applications

The main reasons for the attention focused on ceramics as possible structural materials are their wear resistance and the ability to operate with limited oxidation and ablation at temperatures above 2000°C. Hence, this work is devoted to the study of two classes of materials which can satisfy these requirements: silicon carbide -based ceramics (SiC) for wear applications and borides and carbides of transition metals for ultra-high temperatures applications (UHTCs). SiC-based materials: Silicon carbide is a hard ceramic, which finds applications in many industrial sectors, from heat production, to automotive engineering and metals processing. In view of new fields of uses, SiC-based ceramics were produced with addition of 10-30 vol% of MoSi2, in order to obtain electro conductive ceramics. MoSi2, indeed, is an intermetallic compound which possesses high temperature oxidation resistance, high electrical conductivity (21·10-6 Ω·cm), relatively low density (6.31 g/cm3), high melting point (2030°C) and high stiffness (440 GPa). The SiC-based ceramics were hot pressed at 1900°C with addition of Al2O3-Y2O3 or Y2O3-AlN as sintering additives. The microstructure of the composites and of the reference materials, SiC and MoSi2, were studied by means of conventional analytical techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (SEM-EDS). The composites showed a homogeneous microstructure, with good dispersion of the secondary phases and low residual porosity. The following thermo-mechanical properties of the SiC-based materials were measured: Vickers hardness (HV), Young’s modulus (E), fracture toughness (KIc) and room to high temperature flexural strength (σ). The mechanical properties of the composites were compared to those of two monolithic SiC and MoSi2 materials and resulted in a higher stiffness, fracture toughness and slightly higher flexural resistance. Tribological tests were also performed in two configurations disco-on-pin and slideron cylinder, aiming at studying the wear behaviour of SiC-MoSi2 composites with Al2O3 as counterfacing materials. The tests pointed out that the addition of MoSi2 was detrimental owing to a lower hardness in comparison with the pure SiC matrix. On the contrary, electrical measurements revealed that the addition of 30 vol% of MoSi2, rendered the composite electroconductive, lowering the electrical resistance of three orders of magnitude. Ultra High Temperature Ceramics: Carbides, borides and nitrides of transition metals (Ti, Zr, Hf, Ta, Nb, Mo) possess very high melting points and interesting engineering properties, such as high hardness (20-25 GPa), high stiffness (400-500 GPa), flexural strengths which remain unaltered from room temperature to 1500°C and excellent corrosion resistance in aggressive environment. All these properties place the UHTCs as potential candidates for the development of manoeuvrable hypersonic flight vehicles with sharp leading edges. To this scope Zr- and Hf- carbide and boride materials were produced with addition of 5-20 vol% of MoSi2. This secondary phase enabled the achievement of full dense composites at temperature lower than 2000°C and without the application of pressure. Besides the conventional microstructure analyses XRD and SEM-EDS, transmission electron microscopy (TEM) was employed to explore the microstructure on a small length scale to disclose the effective densification mechanisms. A thorough literature analysis revealed that neither detailed TEM work nor reports on densification mechanisms are available for this class of materials, which however are essential to optimize the sintering aids utilized and the processing parameters applied. Microstructural analyses, along with thermodynamics and crystallographic considerations, led to disclose of the effective role of MoSi2 during sintering of Zrand Hf- carbides and borides. Among the investigated mechanical properties (HV, E, KIc, σ from room temperature to 1500°C), the high temperature flexural strength was improved due to the protective and sealing effect of a silica-based glassy phase, especially for the borides. Nanoindentation tests were also performed on HfC-MoSi2 composites in order to extract hardness and elastic modulus of the single phases. Finally, arc jet tests on HfC- and HfB2-based composites confirmed the excellent oxidation behaviour of these materials under temperature exceeding 2000°C; no cracking or spallation occurred and the modified layer was only 80-90 μm thick.

Refratários magnesianos de panela de aciaria: redução da oxidação inicial, formação da fase espinélio MgAl2O4 e resistência ao dano por choque térmico

A campanha dos refratários magnesianos aplicados como revestimento de trabalho de panelas de aciaria depende da soma de diversos fatores como resistência à corrosão, resistência à oxidação do carbono, estabilidade termomecânica, entre outros. A concepção microestrutural do refratário pode influenciar de forma benéfica ou deletéria no desempenho do refratário in situ. Nesta tese de doutorado os refratários magnesianos comerciais de panela de aciaria foram estudados sob três diferentes aspectos: redução da oxidação prematura do carbono, formação da fase espinélio de alumina e magnésio e resistência ao choque térmico e ao dano por choque térmico. Para reduzir a oxidação precoce do carbono foi desenvolvido um coating cerâmico que atua como uma eficiente barreira física, reduzindo o contato do oxigênio da atmosfera de aquecimento com o carbono presente no refratário. Como resultado reduz-se a oxidação prematura do carbono e eleva-se a vida útil do revestimento. A formação da fase espinélio de magnésia e alumina também influencia o desempenho termomecânico destes refratários, principalmente devido ao incremento volumétrico decorrente de sua formação. Nesta tese foram estudados os mecanismos de formação desta fase in situ, demonstrando experimentalmente o caminho preferencial que leva à formação desta fase mineralógica. O comportamento termomecânico dos refratários magnesianos foi determinado em função da resistência ao choque térmico (parâmetros R, R\'\'\') e quanto à resistência ao dano por choque térmico (parâmetro R\'\'\'\' e Rst). Estes parâmetros foram correlacionados com as respectivas características microestruturais destes refratários. Os resultados apresentados por esta tese de doutorado compõe uma importante ferramenta técnica para as indústrias produtoras de aço e de refratários por fornecer subsídio técnico e científico para fundamentar alterações em refratários já existentes e colaborar com o desenvolvimento de novos refratários de engenharia com elevado desempenho e maior vida útil.

Investigation of feasibility of utilizing available heat resistant materials for hypersonic leading edge applications.

"Volumes I through VIII are unclassified while volume IX is classified secret."

FT-Raman studies of a range of polyimides subjected to high-energy Radiations at room and elevated temperatures

A range of polyimides have been subjected to electron beam radiolysis at different temperatures. These polyimides were chemically designed to suit space applications, being either transparent or having groups which provide oxidation resistance. The structural changes that occur in the polyimides, when subjected to electron beam irradiation doses up to 18.5 MGy and up to temperatures close to their glass transition temperatures, were studied using FT-Raman spectroscopy. The range of polyimides studied included a series of perfluoropolyimides, a silicon-modified polyimide, and Ultem. The changes in the Raman peak intensities of the different groups indicated scission reactions involving the imide rings and ether linkages. (c) 2006 Wiley Periodicals, Inc.

Modification of the B2-type matrix of aluminide diffusion coatings on nickel-base superalloys-bulk aluminide analogues

Pack aluminide coating is a useful method for conferring oxidation resistance on nickel-base superalloys. Nominally, these coatings have a matrix composed of a Ni-Al based B2-type phase (commonly denoted as Β). However, following high-temperature exposure in oxidative envi-ronments, aluminum is depleted from the coating. Aluminum depletion in turn, leads to de-stabilization of the Β phase, resulting in the formation of a characteristic lathlike Β-derivative microstructure. This article presents a transmission electron microscopy study of the formation of the lathlike Β-derivative microstructure using bulk nickel aluminides as model alloys. In the bulk nickel aluminides, the lathlike microstructure has been found to correspond to two distinct components: L10-type martensite and a new Β derivative. The new Β derivative is characterized and the conditions associated with the presence of this feature are identified and compared with those leading to the formation of the L10 martensitic phase. © 1995 The Minerals, Metals & Material Society.

Microstructural study of aluminide surface coatings on single crystal nickel base superalloy substrates

Aluminide diffusion coatings are frequently employed to enhance the oxidation resistance of nickel base superalloys. However, there is a concern that the presence of an aluminide coating could influence the properties of the coated superalloy, especially in respect of fatigue behaviour. To understand the nature of the effects of surface coatings on the fatigue properties of superalloys, an understanding of microstructural development within both the coating and the coating/substrate interfacial zone during high temperature fatigue testing is necessary. This paper is concerned with microstructural changes in aluminide diffusion coatings on single crystal γ′ strengthened superalloy substrates during the course of high temperature fatigue testing. The 'edge on' transmission electron microscopy technique is employed to study cross-sections of two stage (aluminization plus diffusion treatment) coated superalloy samples. The paper examines the degradation of the coating produced by phase transformations induced by loss of aluminum from the coating and/or aging of the coating. Aluminum removal both by interdiffusion with the substrate and by oxidation of the coating surface is considered. Microstructural development in the portion of the substrate influenced by interdiffusion with the coating is also discussed.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.