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 das propriedades termofísicas com variação da expansibilidade de compósito desenvolvido com matriz PUR-NOP e carga funcional de argilomineral

In this study were conducted experimental procedures for determination of variation of the expandability of rigid polyurethane foam (PUR) from a natural oil polyol (NOP), specifically the Castor oil plant, Ricinus communis, pure and additions of the vermiculite in phase dispersed in different percentage within a range from 0% to 20%, mass replacement. From the information acquired, were defined the parameters for production of bodies of test, plates obtained through controlled expansion, with the final volume fixed. Initially, the plates were subjected to thermal performance tests and evaluated the temperature profiles, to later be extracted samples duly prepared in accordance with the conditions required for each test. Was proceeded then the measurement of the coefficient of thermal conductivity, volumetric capacity heat and thermal diffusivity. The findings values were compared with the results obtained in the tests of thermal performance, contributing to validation of the same. Ultimately, it was investigated the influence that changes in physical-chemical structure of the material had exerted on the variation of thermophysical quantities through gas pycnometry, scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectroscopy (EDXRF), infrared spectroscopy using Fourier transform (FTIR), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Based on the results obtained was possible to demonstrate that all load percentage analyzed promoted an increase in the potential expansion (PE) of the resin. In production of the plates, the composites with density near at the free expansion presented high contraction during the cure, being the of higher density adopted as definitive standard. In the thermal performance tests, the heating and cooling curves of the different composites had presented symmetry and values very close for lines of the temperature. The results obtained for the thermophysical properties of composites, showed little difference in respect of pure foam. The percentage of open pores and irregularities in the morphology of the composites were proportionate to the increment of vermiculite. In the interaction between the matrix and dispersed phase, there were no chemical transformations in the region of interface and new compounds were not generated. The composites of PUR-NOP and vermiculite presented thermal insulating properties near the foam pure and percentage significantly less plastic in its composition, to the formulation with 10% of load

Metalização mecânica de ZrO2 com Ti para brasagem ZrO2/Aço com ligas de adição sem metal ativo

Metal/ceramic interfaces using zirconia have dominated the industrial applications in the last decade, due to the high mechanical strength and fracture toughness of zirconia, especially at temperatures below 300 ºC. Also noteworthy is the good ionic conductivity in high temperatures of this component. In this work joining between ZrO2 Y-TZP and ZrO2 Mg-PSZ with austenitic stainless steel was studied. These joints were brazed at high-vacuum after mechanical metallization with Ti using filler alloys composed by Ag-Cu and Ag-Cu-Ni. The influence of the metallization, and the affinity between the different groups (ceramic / filler alloys) was evaluated, in order to achieve strong metal/ceramic joints. Evaluation of joints and interfaces, also the characterization of base materials was implemented using various techniques, such as: x-ray diffraction, leak test, three-point flexural test and scanning electron microscopy with chemical analysis. The microstructural analysis revealed physical and chemical bonds in the metal/ceramic interfaces, providing superior leak proof joints and stress cracking, in order to a good joint in all brazed samples. Precipitation zones and reaction layers with eutetic characteristics were observed between the steel and the filler metal

Modificação superficial do tecido 100% algodão tratado com plasma

The 100% cotton fabric (CO)* treated with plasma of methane CH4 has direct application in all areas that needs of aqueous solutions repellent material like coatings and uniforms applied biomedical, aeronautics, and automobile between others. 100% cotton fabric (CO) samples were treated by plasma with two differents atmosphere: Methane gas (CH4), treatment time was varied in 10 in 10 min. until 60 min., and mixture methane/argon (CH4/Ar), it was varied the proportion 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2 e 9:1, with treatment time of 30 minutes. In both, the fluxe was 5 sccm (second cubic centimeter), pressure 6 mbar, voltage 490 V and current 0,15A. The objective of work was measure the superficial tension of 100% CO then it treated with plasma, using contact angle measures of water and glycerol with the surface. The samples were tested after treatment, with 8 and 12 months to verify the superficial modification effects. It was verified an increase of hydrophobility with the Sessile drop values varied between 116,69º to 137,85º and it carried on after 12 months. The no treated samples shows contact angle equal 0º. OES analysis and Raman spectroscopy were accomplished. In the SEM analysis was verified oligomers. The plasma treatment is correct environmental, It turning greater than conventional treatments

Estudo do efeito do óxido de bário no comportamento de massas para porcelanato

In this work, it is proposed the study of the effect of barium oxide acting as synthetic flow in the behavior of masses for stoneware from the use of raw materials found in the deposits of minerals of the Rio Grande do Norte that it makes use of a great natural potential for the industrialization of the product. The porcelanato is a sophisticated product with excellent final properties being applied as ceramic coating in buildings of high standard of engineering. The raw materials selected for the development of the study had been two types of argilas, two types of feldspatos, dolomita, talco, barium carbonate and silica, being characterized by X-ray fluorescence, X-ray diffraction, granulometric analysis, dilatometric analysis and thermal analysis. Thus, it is intended to define four formulations using the cited raw materials that will be processed, conformed and sintered in the temperatures of 1150 °C, 1175 °C, 1200 °C, 1225 °C e 1250 °C. From the physical characterizations, chemical and morphologic of the formed formulations, the effect of barium oxide is determined in the physical and mechanical properties of the studied system carrying water absorption tests, linear retraction, apparent porosity, apparent specific mass, compacting curve, flexural strength and microstructural analysis by XRD and SEM. After analyzing the results, indicated that barium oxide acts as a flux of high temperature and as the ordering of structure, where the embedded glass phase has the nucleating effect phase potassium silico-aluminum reacting with free silica which together with the high content of potassium concentrated form a new crystalline phase called microcline. The masses studied with the addition of barium oxide present physical-mechanical properties highly satisfactory in reduced firing temperatures, which implies a saving in energy given off in the production and increased productivity

Produção de grês porcelanato a partir de matérias-primas do estado da Bahia

The State Bahia, Brazil, presents different geological sites it with a very expressive variety minerals. It is situated among the very important States which produces minerals for industries, such as pointed aggregate, ornamentals stones and ceramics raw materials. Nowadays only four companies producting ceramics tiles. Porcelainized stoneware tiles is one of the noblest ceramics, depicting low water absorption (typically below of 0,5%), in addition to excellent staining resistance and mechanical strength. The present work aims at investigating the potential of local raw materials for the production of porcelainized stoneware tiles. For this purpose, these materials were characterized by X-ray fluorescence, X-ray diffraction, particle size analysis, thermal gravimetric analysis, thermal differential analysis and dilatometric analysis. Admixtures containing different compositions were prepared and fired at four temperatures, 1100 ºC, 1150 ºC, 1200 ºC and 1250 ºC with isotherm for 60 minute and heathing rate of 5 oC/min. After firing the samples, they were characterized by water absorption tests, linear retraction, analysis, apparent porosity, apparent specific mass, flexural strength, and microstructural analysis by X-ray diffraction and scanning electron microscopy . The results revealed three ceramics with porcelainized stoneware tiles characteristics and porcelain tile will be produce from raw materials originated in the State of Bahia

Avaliação tribológica dos polímeros NBR, PTFE e PTFE gravitado em contato com aço AISI 52100

Low cost seals are made of NBR, Nitrile Butadiene Rubber, a family of unsaturated copolymers that is higher resistant to oils the more content of nitrile have in its composition, although lower its flexibility. In Petroleum Engineering, NBR seal wear can cause fluid leakage and environmental damages, promoting an increasing demand for academic knowledge about polymeric materials candidate to seals submitted to sliding contacts to metal surfaces. This investigation aimed to evaluate tribological responses of a commercial NBR, hardness 73 ± 5 Sh A, polytetrafluoroethylene (PTFE), hardness 60 ± 4 HRE and PTFE with graphite, 68 ± 6 HRE. The testings were performed on a sliding tribometer conceived to explore the tribological performance of stationary polymer plane coupons submitted to rotational cylinder contact surface of steel AISI 52100, 20 ± 1 HRC Hardness, under dry and lubricated (oil SAE 15W40) conditions. After screening testings, the normal load, relative velocity and sliding distance were 3.15 N, 0.8 m/s and 3.2 km, respectively. The temperatures were collected over distances of 3.0±0.5 mm and 750±50 mm far from the contact to evaluate the heating in this referential zone due to contact sliding friction by two thermocouples K type. The polymers were characterized through Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA). The wear mechanisms of the polymer surfaces were analyzed by Scanning Electron Microscopy (SEM) and EDS (Energy-Dispersive X-ray Spectroscopy). NBR referred to the higher values of heating, suggesting higher sliding friction. PTFE and PTFE with graphite showed lower heating, attributed to the delamination mechanism

Análise do comportamento mecânico de espumas cerâmicas a base de alumina obtidas pelo método da réplica

Ceramics with porous cellular structure, called ceramic foams, have a potential use in several applications, such as: thermal insulation, catalyst supports, filters, and others. Among these techniques to obtain porous ceramics the replication method is an important process. This method consists of impregnation of a sponge (usually polymer) with ceramic slurry, followed by a heat treatment, which will happen the decomposition of organic material and sintering the ceramic material, resulting in a ceramic structure which is a replica of impregnated sponge. Knowledge of the mechanical properties of these ceramics is important for these materials can be used commercially. Gibson and Ashby developed a mathematical model to describe the mechanical behavior of cellular solids. This model wasn´t for describing the ceramics behavior produced by the replica method, because it doesn´t consider the defects from this type of processing. In this study were researched mechanical behavior of porous alumina ceramics obtained by the replica method and proposed modifications to the model of Gibson and Ashby to accommodate this material. The polymer sponge used in processing was characterized by thermogravimetric analysis and scanning electron microscopy. The materials obtained after sintering were characterized by mechanical strength tests on 4-point bending and compression, density and porosity and by scanning electron microscopy. From these results it was evaluated the mechanical strength behavior compared to Gibson and Ashby model for solid cellular structure and was proposed a correction of this model through a factor related to struts integrity degree, which consider fissures present in the structure of these materials besides defects geometry within the struts

Biomecânica e otimização topológica com H-adaptatividade em implantes dentários nitretados a plasma em cátodo oco

In recent years there has been a significant growth in technologies that modify implant surfaces, reducing healing time and allowing their successful use in areas with low bone density. One of the most widely used techniques is plasma nitration, applied with excellent results in titanium and its alloys, with greater frequency in the manufacture of hip, ankle and shoulder implants. However, its use in dental implants is very limited due to high process temperatures (between 700 C o and 800 C o ), resulting in distortions in these geometrically complex and highly precise components. The aim of the present study is to assess osseointegration and mechanical strength of grade II nitrided titanium samples, through configuration of hollow cathode discharge. Moreover, new formulations are proposed to determine the optimum structural topology of the dental implant under study, in order to perfect its shape, make it efficient, competitive and with high definition. In the nitriding process, the samples were treated at a temperature of 450 C o and pressure of 150 Pa , during 1 hour of treatment. This condition was selected because it obtains the best wettability results in previous studies, where different pressure, temperature and time conditions were systematized. The samples were characterized by X-ray diffraction, scanning electron microscope, roughness, microhardness and wettability. Biomechanical fatigue tests were then conducted. Finally, a formulation using the three dimensional structural topology optimization method was proposed, in conjunction with an hadaptive refinement process. The results showed that plasma nitriding, using the hollow cathode discharge technique, caused changes in the surface texture of test specimens, increases surface roughness, wettability and microhardness when compared to the untreated sample. In the biomechanical fatigue test, the treated implant showed no flaws, after five million cycles, at a maximum fatigue load of 84.46 N. The results of the topological optimization process showed well-defined optimized layouts of the dental implant, with a clear distribution of material and a defined edge

Mecanismos de desgaste, história térmica e ciclo de vida de componentes de um motor de combustão interna de aeromodelo

We developed an assay methodology that considered the temperature variation and the scanning electron microscopy as a method to quantify and characterize respectively the consumption evolution in three 46 LA machines, with internal combustion and two-stroke engines, 7.64 cm3 cylinder capacity, 23.0 millimeters diameter and 18.4 millimeters course, RPM service from 2.000 to 16.000 rpm, 1.2 HP power, and 272 grams weight. The investigated engines components were: (1) head of the engine (Al-Si alloy), (2) piston (Al-Si alloy) and (3) piston pin (AISI 52100 steel). The assays were carried out on a desktop; engines 1 and 2 were assayed with no load, whereas in two assays of engine 3 we added a fan with wind speed that varied from 8.10 m/s to 11.92 m/s, in order to identify and compare the engine dynamic behavior as related to the engines assayed with no load. The temperatures of the engine s surface and surroundings were measured by two type K thermopairs connected to the assay device and registered in a microcomputer with data recording and parameters control and monitoring software, throughout the assays. The consumed surface of the components was analyzed by scanning electron microscopy (SEM) and microanalysis-EDS. The study was complemented with shape deformation and mass measurement assays. The temperature variation was associated with the oxides morphology and the consumption mechanisms were discussed based on the relation between the thermal mechanical effects and the responses of the materials characterization

Obtenção de compósitos cerâmicos reforçados com carbetos refratários a partir de precursores poliméricos

In this work, were produced ceramic matrix composites based in SiCxOy e Al2O3 reinforced with NbC, by hydrosilylation reaction between D4Vi and poly(methylhydrosiloxane) mixtured with Al2O3 as inert filler, Nb and Al as reactive filler. After the mixture and compactation at 80ºC (warm pressing), the samples were pyrolised at 1200 and 1400ºC and infiltred with ICZ and LZSA respectively, and thermically, physical and structurally characterized by X-ray diffraction, density and porosity, flexural mechanical strength and fracture surface by scanning electron microscopy. The yield ceramic obtained after pyrolysis for studied composition at 1200ºC was 95%. The obtained phases had been identified as being Al3Nb, NbSi2 and NbC. The composite material presented apparent porosity varying of 15 up to 32% and mechanical flexural strenght of 32 up to 37,5MPa. After the fracture surface analysis, were observed a phases homogeneous dispersion, with some domains of amorphous and crystalline aspect. The samples that were submitted the infiltration cycle presented a layer next the surface with reduced pores number in relation to the total volume

Obtenção de pós de Nb a partir da redução aluminotérmica com ignição por plasma

The aluminothermic reduction consists in an exothermic reaction between a metallic oxide and aluminum to produce the metal and the scum. The extracted melted metal of that reaction usually comes mixed with particles of Al2O3 resulting of the reduction, needing of subsequent refine to eliminate the residual impure as well as to eliminate porosities. Seeking to obtain a product in powder form with nanometric size or even submicrometric, the conventional heat source of the reaction aluminothermic , where a resistor is used (ignitor) as ignition source was substituted, for the plasma, that acts more efficient way in each particle of the sample. In that work it was used as metallic oxide the niobium pentoxide (Nb2O5) for the exothermal reaction Nb2O5 + Al. Amounts stoichiometric, substoichiometric and superestoichiometric of aluminum were used. The Nb2O5 powder was mixed with aluminum powder and milled in planetarium of high energy for a period of 6 hours. Those powders were immerged in plasm that acts in a punctual way in each particle, transfering heat, so that the reaction can be initiate and spread integrally for the whole volume of the particle. The mixture of Nb2O5 + Al was characterized through the particle size analysis by laser and X-ray diffraction (DRX) and the obtained product of reaction was characterized using the electronic microscopy of sweeping (MEV) and the formed phases were analyzed by DRX. Niobium powders with inferior sizes to 1 mm were obtained by that method. It is noticed, through the analysis of the obtained results, that is possible to accomplish the aluminothermic reduction process by plasma ignition with final particles with inferior sizes to the original oxide

Mecanismos de desgaste de poliuretano em ensaios de microabrasão

Wear mechanisms and thermal history of two non-conforming sliding surfaces was investigated in laboratory. A micro-abrasion testing setup was used but the traditional rotative sphere method was substituted by a cylindrical surface of revolution which included seven sharp angles varying between 15o to 180o. The micro-abrasion tests lead to the investigation on the polyurethane response at different contact pressures. For these turned counterfaces with and without heat treatment. Normal load and sliding speeds were changed. The sliding distance was fixed at 5 km in each test. The room and contact temperatures were measured during the tests. The polyurethane was characterized using tensile testing, hardness Shore A measurement, Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and Thermomechanical Analyze (TMA). The Vickers micro-hardness of the steel was measured before and after the heat treatment and the metallographic characterization was also carried out. Worn surface of polyurethane was analysed using Scanning Electron Microscope (SEM) and EDS (Electron Diffraction Scanning) microanalyses. Single pass scratch testing in polyurethane using indenters with different contact angles was also carried out. The scar morphology of the wear, the wear mechanism and the thermal response were analyzed in order to correlate the conditions imposed by the pressure-velocity pair to the materials in contact. Eight different wear mechanisms were identified on the polyurethane surface. It was found correlation between the temperature variation and the wear scar morphology.

Redução carbotérmica de TiO2 por descarga em cátodo oco

In this study we used the plasma as a source of energy in the process of carbothermic reduction of rutile ore (TiO2). The rutile and graphite powders were milled for 15 h and placed in a hollow cathode discharge produced by in order to obtain titanium carbonitride directly from the reaction, was verified the influence of processing parameters of plasma temperature and time in the synthesis of TiCN. The reaction was carried out at 600, 700 and 800˚C for 3 to 4 hours in an atmosphere of nitrogen and argon. During all reactions was monitored by plasma technique of optical emission spectroscopy (EEO) to check the active species present in the process of carbothermal reduction of TiO2. The powder obtained after the reactions were characterized by the techniques of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The technique of EEO were detected in all reactions the spectra CO and NO, and these gas-phase resulting from the reduction of TiO2. The results of X-ray diffraction confirmed the reduction, where for all conditions studied there was evidence of early reduction of TiO2 through the emergence of intermediate oxides. In the samples reduced at 600 and 700˚C, there was only the phase Ti6O11, those reduced to 800˚C appeared Ti5O9 phases, and Ti6O11 Ti7O13, confirming that the carbothermal reduction in plasma, a reduction of the ore rutile (TiO2) in a series of intermediate titanium oxide (TinO2n-1) where n varies between 5 and 10

Estudo comparativo das propriedades mecânicas em compósitos da fibra modal e poliester

In the present work, three composites with distinct reinforcements (polyester, modal e polyester + modal), all if a unsaturated orthophthalic polyester resin as matrix were used, in order to conduct a comparative study by mechanical tests and water absorption. The fibre mats were prepared in a mat preparatory by immersion developed in the Textile Engineering Laboratory. The composites were manufactured using a closed mould process by compression using an unsaturated orthophthalic polyester resin as matrix and 1% MEK (methyl ethyl ketone peroxide) as an initiator. In each composite twelve samples with the dimensions of 150x25x3 mm were cut randomly for the mechanical analysis (tension x extension, three points bending and water absorption and Scanning Electron Micsroscopy). The mechanical tests were carried out in the Laboratório de Metais e Ensaios Mecânicos UFRN . All the analyses were carried out according to the ASTM norms. The resultant samples from the mechanical analysis were subjected for the Scanning Electron Microscopy analysis. Based on the results obtained, it was observed that the reinforced composite with two fibres (modal + polyester) presented better results in comparison to the other two composites both in the tension/extension as well on the three point bending tests. In the water absorption test, it was possible to observe an equilibrium in the water absorption by the modal and polyester composite, due to the union of the two fibres. In the SEM images, the regions of rupture in the composites as well as the adsorption between the fiber and the matrix could be observed