Made available in DSpace on 2017-07-21T20:42:39Z (GMT). No. of bitstreams: 1 Hudison.pdf: 7678712 bytes, checksum: 77d524c573ba60402f77fbda4e17c5e9 (MD5) Previous issue date: 2013-03-25 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / In the present study was investigated the API 5L X70 steel mechanical behavior through tensile and instrumented impact tests. Results from the instrumented Charpy impact test have allowed quantify the forces, energies and deflections of the specimens. It was used to obtain the fracture mechanics parameters such as the dynamic fracture toughness JId, the stress intensity factor for dynamic loading KId, as also range the ductile brittle transition temperature. Simultaneously was evaluated the mechanisms that induce to the delamination phenomenon as well as the investigation of their influence on the absorbed energy during the impact test. It was also analyzed the microtexture and mesotexture of different samples from the brittle, ductile and mixed regions from the ductile brittle transition temperature curve. Results have shown that the longitudinal direction was slightly superior mechanical properties when compared to the transverse direction. The dynamic fracture toughness JId was higher for the L-T specimen orientation when compared to the T-L orientation and it tends to increase with increasing temperature for both directions. The stress intensity factor values for dynamic loading was close to in both L-T and T-L orientations. The microtexture has revealed that deformation process from the impact test preserves some of its characteristics from the prior processing such as phase transformations and recrystallization components. While the mesotexture feature has shown higher energy values in the ductile brittle transition temperature curve, it is resulted from the formation of deformation substructure. Results obtained by scanning electron microscopy and light microscopy have shown that the main factors that may be contributing to the formation of crack-divider type delaminations are banded microstructure and elongated ferrite grains. While the microtexture from the edges delamination has shown that propagation mechanism is intergranular. Taylor factor mapping has shown that the mechanism responsible for the formation of delamination is accompanied by low plastic deformation. / No presente trabalho foi investigado o comportamento mecânico do aço API 5L X70 através de ensaios de tração e impacto instrumentado. O ensaio de impacto Charpy instrumentado permitiu quantificar as forças, energias e deflexões dos corpos de prova. Com a utilização destes dados foram obtidos parâmetros da mecânica da fratura, tais como, a tenacidade à fratura dinâmica JId, o fator de intensidade de tensão para carregamento dinâmico KId, além da faixa de valores da temperatura de transição dúctil frágil. Concomitantemente foram avaliados os mecanismos que contribuem na formação do fenômeno conhecido como delaminação, bem como a investigação de sua influência sobre a energia absorvida durante o ensaio de impacto. Foram também analisadas a microtextura e mesotextura de diferentes amostras retiradas da região frágil, dúctil e mista, da curva de transição dúctil frágil do material. Os resultados mostraram que o material possui propriedades mecânicas de impacto ligeiramente superiores na direção longitudinal à laminação comparado à direção transversal. Os valores encontrados para a tenacidade à fratura dinâmica JId são superiores para corpos de prova com orientação L-T quando comparados para a orientação T-L, e tendem a aumentar com o aumento da temperatura para ambas orientações. Os valores encontrados para o fator de intensidade de tensão para carregamento dinâmico foram próximos para ambas as orientações L-T e T-L. A microtextura revelou que após a deformação no ensaio de impacto o aço preserva algumas das características do seu histórico de processamento tais como componentes de transformações de fase e recristalização. Enquanto que o estudo da mesotextura mostrou que maiores valores de energia na curva de transição dúctil frágil resultam na formação de uma subestrutura de deformação. Resultados obtidos por microscopia eletrônica de varredura e microscopia ótica mostraram que os principais fatores que podem estar contribuindo para formação de delaminações do tipo trinca divisora são a microestrutura bandeada e grãos alongados de ferrita. Enquanto que a microtextura nas bordas da delaminação mostrou que o seu mecanismo de propagação é intergranular. O mapeamento do fator de Taylor mostrou que o mecanismo responsável pela formação da delaminação é acompanhado por pouca deformação plástica.

Com o decorrer dos anos o consumo de petróleo e seus derivados aumentou significativamente e com isso houve a necessidade de se investir em pesquisas para descobertas de novas jazidas de petróleo como o pré-sal. Porém, não apenas a localização dessas jazidas deve ser estudada, mas, também, sua forma de exploração. Essa exploração e extração, na maioria das vezes, se dão em ambientes altamente corrosivos e o transporte do produto extraído é realizado através de tubulações de aço de alta resistência e baixa liga (ARBL). Aços ARBL expostos a ambientes contendo H2S e CO2 (sour gas) sofrem corrosão generalizada que promovem a entrada de hidrogênio atômico no metal, podendo diminuir sua tenacidade e causar falha induzida pela presença de hidrogênio (Hydrogen Induced Cracking HIC), gerando falhas graves no material. Tais falhas podem ser desastrosas para o meio ambiente e para a sociedade. O objetivo deste trabalho é estudar a tenacidade, utilizando ensaio Charpy, de um tubo API 5L X65 sour após diferentes tempos de imersão em uma solução saturada com H2S. O eletrólito empregado foi a solução A (ácido acético contendo cloreto de sódio) da norma NACE TM0284 (2011), fazendo-se desaeração com injeção de N2, seguida de injeções de H2S. Os materiais foram submetidos a: ensaios de resistência a HIC segundo a norma NACE TM0284 (2011) e exames em microscópio óptico e eletrônico de varredura para caracterização microestrutural, de inclusões e trincas. As amostras foram submetidas a imersão em solução A durante 96h e 360h, sendo que, após doze dias do término da imersão, foram realizados os ensaios Charpy e exames fractográficos. Foram aplicados dois métodos: o de energia absorvida e o da expansão lateral, conforme recomendações da norma ASTM E23 (2012). As curvas obtidas, em função da temperatura de impacto, foram ajustadas pelo método da tangente hiperbólica. Esses procedimentos foram realizados nas duas seções do tubo (transversal e longitudinal) e permitiram a obtenção dos seguintes parâmetros: energias absorvidas e expansão lateral nos patamares superior e inferior e temperaturas de transição dúctil-frágil (TTDF) em suas diferentes definições, ou seja, TTDFEA, TTDFEA-DN, TTDFEA-FN, TTDFEL, TTDFEL-DN e TTDFEL-FN (identificação no item Lista de Abreviaturas e Siglas). No exame fractográfico observou-se que o material comportou-se conforme o previsto, ou seja, em temperaturas mais altas ocorreu fratura dúctil, em temperaturas próximas a TTDF obteve-se fratura mista e nas temperaturas mais baixas observou-se o aparecimento de fratura frágil. Os resultados mostraram que quanto maior o tempo de imersão na solução A, menor é a energia absorvida e a expansão lateral no patamar superior, o que pode ser explicado pelo (esperado) aumento do teor de hidrogênio em solução sólida com o tempo de imersão. Por sua vez, os resultados mostraram que há tendência à diminuição da temperatura de transição dúctil-frágil com o aumento do tempo de imersão, particularmente, as TTDFEA-DN e TTDFEL-DN das duas seções do tubo (longitudinal e transversal). Esse comportamento controverso, que pode ser denominado de tenacificação com o decorrer do tempo de imersão na solução A, foi explicado pelo aparecimento de trincas secundárias durante o impacto (Charpy). Isso indica uma limitação do ensaio Charpy para a avaliação precisa de materiais hidrogenados. / Over the years the consumption of crude oil and its derivatives increased significantly, creating the necessity to invest in research to discover new sources of pre-salt crude oil. However, not only the location of these deposits should be studied, but also its extraction. This exploration and extraction, in most cases, occur in highly corrosive environments and the transport of the extracted product is performed by high strength low alloy steel pipes (HSLA). HSLA steels exposed to environments containing CO2 and H2S (sour gas) suffer general corrosion that promotes the diffusion of atomic hydrogen into the metal structure, which may decrease its toughness and induce cracks by the presence of hydrogen (Hydrogen Induced Cracking - HIC), leading the material to severe failures. Such events can be disastrous for the environment and the society. The objective of this work is to study the toughness using Charpy Impact Tests on an API 5L X65 sour service steel pipe, submitted to different immersion times in a H2S saturated solution. The used electrolyte was the NACE TM0284 (2011) solution A (acetic acid containing sodium chloride), with deaeration by N2 injection followed by H2S injection. The materials were submitted to HIC resistance tests according to NACE TM0284 (2011) standard and examination by optical microscopy and scanning electron microscopy for microstructural inclusions and cracks characterization. The samples were immersed in the solution for 96h and 360h and after twelve days of immersion, Charpy tests and fracture analysis were performed. Two analytical methods were applied to Charpy tests results: the energy absorbed and lateral expansion, as recommended by the ASTM E23 (2012). The obtained curves, that are a function of impact temperature, were adjusted by the hyperbolic tangent method. This procedure was performed in two different orientations in the pipe (transverse and longitudinal) and allowed the determination of the following parameters: energy absorbed and lateral expansion in the upper and lower levels and ductile-to-brittle transition temperatures (DBTT) in its different definitions: DBTTAE, DBTTAE-DN, DBTTAE-FN, DBTTLE, DBTTLE-DN e DBTTLE-FN. Fracture analysis revealed that the material behaved as expected, meaning that at higher temperatures ductile fracture occurred, at temperatures near DBTT it was obtained a mixed fracture and at lower temperatures it was observed the presence of brittle fracture. Results showed that when the immersion time in the solution was higher, the energy absorbed in upper shelf decreases, and also lateral expansion in upper shelf decreases, which may be explained by the (expected) increase of hydrogen level in solid solution, induced by the immersion time. It was found that there is a tendency of the ductile-to-brittle transition temperature to be lower with the increase of immersion time, particularly the DBTTAE-DN and DBTTLE-DN of the two pipe sections (longitudinal and transversal). This controversial behavior, which may be defined as the toughening by the increase of immersion time in the solution A, was explained by the appearance of secondary cracks during impact test (Charpy). This indicates a limitation of the Charpy test for the accurate characterization of hydrogenated materials, concerning toughness.

Diversos critérios de tenacidade à fratura translaminar dinâmica foram determinados para o laminado híbrido metal-fibra TiGra, empregando-se conceitos e metodologias da Mecânica da Fratura Elástica Linear MFEL (fator-K) e da Mecânica da Fratura Elasto-Plástica MFEP (integral-J). Verificou-se que as tenacidades de iniciação elasto-plástica, Jid, e de carga máxima, Jmd, do TiGra são controladas pelo desenvolvimento, ou supressão de delaminações. Os resultados indicaram que o emprego deste material se justifica mais pela sua resistência à propagação de danos (caracterizada por Jmd) do que à iniciação da fratura dinâmica (por Jid). De modo geral, os requisitos de validade de Jid como verdadeira propriedade do material (JId) foram satisfeitos, embora para Jmd boa parte das restrições quanto ao tamanho mínimo do corpo-de-prova tenha sido violada. Mais freqüentemente, velocidades mais rápidas de impacto beneficiaram as tenacidades-J do TiGra, enquanto que temperaturas mais elevadas afetaram negativamente estas propriedades. Quanto à MFEL, a tenacidade KJd do TiGra foi beneficiada pelo incremento na taxa de carregamento sob temperaturas mais elevadas, enquanto que a tenacidade Kid foi negativamente afetada pela taxa de deformação em todas as temperaturas avaliadas. Temperaturas mais altas também degradaram as propriedades de tenacidade-K do TiGra. Em oposição às tenacidades-J, os critérios KJd e Kid não satisfizeram em absoluto os mais exigentes critérios de contenção de plasticidade estabelecidos pela MFEL, se comparados aos propostos pela MFEP. Por fim, o desempenho mecânico do laminado TiGra foi severamente comprometido quando do cômputo da densidade específica para a determinação das tenacidades J e K por unidade de massa, sendo nesta ocasião o laminado híbrido facilmente superado por vários laminados convencionais da classe dos Carbono-Epóxi. / Several dynamic translaminar fracture toughness criteria have been determined for TiGr hybrid fiber-metal laminate through Linear Elastic (K-factor) and Elastic-Plastic (J-integral) Fracture Mechanics (LEFM and EPFM, respectively) concepts and methodologies. Instrumented Charpy impact testing was carried out over a wide range of temperatures under two loading rates. It has been discovered that the elastic-plastic initiation toughness, Jid, and the toughness at maximum load, Jmd, of TiGr are controlled by either delamination favoring or suppression. Impact tests revealed that the in-service use of TiGr must rely on its resistance to dynamic fracture propagation (as characterized by Jmd) rather than on fracture initiation (by Jid). In a broad sense, the requirements for Jid data validity as a material property (JId) were fulfilled, whereas many restrictive demands in regard to the minimum testpiece size were violated by the Jmd criterion. Generally, higher impact velocities were beneficial to TiGrs J-toughnesses, inasmuch as higher temperatures impaired these properties. Regarding the LEFM approach, KJd toughness of TiGr laminate was imparted by faster impacts at higher temperatures, whilst the strain rate negatively influenced the Kid toughness over the whole temperature range tested. Higher temperatures also degraded the K-toughness properties of TiGr hybrid laminate. Differently from J-toughnesses values, the KJd e Kid criteria did not satisfy at all the more stringent criteria set forth by the LEFM approach with regard to plastic constraint, as compared to those established by EPFM. Finally, the mechanical performance of TiGr laminate was overwhelmingly compromised as the materials specific gravity was taken in account to obtain K and J toughness values by unit weight, so that TiGr was by far exceeded in this regard by conventional Carbon/Epoxy composite laminates.

The thesis deals with the dependence of mechanical characteristics on the anisotropy of polymers Nylon 12 and Ultem 9085 made by a 3D printing technology Fused Deposition Modeling (FDM). The evaluation of the material characteristics was performed on the basis of tensile and non-instrumental impact tests. It was proven that the material characteristics are strongly dependent on anisotropy, i.e. on layer thickness and raster angle for both types of polymers.

This master’s thesis deals with influence of gas content in structure of polymer materials to mechanical properties. Test specimens were prepared by MuCell technology from polyphthalamide reinforced by 50 % of glass fiber content. The theorethical part of this thesis is focused on polymer materials with attention to polyamides and injection moulding technology. In the experimental part, the dependence between the characteristics obtained from the tensile test and the Charpy impact test on the amount of gas in the polymer is examined.

Physical aging of commercially produced polypropylene homopolymers Mosten was studied. The work is focused on monitoring the changes in physical properties of polymer in the time period 90 days from the date of preparation of the test specimen. The aging of polymers was realized at storage temperatures of 23 and 80 °C. The changes in crystallinity, yield strength, modulus, elongation and impact strength using DSC method, tensile tests and impact tests according to Charpy were monitored. Molecular weight distribution was determined by means of GPC at each polymer. Relationships between the changes in physical properties and polymer molecular weight were sought.

At present, structural health monitoring efforts focus primarily on the sensors and sensing systems for detecting instances and locations of damage through techniques such as X-ray, micro CT, acoustic emission, infrared thermography, lamb wave etc., which only detect cracks at relatively large length scales and rely heavily on sensors and sensing systems which are external to the material system. As an alternative to conventional commercially available SHM techniques, the current work explores processing-structure-property relationships starting from carbon nanotube (CNT) based nanocomposites to particulate composites with nanocomposite binder/matrix materials, i.e. hybrid particulate composites to investigate deformation and damage sensing capabilities of inherently sensing materials and structures through their piezoresistive (coupled electro-mechanical) response. Initial efforts focused on controlling the dispersion of CNTs and orientation of CNT filaments within nanocomposites under dielectrophoresis to guide design and fabrication process of nanocomposites by tuning CNT concentration, applied AC electric field intensity, frequency and exposure time. It is observed that a combination of exposure time to AC electric field and the AC field frequency are the key drivers of filament width and spacing and that the network for filament formation is much more efficient for pristine CNTs than for acid treated functionalized CNTs. With the knowledge obtained from controlling the morphological features, AC field-induced long range alignment of CNTs within bulk nanocomposites was scaled up to form structural test coupons. The morphology, electrical and mechanical properties of the coupons were investigated. The anisotropic piezoresistive response both for parallel and transverse to CNT alignment direction within bulk composite coupons under various loading conditions was obtained. It is observed that control of the CNT network allows for the establishment of percolation paths and piezoresistive response well below the nominal percolation threshold observed for random, so called well-dispersed CNT network distributions. The potential for use of such bulk nanocomposites in SHM applications to detect strain and microdamage accumulation is further demonstrated, underscoring the importance of microscale CNT distribution/orientation and network formation/disruption in governing the piezoresistive sensitivities. Finally, what may be the first experimental study in the literature is conducted for real-time embedded microscale strain and damage sensing in energetic materials by distributing the CNT sensing network throughout the binder phase of inert and mock energetic composites through piezoresistive response for SHM in energetic materials. The incorporation of CNTs into inert and mock energetic composites revealed promising self-diagnostic functionalities for in situ real-time SHM applications under quasi-static and low velocity impact loading for solid rocket propellants, detonators and munitions to reduce the stochastic nature of safety characterization and help in designing insult tolerant energetic materials. / Ph. D.

[pt] O objetivo deste trabalho foi avaliar as propriedades mecânicas, físicas e microestruturais de materiais compósitos cimentícios reforçados por fibras naturais e de laminados de bambu. O trabalho experimental foi direcionado para a determinação da tenacidade. Para se determinar a tenacidade foram utilizados três tipos de ensaios: impacto Charpy, impacto balístico e flexão em 3 pontos. Após os ensaios, a superfície de fratura dos corpos-de-prova foi analisada por microscopia eletrônica de varredura (MEV). Esta análise microestrutural serviu para determinar os modos de fratura e validar as hipóteses feitas nos modelos matemáticos utilizados. Foram usados modelos adaptados da literatura para a determinação da tenacidade e os valores teóricos obtidos foram confrontados com os experimentais. Determinou-se também através de modelos encontrados na literatura a tensão interfacial de todas as fibras utilizadas nesta pesquisa. Os modelos empregados para calcular a tenacidade e a tensão de adesão interfacial, se mostraram eficientes e válidos. Em segundo plano, porém não menos importante, ficou a determinação das propriedades térmicas dos materiais utilizados. Foram efetuados ensaios de condutividade térmica do compósito e ensaios termogravimétricos das fibras vegetais e do bambu. Os compósitos cimentícios foram reforçados por diferentes fibras naturais: polpa refinada de bambu (CPB), polpa de sisal (CPS), polpa de eucalipto (CPE), fibras curtas de sisal (CPFS) e wollastonita (CPW). As proporções das polpas de bambu, sisal e eucalipto utilizadas como reforço nas matrizes cimentícias foram de 8 por cento e 14 por cento em relação à massa do cimento, a da fibra curta de sisal (25 mm) foi de 3 por cento em relação ao volume e a da wollastonita foi de 11,5 por cento em relação à massa. Compóstios híbridos feitos com wollastonita e polpa de bambu (CPBW) foram também produzidos apenas variando a proporção da polpa de bambu em 8 por cento e 14 por cento e mantendo fixa a da wollastonita em 11,5 por cento. Como uma tentativa de se melhorar a resistência ao impacto, laminados CPB/AL foram também fabricados colando duas chapas de alumínio (liga 5052 H34) de espessura 0,8 mm em ambas às faces dos compósitos reforçados por fibra de bambu, formando assim compósitos sanduíche (CPBA). O bambu Moso (Phyllostachys heterocycla pubescens) com 5 anos de idade foi usado para fabricação dos laminados de bambu, sendo tratado com água fervida para a prevenção de ataques biológicos. Técnicas para a extração do laminado a partir de seu formato natural foram estudadas estabelecendo suas vantagens e desvantagens. Para o ensaio de impacto foram utilizados corpos-de-prova com dimensão nominal de 120 mm x 15 mm x 6 mm perfazendo um total de 18 corpos-de-prova. Para o de flexão foram realizados ensaios com uma lâmina simples de bambu (BL) e bambu laminado colado (BLC) com 3 camadas de lâminas dispostas ortogonalmente. Os resultados dos testes de impacto Charpy e flexão em 3 pontos comprovaram a boa tenacidade do bambu laminado quando submetido a cargas de impacto (42,54 kJ/m2) e a cargas estáticas (19,77 kJ/m2 para o laminado e 17,63 kJ/m2 para o laminado colado). Compósitos sanduíche constituídos de alumínio e laminados de bambu foram também fabricados. Estes foram analisados através de ensaios de impacto balísticos seguindo as recomendações da norma NIJ 0101.04. Observações no microscópico eletrônico de varredura foram realizadas para se analisar os mecanismos de falha dos laminados. / [en] The main objective of this work was to evaluate the mechanical, physical and microestructure properties of cementitious composite materials and bamboo laminates. The experimental program was focused on the determination of toughness. Three diferent types of tests were performed in order to establish it: Charpy impact, ballistic impact and three point bending test. After the tests, the fractured surface of the failed test specimens was observed using a Scanning Electron Microscope (SEM) to establish the failure mode. Mathematical models adapted from the available literature were used to determine the toughness from which the values were confronted to the ones obtained experimentally. It was also determined by mathematical models the interfacial bond stress of all fibers used in this research. The two models, used in the toughness and interfacial bond stress calculation, showed to be efficient, providing valid results. In second plan, but not less important, was the determination of the materials thermal properties. Thermal conductivity tests of the composites and thermogravimetry of the fibers and bamboo were performed. The cementitious composites were reinforced by different natural fibers: refined bamboo pulp (CPB), sisal pulp (CPS), eucalyptus pulp (CPE), short sisal fibers (CPFS) and wollastonite. The mass fraction of bamboo, sisal and eucalyptus pulp studied were 8 percent and 14 percent. For the wollastonite fiber the mass fraction studied was 11.5 percent and for the short sisal fiber a 3 percent volume fraction was studied. Hybrid composites made with wollastonite and bamboo pulp (CPBW) were also produced varying the bamboo fraction mass to 8 percent and 14 percent but keeping constant to 11.5 percent the wollastonite mass fraction. The slurry de-watering process was used in the production of all composites described before. To reduce the adverse effects of weathering on the cellulose fibers and to improve the impact load and flexural resistance of the composite, aluminum thin sheets were used to produce a sandwich composite lamina with the CPB, which was denominated as CPBA. Compound Adhesive gel from Otto Baumgart which is a type of epoxy was used to fix the aluminum sheets on the CPB. The use of aluminum has proved to give much higher impact resistance results when compared to the CPB ones. The 5 years old Moso bamboo (Phyllostachys heterocycla pubescens), which was previously treated in boiled water to eliminate biological agents, was used to produce the bamboo laminates. Techniques were developed to extract bamboo laminates from its natural form, establishing its advantages and disadvantages. For the Charpy impact test, a total of 18 specimens with nominal dimensions of 120 mm x 15 mm x 6 mm were tested. Laminated (BL) and 3 layer cross ply laminated bamboo (BLC) were tested in bending. A total of 9 specimens were tested per bamboo configuration. The BL specimens had nominal dimensions of 120 mm x 30 mm x 6 mm and the BLC were 120 mm x 30 mm x 17 mm. The results demonstrated the good toughness of bamboo laminates when subject to dynamic (42.54 kJ/m2) and to static load (19.77 kJ/m2 for the laminate and 17.63 kJ/m2 for the cross ply laminate). Aluminum thin sheets were again used to make sandwich composites, but now using the bamboo laminate (BLCA). The BLCA was tested using the ballistic impact test following the standard NIJ 0101.04. Analysis on the Scanning Eléctron Microscope (SEM) were performed in order to establish the laminate s failure mechanisms.

The diploma thesis is aimed to assesment of the influence of the specimen orientation during the Small Punch Tests (SPT). Steel ČSN 41 0214, or its equivalent steel RFe80, W.-Nr. 1.104 was chosen for experiments. Resulting records from SPT were evaluated using already known correlations which are reported in literature. The correlation values were compared with values obtained by the standard tests like Charpy impact test and tensile test. The influence of axial, radial and tangential test specimens orientation is discussed in relation to Ductile-to-Brittle fracture behaviour of the steel.

This thesis is focused on application samples with the inner insert used for Charpy impact test. This insert is welded to additional material by electron beam with pre-selected welded parameters. These parameters were chosen from data of performed experiments on homogenous welds. Resulting heterogenous weld was performed of evaluation of the microstructure, chemical composition and microhardness. Experimental materials were used austenitic steel 17 240 and ferritic steel 17 153 used on high-temperature applications.