O presente estudo teve como objetivo avaliar as propriedades de dois compósitos convencionais [Charisma Diamond (CD) e Filtek Z250XT (FZ250XT)] e dois do tipo Bulk Fill [Aura Bulk Fill, (ABF) e Filtek Bulk Fill (FBF)] em função da profundidade de polimerização e modo de obtenção (O) dos espécimes submetidos ou não a tratamento térmico (TT, 170?C x 10 min)) e um protocolo de envelhecimento acelerado (C, 150000 ciclos, 14,7 N). Para a obtenção dos corpos de prova em forma de disco (10 mm diâmetro e 1 mm espessura) utilizou-se dois tipos de molde de poliéster (segmentado e não segmentado). Foram fotoativados (1000 mW/cm2 X 20 s) nas espessuras de 2 mm (convencionais) e 5 mm (Bulk Fill.). As propriedades avaliadas foram: Grau de conversão (GC), dureza (KHN) e resistência à flexão biaxial (RFB). A análise estatística do GC % para as resinas convencionais mostrou diferença no fator Condição (imediato 58,8 %, sem TT 24h 66,3 %, com TT 83,8 %), na interação Marca X Tratamento Térmico a CD com TT (88,1 %) > FZ250XT (79,6 %) mas nas outras condições foi semelhante. Quanto às resinas do tipo Bulk, a FBF (73,5 %) > ABF (71,8 %), o GC em função da profundidade diminuiu, os primeiros dois milímetros foram semelhantes 1 mm (77,0 %), 2 mm (77,4 %) > 3 mm ( 72,1 %) e 4 mm (70,8 %), semelhantes entre si, e o 5 mm obteve o menor GC (66,2 %). Comparado o 5 mm, a ABF (61,1 %) < FBF (71,4 %). No fator Condição o GC aumenta em 24 h (70,2 %) comparada com o imediato (61,7 %) e com o tratamento térmico aumenta ainda mais (86,2 %). Com o tratamento térmico, a FBF foi a que obteve o maior aumento (88,4 %), ABF (84,1 %), mas as duas sem tratamento térmico não apresentaram diferença significante ABF (69,9 %), FBF (70,5 %). Os valores de KHN tanto para as resinas convencionais como para as reinas do tipo Bulk Fill variaram em função da marca; resinas convencionais FZ250XT (64,8 KHN) > CD (50,8 KHN) e resinas do tipo Bulk Fill FBF (47,2 KHN) > ABF (33,1 KHN); em função da Forma de Obtenção, resinas convencionais Bloco-topo (61,7 KHN) < Fatia-topo (67,3 KHN), Bloco-base (54,0 KHN) > Fatia-base (48,2 KHN), e as resinas do tipo Bulk Fill Bloco-topo (44,5 KHN) < Fatia-topo (48,1 KHN), Bloco-base (38,0 KHN) > Fatia-base (29,9 KHN); e em função do Tratamento Térmico, resinas convencionais com TT (54,15 KHN) > sem TT (53,23 KHN) e resinas do tipo Bulk Fill com TT (44,4 KHN) > sem TT (35,9 KHN). Quanto à RFB, o fator Forma de Obtenção apresentou diferenças significativas para as quatro resinas; o Tratamento térmico aumentou à RFB nas 4 resinas estudadas, a porcentagem de aumento foi de 16,1 % para a resina CD, de 4,7 % para a FZ250XT, de 14,1 % para a ABF e de 28,3 % para a FBF. Com base nos resultados obtidos, pode-se concluir que: maior grau de conversão conduziu à maior resistência à flexão; O tratamento térmico conduziu a um aumento de todas as propriedades estudadas. A ciclagem mecânica, utilizada como protocolo de envelhecimento, permitiu a diferenciação dos materiais. / The aim of this study was to evaluate the properties of two conventional composites [Charisma Diamond (CD) e Filtek Z250XT (FZ250XT)] and two bulk fill composites Fill [Aura Bulk Fill, (ABF) e Filtek Bulk Fill (FBF)] regarding the depth of polymerization and the mode of acquisition (O) of the specimens which were submitted or not submitted to heat treatment (HT, 170 ?C x 10 min) and a protocol of accelerated aging (C, 150,000 cycles, 14.7 N). For the acquisition of the samples in disc format (10 mm in diameter and 1 mm in thickness) two different polyester molds were used (segmented and non-segmented). The samples were light cured in the thickness of 2 mm (conventional composites) and 5 mm (Bulk Fill composites). The properties evaluated were degree of conversion (DC %), hardness (KHN) and biaxial flexural strength (BFS). Statistical analyses of the DC % for the conventional composites showed differences for the factors Condition (immediate 58.8 % < without HT 24h 66.3 % < with HT 83.8 %), in the interaction Brand X Heat Treatment the group CD with HT (88.1 %) was higher than FZ250XT (79.6 %) but for all other conditions the results were similar. As for the Bulk Fill resins, the DC% for FBF (73.5 %) showed higher DC % when compared to ABF (71.8 %). The DC% in function of depth decreased: for the first two millimeters the results were similar: 1 mm (77.0 %) = 2 mm (77.4 %) > 3 mm (72.1 %) = 4 mm (70.8 %), and the 5 mm obtained the lowest DC % (66.2 %). Comparing the 5 mm level among brands, ABF (61.1 %) was lower than FBF (71.4 %). For the factor Condition the DC % increases in 24h (70.2 %) compared to immediate (61.7 %) and with the HT increases even more (86.2 %). With the HT FBF obtained the highest increase (88.4 %), ABF (84.1 %), but both without HT present no statistically significant difference: ABF (69.9 %), FBF (70.5 %). The KHN values for both the conventional composites and the bulk fill ones varied based on the brand; conventional composites: FZ250XT (64,8 KHN) > CD (50.8 KHN) and Bulk Fill resins: FBF (47,2 KHN) > ABF (33,1 KHN); for the mode of acquisition, conventional resins block-top (61.7 KHN) lower than slice-top (67.3KHN), block-base (54.0 KHN) higher than slice-base (48.2 KHN); the bulk fill resins presented the results block-top (44.5 KHN) lower than slice-top (48.1 KHN), block-base (38.0 KHN) higher than slice-base (29.9 KHN); and regarding the HT, conventional resins with HT (54.15 KHN) higher than no HT (53.23 KHN) and bulk fill resins with HT (44.4 KHN) higher than without HT (35.9 KHN). Regarding BFS the factor mean of acquisition presented statistically significant differences for the 4 composites; heat treatment increased the BFS for all resins tested. 16.1 % was the percentage of increase for the CD resin, 4.7 % for FZ250XT, 14.1 % for ABF and 28.3 % for FBF. Based on the results obtained it can be concluded that: the higher conversion rate led to higher flexural strength resistance; the heat treatment led to an increase of all properties evaluated. Mechanical cycling, used as aging protocol, permitted the differentiation of materials.

Das Trag- und Verbundverhalten textiler Bewehrungen wurde in den vergangen Jahren umfassend experimentell untersucht. Die dabei gewonnenen Erkenntnisse stützen sich jedoch fast ausschließlich auf einaxiale Beanspruchungszustände. Grundsätzlich können aus dem Vergleich von Versuchen an Rovings und an textilen Bewehrungsstrukturen Rückschlüsse auf den Einfluss der Quer- und Stützfäden und der verschiedenen Bindungstechniken auf das einaxiale Tragverhalten von Textilbeton getroffen werden. Offen bleibt jedoch, inwieweit sich die gefundenen Gesetzmäßigkeiten auf mehraxiale Beanspruchungssituationen übertragen lassen. Dadurch werden Fragen bezüglich des Tragverhaltens textiler Bewehrungen unter mehraxialen Zugbeanspruchungen aufgeworfen, welche die Motivation für die vorliegende Arbeit liefern. Die hierzu durchgeführten experimentellen Untersuchungen umfassen 84 Einzelversuche und wurden in einem speziell für zweiaxiale Zugbeanspruchungen entwickelten Versuchsaufbau durchgeführt. Als textile Bewehrungen kamen zwei verschiedene Gelegearten aus AR-Glas und Carbon zum Einsatz. Die Ergebnisse konnten die bisher ausschließlich an einaxialen Dehnkörpern gewonnenen Erkenntnisse über das Tragverhalten textiler Bewehrungen grundsätzlich bestätigen. Für den Übergang von Zustand I zum Zustand II konnte eine Abhängigkeit der Erstrissspannung vom Spannungsverhältnis nachgewiesen werden. Die Merkmale der Zustände IIa und IIb zeigen hingegen keine signifikante Abhängigkeit vom Verhältnis aus Längs- und Querzugspannung. Darüber hinaus haben offenbar durch Querzug induzierte bewehrungsparallele Risse keine maßgeblichen Auswirkungen auf das Verbundverhalten der Rovings in Längsrichtung. Eine wesentliche Erkenntnis aus den biaxialen Zugversuchen mit Carbon betrifft den Einfluss der Welligkeit. Es wurde deutlich, dass der Abbau der Welligkeit in beschichteten textilen Bewehrungen hochgradig lastabhängig ist. In zahlreichen Versuchen mit Carbon kam es innerhalb des Zustands IIb zu Delamination, einem bisher in diesem Umfang nicht beobachteten Effekt. Die Erkenntnisse hinsichtlich des Abbaus der Welligkeit wurden im Anschluss auf das Tragverhalten von AR-Glas übertragen und führten zu einer Neubewertung des bei AR-Glas beobachteten Steifigkeitsdefizits im Zustand IIb. Weiterhin wurde der Einfluss der Orientierung der Bewehrung unter einaxialer Beanspruchung an scheibenartigen Probekörpern untersucht. Es zeigte sich, dass die untersuchten Bewehrungen aus AR-Glas hinsichtlich der Tragfähigkeit bei schiefwinkliger Beanspruchung deutlich unempfindlicher reagieren als Bewehrungen aus Carbon. Für die Reduktion der effektiven Faserbruchspannungen wurde ein mathematisches Modell vorgestellt, welches eine getrennte Beschreibung der geometrischen Einflüsse sowie alle sonstigen, die Faserbruchspannung reduzierenden Effekte erlaubt. / The load bearing and bond behaviour of textile reinforcements has been comprehensively studied experimental in recent years. The findings are based almost exclusively on uniaxial loading. Generally, from the comparison of tests on rovings and fabrics conclusions can be drawn about the influence of transverse and supporting threads and different binding patterns on the uniaxial load-bearing behaviour. However, it remains open, to what extend the found principles are applicable to multi-axial loading situations. This raises questions about the load bearing behaviour under multi-axial tension loading, which provide motivation for this work. For the experimental studies on 84 specimens a specially developed test setup for biaxial tensile loading was used. Two different types of textile reinforcements made from AR-glass and carbon fibres were examined. The results generally approve the findings on the structural behaviour of textile reinforcements exclusively derived from uniaxial tests. A relationship between first cracking stress level and biaxial stress ratio has been found. The characteristics of the cracking phases and during stabilized cracking, however, show no significant dependencies on the ratio of longitudinal and transverse tensile stresses. Furthermore, parallel cracks induced by transverse tensile stresses have no significant impact on the bond behaviour of longitudinal rovings. An essential result from biaxial tensile tests with carbon is the strong influence of waviness. It became clear that the reduction of waviness in coated textile reinforcement is highly load-dependent. In numerous experiments with carbon reinforcement delamination occurred during stabilized cracking – an effect, that has been observed in this large scale for the first time. The findings regarding the reduction of the waviness were subsequently applied to AR-glass and led to a revaluation of the known stiffness deficit in the phase IIb. Furthermore, the influence of reinforcement orientation has been studied on discoidal specimens under uni-axial loading. It was found that the load bearing capacity of carbon reinforcement is much more sensible to load orientation than AR-glass. A mathematical model was presented, which allows the separate description of geometric factors and as well as all other effects that reduce the fibre tensile strength.

[pt] Um grande número de novos materiais geotécnicos foi desenvolvido baseado na adição de materiais fibrosos, sendo incorporados como elementos de reforço. A técnica de solo reforçado pode ser representada pela produção e aplicação, não somente de fibra natural, mas também de fibras sintéticas e poliméricas. Estudos anteriores de solos reforçados com fibras de polipropileno têm mostrado melhora significativa das propriedades mecânicas dos solos, tais como o aumento da resistência de pico e resistência pós-pico, ductilidade e tenacidade. Estes resultados mostram um grande potencial deste tipo de fibra, quando utilizado como reforço de solos, por exemplo, em base de fundações superficiais, aterros sobre solos moles e liners de cobertura de aterros sanitários. A partir de ajustes matemáticos para determinar a interação entre solos granulares e observações do comportamento global em macro-escala tornou possível analisar o comportamento de solos granulares reforçados com fibras de uma forma micro-mecânica. A modelagem numérica do comportamento mecânico de solos reforçados com fibras de polipropileno, através de uma análise micro-mecânica, utiliza como ferramenta o Método dos Elementos Discretos (MED), que permite a representação do solo em 2D, a partir de um conjunto de partículas de elementos discretos circulares. O MED descarta a visão clássica do solo como uma forma contínua, proporcionando a possibilidade de modelá-lo como partículas constituintes. Sua formulação baseia-se no equilíbrio de forças e de deslocamentos gerados pelos contatos, os quais são descritos através das leis da física clássica, permitindo o mapeamento dos movimentos de cada partícula. A vantagem da micro-mecânica é a possibilidade de explicitar microestruturas, tais como fibras de polipropileno, responsáveis pela mudança no comportamento do solo. Com base no estudo deste fenômeno, causado pela inserção de fibras de polipropileno em materiais granulares, formulações matemáticas foram propostas com a finalidade de descrever o comportamento de solos reforçados através da implementação do código de elementos discretos (DEMlib). Após a calibração e validação do programa, a influência decorrente da inserção do reforço de fibra ao solo foi analisada, sendo realizadas simulações de ensaios biaxiais em amostras discretas de areia, com e sem o reforço fibroso. O comportamento micro-mecânico de misturas reforçadas permitiu avaliar os efeitos das mudanças no teor de fibras presente na matriz de solo, bem como diferentes rigidezes das fibras. Conclui-se que o estudo realizado pelo Método dos Elementos Discretos identificou a real interação entre as partículas do solo e do reforço em forma de fibra, indicando que as fibras, quando inseridas no solo, podem sofrer deformações plásticas de tração e alongamento até atingir a ruptura, proporcionando a melhora nos parâmetros mecânicos do solo. / [en] A large number of new geotechnical materials was developed based on the addition of fibrous materials being incorporated as reinforcement. The technique of reinforced soil can be represented by the production and application, not only natural fiber, but also synthetic fibers and polymer. Previous studies of soil reinforced with polypropylene fibers have shown significant improvement of mechanical properties of soils, such as increasing the resistance peak and postpeak strength, ductility and toughness. These results show a great potential for this type of fiber, when used as soil reinforcement, for example, based on shallow foundations, embankments over soft soils and liners for landfill cover. From mathematical adjustments to determine the interaction between granular soils and the observation of global macro-scale become possible to analyze the behavior of granular soils reinforced with fibers in a micro-mechanics. The numerical modeling of mechanical behavior of soil reinforced with polypropylene fibers, through a micro-mechanical analysis, the tool uses as the Discrete Element Method (DEM), which allows the representation of the soil in 2D, from a set of particles circular discrete elements. The MED rule out the classical view of soil as a continuous form, providing the ability to model it as a constituent particle. Its formulation is based on the balance of forces and displacements generated by the contacts, which are explained through the laws of classical physics, allowing the mapping of movements of each particle. The advantage of micro- mechanics is the possibility of explicit microstructures, such as polypropylene fibers, responsible for the change in the behavior of the soil. Based on the study of this phenomenon, caused by the insertion of polypropylene fibers in granular materials, mathematical formulations have been proposed in order to describe the behavior of reinforced soils through the implementation of the Code of discrete elements (DEMlib). After calibration and validation program, the influence due to the insertion of fiber reinforcement to the soil was analyzed, and simulations of biaxial tests on discrete samples of sand, with and without the fibrous reinforcement. The micro-mechanical behavior of blends reinforced allowed evaluating the effects of changes in fiber content present in the soil matrix and different rigidities of the fibers. We conclude that the study by the Discrete Element Method identified the actual interaction between the soil particles and the reinforcement in the form of fiber, indicating that the fibers, when inserted into the soil, may undergo plastic deformation and tensile elongation until the rupture, providing an improvement in mechanical parameters of soil.

Made available in DSpace on 2016-12-08T15:56:19Z (GMT). No. of bitstreams: 1 Ricardo Kirchhof Unfer.pdf: 99775 bytes, checksum: 27709fdea77151b3e21cfdaf92146d6e (MD5) Previous issue date: 2015-08-28 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The new contributions of present thesis are an alternative experimental waviness method and a new theoretical model for evaluation of limit strains of sheet metal forming in the automotive industry, employing the analysis of roughness and waviness parameters evolution with the equivalent plastic strain and a new ductile rupture criterion as function of stress triaxiality. For validation of proposed experimental waviness method and rupture criterion, specimens of IF steel sheet of thickness 0.72mm, 0.82mm and 0.85mm were tested under tensile test and Nakazima sheet forming test with Marciniak flat punch. The specimens were deformed in incremental steps in different strain path such as: balanced biaxial stretching, plane strain, uniaxial tension and pure shear. Present proposed method consider that roughness and waviness parameters are important surface quality index and useful as indicator of onset of visible local necking and should be monitored in sheet metal forming. Thus, a Waviness Limit Curve, WLC, is proposed to be plotted in Map of Principal Limit Strains (MDLC) of sheet metal as an alternative to the forming limit strain curve, FLC. Various parameters of roughness and waviness such as arithmetic average roughness (Ra), maximum peak-valley roughness (Rt), arithmetic average waviness (Wa), total heigth peak-valley waviness (Wt), maximum peak height waviness (Pp) and maximum valley depth waviness (Pv) were measured during the uniaxial and biaxial testing. Tensile test of IF steel specimens at 0º, 45º and 90º to the rolling direction, RD, and Nakazima type of IF steel specimens at 0º RD only, in which a mesh of 2.5mm circles were printed, were employed. During the uniaxial and biaxial testing, the following plastic deformations were calculated in each straining step from the printed circles in the sheet surface: major true strain (&#61541;1) and minor true strain (&#61541;2). Parameters of roughness and waviness versus equivalent plastic strain curves were plotted to obtain a phenomenological equation of 4th and 3rd degree polynomials, using the Hill 1979 yield stress criterion. Furthermore, the growth rate of parameters Wa and Wt with equivalent plastic strain were calculated. From the growth rate, it was possible to conclude that the sheet 12 thickness imperfections, measured by Wa and Wt, evolve during material deformation, being possible to predict with accuracy the influence of equivalent plastic strain in the onset of local necking. From the experimental analysis, it was concluded that the maximum peak-valley waviness parameter (Wt) was the best option to chacaracterized the beginning of local necking in IF steel sheet forming. Thus, from the analysis of waviness growth rate parameters, Wa and Wt, during plastic strains, it was possible to propose a criterion of local necking inception. This allowed to obtain and plot an experimental Waviness Limit Curve (WLC) in the map MDLC: the beginning of local necking was established when the normalized parameter Wt* (=Wt/Wto) attained a critical value Wt*= 2.5, but with distinct values of equivalent strains. A second mathematical model was proposed for local necking criterion to obtain the FLC of IF steel sheets, employing stress triaxiality analysis and the Hill 1979 yield stress criterion. 2nd degree polynomials were obtained from plotted and adjusted phenomenological curves in graphs of equivalent strain at rupture versus stress triaxiality, considering the different plastic strain path in the formability testing. The IF steel specimens showed ductile rupture, according to scanning electronic microscope examinations, which showed that rupture occurred due to formation, growth and coalescence of large quantity of pores in many specimens of balanced biaxial (BB) and plane strain (DP). Also, mixed rupture of ductile type due to shear mechanisms in certain regions of tensile test (TS) and Nakazima uniaxial tension (UTN) specimens were shown. / As propostas de ineditismo da presente tese foram mostrar um método experimental alternativo de rugosidades e um modelo teórico de ruptura novo para se avaliar as deformações limites de conformação de chapas metálicas da indústria automobilística, empregando-se uma análise da evolução dos parâmetros de ondulação da rugosidade com a deformação plástica equivalente e um critério de ruptura dúctil em função da triaxialidade das tensões. Para validação do método experimental de rugosidades e do critério de ruptura propostos, utilizou-se corpos de prova de chapas de aço IF de 0,72mm, 0,82mm e 0,85mm de espessura, que foram submetidas aos ensaios de tração simples e ensaio de estampagem tipo Nakazima com punção plano de Marciniak. As amostras foram sujeitas a deformação incremental em diferentes trajetórias de deformação, tais como: estiramento biaxial balanceado, deformação plana, estiramento uniaxial e cisalhamento puro. O presente método proposto considera que parâmetros de rugosidade e ondulação são índices importantes de qualidade da superfície e servem como indicador preciso do início da estricção local visível e devem ser monitorados na conformação de chapas metálicas. Portanto, propõe-se traçar uma Curva Limite de Ondulação da Rugosidade, CLOR, no Mapa das Deformações Principais Limite de Conformação (MDLC) das chapas metálicas como alternativa da curva limite de conformação, CLC. Vários parâmetros do perfil de rugosidade e da ondulação da rugosidade tais como a rugosidade média aritmética (Ra), altura máxima pico-vale (Rt), ondulação média aritmética (Wa), a altura máxima da ondulação pico-vale (Wt), altura máxima de pico da ondulação (Pp) e profundidade máxima de vale (Pv) foram medidos durante os ensaios uniaxiais e biaxiais. Foram utilizados corpos de prova de aço IF em tração simples a 0º, 45º e 90º da direção de laminação, DL, e corpos de prova tipo ensaio Nakazima de aço IF somente a 0º DL nos quais foram impressos uma malha de círculos de 2,5 mm de diâmetro. Durante os ensaios uniaxiais e 10 biaxiais, as seguintes deformações plásticas foram calculadas em cada etapa a partir da malha de circulos impressos na superficie da chapa: a deformação verdadeira longitudinal maior (&#61541;1) e a deformação verdadeira transversal menor (&#61541;2). Curvas dos parâmetros de rugosidade e ondulações versus deformação plástica equivalente, empregando-se o critério de escoamento plástico de Hill (1979), foram traçados para se obter equações fenomenológicas do tipo polinomial de 4° e 3° graus. Além disso, foram calculadas as taxas de crescimento dos parâmetros Wa e Wt com a deformação plástica equivalente. A partir das curvas de taxas crescimento, foi possível concluir que as imperfeições na espessura da chapa, medidas por meio de Wa e Wt, evoluem durante a deformação do material, sendo possível prever com precisão a influência da deformação plástica equivalente no início do surgimento da estricção local. Concluiu-se então que o parâmetro da altura máxima total pico-vale das ondulações (Wt) é a melhor opção para caracterizar o início da estricção local em chapas de aço IF. Portanto, a partir da análise das taxas de crescimento dos parâmetros de ondulação, Wa e Wt, durante as deformações plásticas, foi possível propor um critério para o surgimento da estricção local. Isto permitiu obter e traçar a curva experimental de Limite de Ondulação da Rugosidade, (CLOR), no Mapa MDLC: o início da estricção local foi quando o parâmetro normalizado Wt* (=Wt/Wto) atingiu o valor crítico Wt*=2,5, mas com valores distintos da deformação equivalente. Um segundo modelo matemático foi proposto como critério de estricção local para obtenção da CLC de chapas de aço IF, empregando-se análise da triaxialidade de tensões e o critério de escoamento plástico de Hill (1979). Foram obtidos polinômios de 2º grau por meio de curvas fenomenológicas ajustadas e traçadas nos gráficos de triaxialidade de tensões versus deformação equivalente de ruptura, considerando-se as diferentes trajetórias da deformação plástica dos ensaios de conformabilidade. As amostras de chapa de aço IF mostraram ruptura dúctil conforme exame no microscópio eletrônico de varredura, o qual mostra que a fratura ocorreu devido a formação, crescimento e coalescência de uma grande quantidade de espaços vazios ou poros na maioria dos corpos de prova tipo Biaxial Balanceado (BB) e Deformação Plana (DP). Também, as amostras apresentaram fraturas mistas do tipo dúcteis e com mecanismos de cisalhamento em determinadas regiões das amostras fraturadas em Tração Simples (TS) e Tração Uniaxial de Nakazima (UTN).

Fundação de Amparo a Pesquisa no Estado do Rio Grande do Sul / The aim of this study was to evaluate the effect of hard machining, thermal cycle for glazing and acid etching on the surface roughness and flexural strength of a leucite glass-ceramic. Additionally, it was investigated whether the roughness after machining would be influenced by the machining order and by the pair of burs employed. Six pair of burs were used to produce 144 discs by automated machining, which were divided into groups (n=24): 1) machining (M); 2) machining and heat treatment (MH); 3) machining and acid etching (MA); 4) machining, heat treatment and acid etching (MHA); 5) machining and polishing (MP); 6) machining, polishing and acid etching (MPA). The roughness after each treatment was measured using a contact profilometer. The discs were submitted to a piston-on-three ball flexure test (ISO 6872/2008). Weibull analysis was used to compare the characteristic strength (σ0) and Weibull modulus (m) of the groups. The effect of the treatments, machining order and pair of burs on the surface roughness of the specimens was analyzed. Machining reduced the σ0 when compared to polishing. The polishing protocol was able to eliminate the defects introduced by machining, which was observed by means of scanning electron microscopy. The heat treatment did not alter the roughness, but reduced the σ0 and created amorphous material on the ceramic surface, as shown by the x-ray diffraction. Acid etching increased roughness, without reduce σ0. The Weibull modulus did not differ significantly among the groups, which means that all the treatments resulted in similar defects distribution. Spearman s coefficient (rs) indicated strong and significant correlation between machining order and roughness (rsRa = -0,66; rsRz = -0,73). The roughness after machining differed significantly according to the pair of burs employed (p<0,05). Thus, hard machining and thermal cycle for glaze demonstrated a negative effect on the ceramic strength, as opposed to acid etching, which does not appear to affect the flexural strength of the material. Variability in the roughness data could be expected after machining, since the Ra and Rz values seem to be influenced by the machining order and the pair of burs employed. / O presente trabalho objetivou avaliar o efeito da usinagem de corte duro, do ciclo térmico de glazeamento e do condicionamento ácido na rugosidade superficial e na resistência flexural de uma cerâmica vítrea reforçada por leucita. Adicionalmente, buscou-se investigar se a rugosidade após usinagem seria influenciada pela ordem de usinagem e pelo par de brocas utilizado. Seis pares de brocas foram empregados na confecção de 144 discos por usinagem automatizada, os quais foram divididos nos grupos (n=24): 1) usinagem (U); 2) usinagem e tratamento térmico (UT); 3) usinagem e condicionamento ácido (UCA); 4) usinagem, tratamento térmico e condicionamento ácido (UTCA); 5) usinagem e polimento (UP); 6) usinagem, polimento e condicionamento ácido (UPCA). A rugosidade (Ra e Rz) após os tratamentos foi mensurada em perfilômetro de contato. Os discos foram submetidos ao ensaio de flexão biaxial piston-on-three ball (ISO 6872/2008). Análise de Weibull foi utilizada para comparar-se os grupos quanto à resistência característica (σ0) e ao módulo de Weibull (m). Os efeitos dos tratamentos, da ordem de usinagem e dos diferentes pares de brocas sobre a rugosidade superficial dos corpos de prova foi estudado. A usinagem reduziu a σ0, quando comparada ao grupo UP. O protocolo de polimento adotado foi capaz de eliminar os defeitos oriundos da usinagem, o que foi verificado por meio de imagens em microscopia eletrônica de varredura. O tratamento térmico não alterou a rugosidade, mas reduziu a σ0 e ocasionou a formação de material amorfo na superfície da cerâmica, como mostrado pela difração de raios-x. O condicionamento ácido aumentou a rugosidade, sem alterar a σ0. O valor de m não diferiu significativamente entre os grupos, o que significa dizer que os tratamentos aplicados na cerâmica resultaram em distribuição similar de defeitos. Coeficiente de Spearman (rs) indicou correlação forte e significativa entre ordem de usinagem e rugosidade (rsRa = -0,66; rsRz = -0,73), a qual diferiu significativamente conforme o par de broca empregado para a usinagem (p<0,05). Sendo assim, a usinagem de corte duro e o ciclo térmico usado no glazeamento demostraram efeito negativo na resistência da cerâmica, em oposição ao condicionamento ácido, o qual parece não afetar a resistência do material. Variabilidade dos dados de rugosidade pode ser esperada após usinagem, uma vez que os valores de Ra e Rz parecem ser influenciados pela ordem de usinagem e pelo par de brocas utilizado.

Orientador: Prof. Dr. Jeverson Teodoro Arantes Junior / Tese (doutorado) - Universidade Federal do ABC, Programa de Pós-Graduação em Nanociências e Materiais Avançados, Santo André, 2018. / Investigamos, sistematicamente, as propriedades estruturais e eletrônicas do óxido de zinco nanoporoso sob tração e compressão biaxial utilizando cálculos de primeiros princípios baseados na Teoria do Funcional da Densidade. O sistema apresenta uma alta concentração de nanoporos lineares orientados nas direções cristalográcas [0001] e [01-10], bem como um lme no nanoporoso. Para compressões maiores do que 4% com relação ao parâmetro de rede, foi observada uma distorção estrutural nas regiões menos densas do material poroso, mostrando uma tendência à mudança de fase localizada. O coe- ciente de Poisson calculado dos nanoporos orientados na direção [0001] foi negativo. Isto signica que quando o material poroso foi tracionado, expandiu-se transversalmente. Já quando comprimido, o material contraiuse na direção transversal. Os materiais que possuem esta característica são conhecidos como materiais auxéticos. Nossos resultados mostram que o valor do gap de energia foi modulado pelas deformações biaxiais com uma tendência oposta ao bulk. A densidade dos estados eletrônicos conrmou nossas observações. A tendência estrutural inversa da superfície dos nanoporos é o principal mecanismo para o comportamento inverso do gap sob compressão e tração. Dentro do nosso conhecimento, este é o primeiro reporte de um comportamento inverso do gap de energia de estruturas de ZnO sob compressão e tração biaxial. Nossos resultados sugerem que a nanoporosidade, conjuntamente com tra- ção e compressão biaxial, podem ser empregadas como um método dentro da engenharia de gap para customizar materiais funcionais que requerem controle da atividade eletrônica. / This work investigated, systematically, the structural and electronic properties of nanoporous zinc oxide, under biaxial strain, through rst-principles methods, based on total energy ab initio calculations using Density Functional Theory. The system was in a massive nanopore concentration regime. We studied linear pores in [0001] and [01-10] direction and a porous thin lm. Using a biaxial tension above 4% of the ZnO bulk lattice parameter, we observed a distortion resulting in a local phase change region in the material's structure. The calculated Poisson's coecient was negative for the [0001] pore. When stretched, they become thicker in the perpendicular direction to the applied force. These materials are known as auxetic. Our results show that the energy band gap value is tuned by the strain with an uncommon opposite trend related to the bulk. The density of electronic states conrmed the energy gap modulation. The structural inverse trend of nanopores surface is the principal mechanism for gap inverse behavior under compressive and tensile strain. From the best of our knowledge, this is the rst report about opposite Egap trend in strained nanopores. Our results suggest that nanoporosity and biaxial strain could be employed as a method within the band gap engineering for tailored functional matexi rials that require control of the electronic activity.

Das Trag- und Verbundverhalten textiler Bewehrungen wurde in den vergangen Jahren umfassend experimentell untersucht. Die dabei gewonnenen Erkenntnisse stützen sich jedoch fast ausschließlich auf einaxiale Beanspruchungszustände. Grundsätzlich können aus dem Vergleich von Versuchen an Rovings und an textilen Bewehrungsstrukturen Rückschlüsse auf den Einfluss der Quer- und Stützfäden und der verschiedenen Bindungstechniken auf das einaxiale Tragverhalten von Textilbeton getroffen werden. Offen bleibt jedoch, inwieweit sich die gefundenen Gesetzmäßigkeiten auf mehraxiale Beanspruchungssituationen übertragen lassen. Dadurch werden Fragen bezüglich des Tragverhaltens textiler Bewehrungen unter mehraxialen Zugbeanspruchungen aufgeworfen, welche die Motivation für die vorliegende Arbeit liefern. Die hierzu durchgeführten experimentellen Untersuchungen umfassen 84 Einzelversuche und wurden in einem speziell für zweiaxiale Zugbeanspruchungen entwickelten Versuchsaufbau durchgeführt. Als textile Bewehrungen kamen zwei verschiedene Gelegearten aus AR-Glas und Carbon zum Einsatz. Die Ergebnisse konnten die bisher ausschließlich an einaxialen Dehnkörpern gewonnenen Erkenntnisse über das Tragverhalten textiler Bewehrungen grundsätzlich bestätigen. Für den Übergang von Zustand I zum Zustand II konnte eine Abhängigkeit der Erstrissspannung vom Spannungsverhältnis nachgewiesen werden. Die Merkmale der Zustände IIa und IIb zeigen hingegen keine signifikante Abhängigkeit vom Verhältnis aus Längs- und Querzugspannung. Darüber hinaus haben offenbar durch Querzug induzierte bewehrungsparallele Risse keine maßgeblichen Auswirkungen auf das Verbundverhalten der Rovings in Längsrichtung. Eine wesentliche Erkenntnis aus den biaxialen Zugversuchen mit Carbon betrifft den Einfluss der Welligkeit. Es wurde deutlich, dass der Abbau der Welligkeit in beschichteten textilen Bewehrungen hochgradig lastabhängig ist. In zahlreichen Versuchen mit Carbon kam es innerhalb des Zustands IIb zu Delamination, einem bisher in diesem Umfang nicht beobachteten Effekt. Die Erkenntnisse hinsichtlich des Abbaus der Welligkeit wurden im Anschluss auf das Tragverhalten von AR-Glas übertragen und führten zu einer Neubewertung des bei AR-Glas beobachteten Steifigkeitsdefizits im Zustand IIb. Weiterhin wurde der Einfluss der Orientierung der Bewehrung unter einaxialer Beanspruchung an scheibenartigen Probekörpern untersucht. Es zeigte sich, dass die untersuchten Bewehrungen aus AR-Glas hinsichtlich der Tragfähigkeit bei schiefwinkliger Beanspruchung deutlich unempfindlicher reagieren als Bewehrungen aus Carbon. Für die Reduktion der effektiven Faserbruchspannungen wurde ein mathematisches Modell vorgestellt, welches eine getrennte Beschreibung der geometrischen Einflüsse sowie alle sonstigen, die Faserbruchspannung reduzierenden Effekte erlaubt. / The load bearing and bond behaviour of textile reinforcements has been comprehensively studied experimental in recent years. The findings are based almost exclusively on uniaxial loading. Generally, from the comparison of tests on rovings and fabrics conclusions can be drawn about the influence of transverse and supporting threads and different binding patterns on the uniaxial load-bearing behaviour. However, it remains open, to what extend the found principles are applicable to multi-axial loading situations. This raises questions about the load bearing behaviour under multi-axial tension loading, which provide motivation for this work. For the experimental studies on 84 specimens a specially developed test setup for biaxial tensile loading was used. Two different types of textile reinforcements made from AR-glass and carbon fibres were examined. The results generally approve the findings on the structural behaviour of textile reinforcements exclusively derived from uniaxial tests. A relationship between first cracking stress level and biaxial stress ratio has been found. The characteristics of the cracking phases and during stabilized cracking, however, show no significant dependencies on the ratio of longitudinal and transverse tensile stresses. Furthermore, parallel cracks induced by transverse tensile stresses have no significant impact on the bond behaviour of longitudinal rovings. An essential result from biaxial tensile tests with carbon is the strong influence of waviness. It became clear that the reduction of waviness in coated textile reinforcement is highly load-dependent. In numerous experiments with carbon reinforcement delamination occurred during stabilized cracking – an effect, that has been observed in this large scale for the first time. The findings regarding the reduction of the waviness were subsequently applied to AR-glass and led to a revaluation of the known stiffness deficit in the phase IIb. Furthermore, the influence of reinforcement orientation has been studied on discoidal specimens under uni-axial loading. It was found that the load bearing capacity of carbon reinforcement is much more sensible to load orientation than AR-glass. A mathematical model was presented, which allows the separate description of geometric factors and as well as all other effects that reduce the fibre tensile strength.

A ABNT NBR 6118:2014 &#8211; Projeto de Estruturas de Concreto apresenta quatro métodos para dimensionamento de pilares, sendo necessário o uso de envoltórias de momentos quando houver flexão composta oblíqua. Devido à complexidade, não se considera de forma adequada a não linearidade física, a verificação de flexão composta oblíqua e as imperfeições geométricas locais. Este trabalho apresenta diretrizes para o dimensionamento de pilares retangulares de concreto com armadura simétrica, submetidos à flexão composta oblíqua, empregando-se as envoltórias mínimas e resistentes para verificação da armadura. São feitas análises de como as não linearidades influem no estado-limite último de instabilidade e como elas devem ser consideradas nos métodos de dimensionamento. São indicadas duas situações que podem ser críticas para o pré-dimensionamento. São elaborados roteiros para determinação das envoltórias solicitantes, para cada método de dimensionamento, e das envoltórias resistentes, por meio do cálculo direto ou com o uso de ábacos para flexão composta normal. Há, também, dois apêndices, um sobre a determinação dos diagramas momento fletor &#8211; força normal &#8211; curvatura para qualquer tipo de seção, e outro sobre obtenção dos diagramas de interação (Nu, Mu), construção de ábacos para flexão composta normal e definição da taxa mecânica de armadura &#969;, sem o uso de ábacos para concretos de classe até C50. Concluindo, este trabalho constitui uma bibliografia atualizada para o projeto de pilares seguros e economicamente viáveis, esclarecendo conceitos tais como momento fletor resistente, envoltórias solicitantes e resistentes e utilização das não linearidades nos métodos de dimensionamento. / The Brazilian Code ABNT NBR 6118:2014 &#8211; Design of concrete structures presents four methods for columns dimensioning, requiring the use of envelopment of moments when there is biaxial bending. Due to complexity, do not accurately consider physical nonlinearity, biaxial bending and local geometric imperfections. This work presents guidelines for the design of concrete rectangular columns with symmetrical reinforcement, subjected to biaxial bending, employing the minimum and resisting envelopment curves for the verification of the reinforcement. Analysis are made of how nonlinearities influence in the ultimate limit state of instability and how they should be considered in design methods. Two situations are indicated that can be critical for the pre-dimensioning of the reinforcement. Procedures are developed to determine the envelopment of acting moments, for each design method, as well as the envelopment of resisting moments by means of either direct method or use of abacuses for eccentrical compression. There is also two appendixes, one about the determination of the diagrams bending moment &#8211; normal force &#8211; curvature for any kind of section, and another one about getting interaction diagrams (Nu, Mu), construction of abacuses for eccentrical compression and definition of &#969;, the reinforcement mechanical rate, without the use of abacuses for C50 concrete class or below. In conclusion, this constitutes an updated bibliography for the safe and economically viable columns project, clarifying concepts such as resistant moment, envelopments of acting and resisting moments, and the use of nonlinearities in the design methods.

Les pièces des structures aéronautiques telles que les arbres des turboréacteurs, les roues, les freins ou les trains d’atterrissage sont fabriquées avec des aciers à très haute résistance. Leur structure martensitique, renforcée par des précipités de taille inférieure au micromètre, confère à ces aciers une excellente résistance : leur limite d'élasticité peut dépasser les 1900 MPa et leur résistance mécanique atteindre les 2300 MPa. Ces matériaux sont choisis pour ces excellentes propriétés mécaniques sur la base de leur comportement en traction. Toutefois, leur déformation à striction (maximum de la charge) est de quelques pourcents seulement. Les méthodes de dimensionnement sous chargement critique actuelles considèrent qu’aucun point de la structure ne doit être soumis à une déformation supérieure à la déformation à striction. Ce type d’approche est ici très conservatrice puisque les aciers THR continuent de se déformer plastiquement, ceci jusqu’à plusieurs dizaines de pourcent après le début de la striction. L’objet de ces travaux est de définir un modèle d’amorçage de la rupture applicable au dimensionnement de ces structures pour un acier type : le ML340. Ce matériau est actuellement utilisé dans les arbres de turboréacteur LEAP.Le comportement élasto-plastique du matériau a été étudié grâce à des essais menés sur différents types d’éprouvettes : tractions lisses, axisymétriques entaillées, déformation plane, plates entaillées, traction-torsion. Un modèle simple de von Mises à écrouissage isotrope permet de reproduire l’ensemble de la base. Ce modèle est ajusté sur les essais de traction pour lesquels un suivi optique de la variation du diamètre minium a été mis en place. La loi d’ ́écrouissage est ensuite ajustée en prenant en compte à la fois l'élongation et la variation du diamètre. On montre en particulier que l'extrapolation du comportement, méthode consistant à prolonger les données obtenues avant l'apparition de la striction, peut conduire à une mauvaise prédiction du comportement des éprouvettes.La base expérimentale a également été employée pour étudier l’amorçage de la rupture. L’observation des faciès montre un mode de rupture ductile avec des cupules fines. Cependant, l'initiation est brutale pour tous les essais et le développement de l’endommagement en volume reste très limité, voire nul. Ces constatations conduisent à proposer l’emploi d’un critère d’amorçage découplé : ce modèle fait intervenir la triaxialité des contraintes et le paramètre de Lode. Cette double dépendance est nécessaire pour bien décrire la rupture sur toute la base expérimentale. L’identification des paramètres du modèle se base sur l'évaluation des champs mécaniques à partir des simulations élasto-plastiques par éléments finis représentant les essais. Le modèle est également capable de prédire les emplacements des points d’amorçages observés, ces informations peuvent être utilisées pour ajuster plus finement le modèle. / Aeronautical structures such as jet engines shafts, wheels, brakes or landing gears are made of Ultra High Strenth Steels (UHSS). Due to their hard martensitic matrix reinforced with second phase particles, such steels exhibit extreme mechanical resistance, their yield strength can overcome 1900 MPa and their ultimate tensile strength can reach 2300 MPa. Such materials are selected based on their tensile properties, however strain at necking (maximum load) is only few percent. Conventional certified design methods assume that failure occurs when a given point of the structure reaches this strain. Regarding UHSS this approach is very conservative; those materials are still able to bear large strains after necking start. The aim of this work is to define a failure initiation model able to predict ductile failure of such structures for extremes loadings. The ML340 steel, material of LEAP jet-engine shafts, have been selected for this study.Elasto-plastic behavior is investigated with various mechanical tests. Uniaxial tensile test were performed on round bars specimens, either smooth or notch, and flat specimens, either u notched or plane strain. Traction/torsion and compression/torsion biaxial tests were performed on tubes specimens. A simple isotropic von Mises plasticity model was found sufficient to describe mechanical behavior of this experimental database. This model was calibrated based on round smooth tensile tests, a longitudinal extensometer and a non contact method, measuring diameter reduction, were used in order to monitor strains. Hardening law was adjust with both sets of data using a reverse method, hence material striction is take into account during the identification. Identification method extrapolating plastic behavior based on tensile data measured before the striction begining is shown to overperdict plastic behavior.Failure initiation was also investigated through fracture tests. Every fractography display very fine dimples related to ductile fracture, however fracture apears to be very brutal and very few damage was observed underneath fracture surface. As a result an uncoupled fracture initiation model is proposed, damage indicator is driven by both stress triaxiality and a Lode parameter. This dual dependency is necessary in order to represent fracture for the whole database. Model parameters identification relies on the evaluation of local stress state for each test, this could be achieved with 3D elasto-plastic simulations. As a result fracture model was able to predict correct fracture initiation point positions observed on round tensile tests and flat u notch tests.

This research is the first systematic investigation of solid-state orientation as a novel method for controlling drug release from biodegradable polymers. The effect of various degrees of polymer orientation was studied in oriented Poly (L-lactic acid) (PLA) films containing curcumin and theophylline as model drugs. Additionally, direction specific drug release was studied from oriented PLA rods containing paracetamol. The films oriented to 2X uniaxial constant width (UCW) or 2X2Y biaxial draw ratio showed retardation of drug release, when their nematic structure was stabilised by the presence of crystalline theophylline. Contrarily, the same films when contained solid solution of curcumin, shrunk in the release medium and exhibited a release profile similar to the un-oriented films. All films oriented to the UCW draw ratio ≥ 3X contained α crystalline form of PLA and showed acceleration of drug release proportionate to the draw ratio. According to the proposed mechanism augmented formation of water filled channels in these films was responsible for faster drug release. Similarly, the paracetamol loaded PLA rods die-drawn to uniaxial draw ratios ≥ 3X exhibited enhancement of drug release. Importantly, the amount of drug released along the oriented chain axis was significantly larger than that in the perpendicular direction. Drug release from the die-drawn rods was accelerated by a greater degree than that observed from the oriented films. This can be correlated to the differences in their size, geometry and the crystalline form of PLA. In conclusion, the current study provided substantial evidence that solid-state orientation can offer a control over drug release from PLA.