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The ductile fracture process, which consists of the nucleation, growth and coalescence of microvoids, was extensively studied for materials deforming homogeneously. For materials with a non-homogeneous deformation behavior, such as those having hexagonal closed packed (HCP) crystal structure, experimental and numerical data is lacking. Therefore, the fracture properties of materials with such HCP structure, like titanium (used in aerospace and biomedical applications), zirconium (nuclear industry) and magnesium (manufacturing industry) are not well understood. The main research objective of this Ph.D. thesis is to better understand the mechanisms governing fracture in commercially pure (CP) titanium. In particular, the effect of grain orientation on void growth is investigated. The fracture process of CP titanium was visualized in model materials containing artificial holes. These model materials were fabricated using a femtosecond laser coupled with a diffusion bonding technique to obtain voids in the interior of titanium samples. Diffusion bonding was carried out either above or below the phase transformation temperature resulting in different microstructures. Changes in void dimensions during in-situ straining were recorded in three dimensions using x-ray computed tomography. Void growth obtained experimentally was compared with the Rice and Tracey model which predicted well the average void growth. However, a large scatter in void growth was observed experimentally and was explained in terms of differences in grain orientation which was confirmed by crystal plasticity simulations. It was also shown that grain orientation has a stronger effect on void growth than intervoid spacing and material strength. Intervoid spacing, however, appears to control whether the intervoid ligament failure is ductile or brittle. While this study showed a good agreement between experiments and simulations on average, there is no direct void growth comparison for particular grain orientations. In a follow-up study, an experimental approach was developed to directly relate the growth of a void to its underlying grain orientation. This is achieved by first annealing CP titanium samples below the α-β phase transformation temperature, then performing electron backscatter diffraction iii (EBSD) and finally diffusion bonding the samples together. Samples were then tested in x-ray tomography. This study showed the importance of the local state of strain on void growth. Crystal plasticity simulations that take into account the particular grain orientation and the local state of strain were found to predict well experimental void growth. Crystal plasticity simulations confirmed that the orientation of the voidcontaining grain is more important than the orientation of surrounding grains and more important than the volume fraction of voids, in order to determine void growth. This thesis on the growth and coalescence of voids is important to validate and improve the predictions of ductile fracture models and to design new materials with improved fracture properties.

Continuous bending under tension (CBT) has been shown to increase room temperature elongation-to-failure (ETF) in various sheet metals past that of simple tension (ST). In commercially pure titanium (CP-Ti) Grade 4, up to 3x extended elongation over ST has been achieved. A greater understanding of deformation mechanisms in CBT would allow for its elongation-enhancing effects to be more fully exploited in HCP and other metals, creating potential for new forming strategies. While most of the extended ETF has been attributed to delayed localization via incremental deformation inherent to the CBT process, together with compressive stabilization and relaxation of mechanical strain fields, contributions of microscale components relating to damage evolution, defect structures, and slip system activity intrinsic to the process are also likely to play a role. CBT-induced cyclic bending/unbending stresses combined with applied macroscopic tension create complex through-thickness stress profiles, where differing hardening behavior is expected near the surfaces compared with the middle of the sheet. This work uses high resolution EBSD characterization of geometrically necessary dislocation (GND) density together with X-ray diffraction (XRD)-based evaluations of total dislocation density and in-plane digital image correlation (DIC) to provide an in-depth analysis of through-thickness dislocation development and associated hardening rates throughout the CBT process in CP-Ti Grade 4 sheet metal. It was found that dislocation density is relatively uniform across the sheet at lower cycles, increases in the sheet center at higher cycles, and eventually approaches saturation near failure. Namely, dislocation accumulation occurs more slowly in the ratcheting, bending/unbending portions of the sheet (i.e., near the surfaces) from cyclic load reversals, and develops faster in the central tensile portion, where dislocation density up to 1.43x higher than near the surfaces was observed. The fraction of 〈c+a〉-type dislocations stayed below ~27% within the sheet, decreasing with increased strain, suggesting that the texture evolves such as to favor 〈a〉-type slip. Indications of stronger texture evolution occurring in the ratcheting (cyclic) regions were observed, with central texture resembling that of a sample deformed in ST. High dislocation densities in the sheet center were found to precede significant central void accumulation, concentrating damage away from peak surface stresses, presumably contributing to delayed failure.

A higienização das próteses parciais ou totais removíveis é fundamental para a durabilidade do tratamento e prevenção de patologias orais. O objetivo deste estudo foi avaliar o efeito de agentes higienizadores de prótese na cor, corrosão e rugosidade superficial do titânio c.p., ligas metálicas e resina acrílica termopolimerizável, simulando um período de 180 dias de higienização. Espécimes em formato de discos (12 mm x 3 mm) foram confeccionados em: titânio comercialmente puro (Tritan - Ti c.p.), liga de níquel-cromo-molibdênio-titânio (Vi-Star), liga de níquel-cromo (Fit Cast-SB Plus) e liga de níquel-cromo-berílio (Fit Cast-V). Cada disco fundido foi incluído em mufla previamente preparada por matrizes retangulares de teflon (38 mm x 18 mm x 4 mm), incorporando-se o disco metálico à resina acrílica termopolimerizável. Os corpos-de-prova (n=5) foram imersos em soluções dos agentes higienizadores: hipoclorito de sódio a 0,05%, Periogard, Cepacol, pastilha Corega Tabs, pastilha Medical Interporous e pastilha Polident 3 Minute. Como controle, foi utilizada a água deionizada. Foram realizados ensaios de estabilidade de cor por meio de espectrocolorímetro (Color-guide 45/0), resistência à corrosão por meio da análise visual da presença de manchas no metal e análise da alteração de massa (balança eletrônica analítica), e rugosidade superficial por meio de rugosímetro (Surftest SJ-201P). Além disso, foi realizada análise quantitativa de liberação de íons metálicos por meio de espectrometria de massa com plasma indutivamente acoplado (ICP-MS - ELAN DRC II). Os resultados de estabilidade de cor, alteração de massa e rugosidade foram submetidos à ANOVA e teste de Tukey (p< 0,05). Quanto à estabilidade de cor da resina acrílica termopolimerizável (E), houve diferença estatisticamente significante entre o titânio c.p. e as ligas. A resina associada ao Ti c.p. apresentou menor alteração de cor, enquanto que a resina associada à Fit Cast-SB Plus apresentou a maior alteração de cor (1,33 ± 1,11 e 5,06 ± 1,96, respectivamente). Com relação à presença de manchas no metal, o hipoclorito de sódio causou manchamento nos espécimes das ligas Vi-Star e Fit Cast-V. Quando avaliada a alteração de massa (g), o Cepacol e a pastilha Corega Tabs propiciaram maior perda de massa. Entre os metais, a amostra do Ti c.p. apresentou maior perda de massa. Quanto à rugosidade (Ra, µm) da resina, o Cepacol causou maior rugosidade, enquanto que a pastilha Corega Tabs e o Periogard propiciaram maior lisura no corpo-de-prova. A resina associada ao Ti c.p. e ao Fit Cast-SB Plus apresentaram maior rugosidade. Quanto à rugosidade do metal, os produtos de imersão não influenciaram nos resultados, mas a liga Fit Cast-SB Plus apresentou maior rugosidade após a imersão. A liberação de íons mais expressiva foi constatada nas ligas Vi-Star e Fit Cast-V após a imersão na pastilha Medical Interporous. Pode-se concluir que as ligas Vi-Star e Fit Cast-V podem ser consideradas seguras para a confecção de aparelhos protéticos removíveis, mas com a condição de não utilizar o hipoclorito de sódio a 0,05% ou a pastilha Medical Interporous para a higienização, pois causaram corrosão e maior liberação de íons, respectivamente. / The hygiene care of the removable partial and complete dentures is required for the longevity of the treatment and prevention of oral diseases. The aim of this study was to evaluate the effect of denture cleansers on color, corrosion and surface roughness of the commercially pure titanium, metal alloys and heat-polymerized acrylic resin, simulating a period of 180 days of hygiene. Disk-shaped specimens (12 mm x 3 mm) had been fabricated with commercially pure titanium (Tritan - Ti c.p.), nickel-chromium-molybdenum-titanium alloy (Vi-Star), nickel-chromium alloy (Fit Cast-SB Plus) and nickel-chromium-beryllium alloy (Fit Cast-V). Each cast disc was invested in the flasks previously prepared by Teflon rectangular matrices (38 mm x 18 mm x 4 mm), incorporating the metal disk to the heat-polymerized acrylic resin. The specimens (n= 5) had been immersed in the solutions: sodium hypochlorite 0.05%, Periogard, Cepacol, Corega Tabs, Medical Interporous and Polident 3 Minute. As a control, it was used deionized water. It was accomplished assays of color stability by means of a colorimeter (Color-guide 45/0), corrosion resistance by means of visual analysis of tarnishes on the metal and mass alteration analysis (analytical electronic balance), and surface roughness by means of a surface analyzer (Surftest SJ-201P). Besides, the quantitative analysis of metal ions release was accomplished by means of inductively coupled plasma mass spectrometry (ICP-MS - ELAN DRC II). Color stability, mass alteration and roughness results were submitted to ANOVA and Tukey test (p<0.05). Considering the color stability of the heat-polymerized acrylic resin (E), there were statistically significant difference between the titanium c.p. and the alloys. The resin associated with the Ti c.p. showed lesser color alteration, whereas the resin associated with Fit Cast-SB Plus showed the higher color alteration (1,33 ± 1,11 e 5,06 ± 1,96, respectively). In relation to the presence of tarnishes on the metals, the sodium hypochlorite caused tarnishes on specimens of the Vi-Star and Fit Cast-V alloys. When evaluated the mass alteration (g), Cepacol and Corega Tabs propitiated higher weight loss. Between the metals, the Ti c.p. samples showed greater weight loss. Considering the resin roughness (Ra, µm), Cepacol caused higher roughness, whereas Corega Tabs and Periogard propitiated greater smoothness on the specimens. The resin associated with the Ti c.p. and Fit Cast-SB Plus showed higher roughness. Considering the metal roughness, the immersion products did not influence on the results, but the Fit Cast-SB Plus showed greater roughness after immersion. The ionic release most significant was with the Vi-Star and Fit Cast-V alloys after immersion in Medical Interporous. It could be concluded that the Vi-Star and Fit Cast-V alloys can be considered safe for removable prosthesis finish, but with the condition of do not use sodium hypochlorite 0.05% or Medical Interporous tablet for hygiene, because they caused corrosion and greater ionic release, respectively.

O objetivo do trabalho foi avaliar a influência do envelhecimento artificial acelerado e do fluorfosfato acidulado a 1,23% sobre a rugosidade superficial e alteração de cor de duas cerâmicas odontológicas de ultra-baixa fusão para titânio (Triceram- Dentaurum, e Noritake Ti22- Noritake), livre de metal ou com subestrutura em titânio comercialmente puro (Tritan- Dentaurum). A partir de uma matriz cilíndrica em teflon foram confeccionados, ao todo, 80 corpos-de-prova, com 15mm de diâmetro e 2,5mm de espessura, sendo 40 para cada cerâmica, 20 amostras livre de metal e 20 metalocerâmicas, que foram divididas em dois grupos de 10 amostras cada, sendo submetidas ao envelhecimento artificial acelerado (Sistema Acelerado de Envelhecimento para não-metálicos C-UV - Comexim Matérias Primas Ltda, São Paulo, Brasil) ou ao armazenamento em fluorfosfato acidulado a 1,23%. A rugosidade superficial foi realizada em rugosímetro SJ - 201P (Mitutoyo, Tokyo, Japão) em dois momentos: inicial (R1) foi aquela mensurada logo após obtidos os corpos-de-prova e a rugosidade superficial final (R2) aquela obtida após o envelhecimento artificial acelerado ou armazenamento em fluorfosfato acidulado a 1,23%. Para verificar as alterações de cor ocorridas nas cerâmicas odontológicas utilizou-se o Espectrofotômetro PCB 6807 BYK GARDNER (Columbia, Estados Unidos). Foram feitas leituras antes e após as etapas de envelhecimento artificial acelerado e armazenamento em fluorfosfato acidulado a 1,23%. Os resultados médios e desvios padrão para os corpos-de-prova livre de metal com envelhecimento artificial acelerado foram: a) rugosidade superficial: Triceram antes 0,390 ± 0,097, após 0,431 ± 0,100; Noritake Ti 22 antes 0,299 ± 0,075, após 0,312 ± 0,076; b) alteração de cor: Triceram 0,28 ± 0,14; Noritake Ti 22 0,33 ± 0,22; e para os corpos-de-prova submetidos ao armazenamento em fluorfosfato acidulado a 1,23% foram: a) rugosidade superficial: Triceram antes 0,325 ± 0,036 , após 2,199 ± 0,889; Noritake Ti 22 antes 0,317 ± 0,094, após 2,760 ± 0,833; b) alteração de cor: Triceram 5,39 ± 1,61; Noritake Ti 22 7,31 ± 0,71. Para as amostras metalocerâmicas com envelhecimento artificial acelerado foram: a) rugosidade superficial: Triceram antes 0,282 ± 0,06, após 0,315 ± 0,095; Noritake Ti 22 antes 0,269 ± 0,062, após 0,290 ± 0,075; b) alteração de cor: Triceram 0,57 ± 0,11; Noritake Ti 22 0,41 ± 0,08; e para os corpos-de-prova submetidos ao armazenamento em fluorfosfato acidulado a 1,23% foram: a) rugosidade superficial: Triceram antes 0,137 ± 0,026, após 2,560 ± 0,377; Noritake Ti 22 antes 0,125 ± 0,34, após 3,174 ± 0,565; b) alteração de cor: Triceram 7,56 ± 1,21; Noritake Ti 22 7,69 ± 1,26. Os resultados obtidos mostraram que o envelhecimento artificial acelerado simulando dez anos de uso clínico da restauração não afetou a rugosidade superficial de nenhuma das cerâmicas avaliadas, em nenhum grupo; que apenas o grupo da cerâmica Triceram com subestrutura em titânio comercialmente puro revelou valores de &Delta;E estatisticamente maiores que os demais, revelando que o envelhecimento artificial acelerado influenciou a coloração desse grupo. Entretanto, a alteração de cor apresentou-se menor que um, sendo considerada clinicamente indetectável; que após o armazenamento em fluorfosfato acidulado foi observado aumento de rugosidade superficial semelhante estatisticamente para ambas as cerâmicas estudadas, tanto em amostras livres de metal quanto metalocerâmicas; que a alteração total de cor, após armazenamento em fluorfosfato acidulado, todos os grupos revelaram valores inaceitáveis clinicamente (&Delta;E > 3,3) / The purpose of this study was to evaluate the influence of accelerated artificial aging and of 1.23% acidulated phosphate fluoride over superficial roughness and color stability of two low-fusing dental ceramics for titanium (Triceram- Dentaurum, and Noritake Ti22- Noritake), metal-free or metalceramics using commercially pure titanium (Tritan- Dentaurum). 80 cylindrical samples, with 15mm of diameter and 2.5mm of thickness, being 40 for each ceramic, 20 metal free and 20 metal-ceramics, which were divided into two groups of 10 samples, being submitted to the accelerated artificial aging (System Accelerated of Aging for not-metallic C-UV - Comexim Raw materials Ltda, São Paulo, Brazil) or storage in 1.23% acidulated phosphate fluoride. Superficial roughness was accomplished by roughness tester SJ - 201P (Mitutoyo, Tokyo, Japan) in two moments: initial measured after obtained the samples and final superficial roughness after the accelerated artificial aging or storage in 1.23% acidulated phosphate fluoride. Color changes were analyzed by a spectrophotometer PCB 6807 BYK GARDNER (Columbia, United States). The average results and standard deviations for the metal free over accelerated artificial aging were: a) superficial roughness: Triceram before 0.390 ± 0.097, after 0.431 ± 0.100; Noritake Ti22 before 0.299 ± 0.075, after 0.312 ± 0.076; b) color evaluation: Triceram 0.28 ± 0.14; Noritake Ti22 0.33 ± 0.22; and for samples submitted to the storage in 1.23% acidulated phosphate fluoride were: a) superficial roughness: Triceram before 0.325 ± 0.036, after 2.199 ± 0.889; Noritake Ti22 before 0.317 ± 0.094, after 2.760 ± 0.833; b) Color evaluation: Triceram 5.39 ± 0.61; Noritake Ti22 7.31 ± 0.71. The data were submitted to ANOVA and Duncan statistics analysis to p &le; .05. The obtained results showed that the accelerated artificial aging simulating ten years of clinical use of the restoration did not affect the superficial roughness of none of the evaluated ceramics, in no group; which only the group of the Triceram with substructure in commercially pure titanium revealed values statistically greater than the rest, revealing that the accelerated artificial aging influenced the color of this group. However, the values of color alteration was smaller than 1, being considered clinically acceptable ; which after the storage in 1.23% acidulated phosphate fluoride was observed increased values of superficial roughness with significant difference between both studied ceramics, as in metal-free samples as in metal-ceramics; which the color alteration, after storage in 1.23% acidulated phosphate fluoride, revealed to all the groups evaluated unacceptable values clinically (&Delta;E > 3.3).

O objetivo deste trabalho foi avaliar o efeito do ambiente de sinterização vácuo e argônio na resistência de união (RUMC) de cerâmicas às ligas de Ni-Cr (Fit Cast SB), Co-Cr (Star Loy C) e titânio comercialmente puro (Tritan). A partir de uma matriz de teflon, foram obtidos 60 padrões de resina/cera em forma de cilindro, com 8 mm de comprimento e 5 mm de diâmetro. Os padrões foram incluídos e os anéis foram levados ao forno e submetidos a ciclos térmicos para a expansão do revestimento. Em seguida, os anéis para fundição em Ni-Cr e Co-Cr foram levados à máquina de fundição por indução eletrônica. Os anéis referentes ao titânio foram levados à máquina de fundição por arco voltaico. Após resfriamento dos anéis, as fundições foram desincluídas e jateadas com óxido de alumínio (100 &mu;m). Depois de recortados dos canais de alimentação, os cilindros metálicos foram preparados para aplicação da cerâmica. Em seguida, foi realizada a aplicação e sinterização da cerâmica à vácuo ou em argônio. Para as ligas alternativas, foi utilizada a cerâmica IPS Classic V e para o titânio, a Triceram. Na sequência, os cilindros compostos pelo metal e disco cerâmico (5 mm de diâmetro e 2 mm de espessura) (n=10) foram submetidos aos ensaios de RUMC por cisalhamento na máquina de ensaios universais com célula de carga de 500 Kg e velocidade do travessão móvel de 0,5 mm/min. Após os ensaios, foram realizadas análises das fraturas por meio de microscopia óptica (MO) (15X) e microscopia eletrônica de varredura (MEV). Os dados de RUMC (MPa) obtidos foram analisados estatisticamente pelos testes ANOVA e Tukey (&alpha;=0,05). Os resultados demonstraram que a sinterização à vácuo propiciou obtenção de maiores valores (MPa) de RUMC (76,58) que a sinterização em argônio (51,31). Quanto às ligas avaliadas, as de Ni-Cr e Co-Cr apresentaram maiores valores de RUMC (71,32 e 71,28, respectivamente) que o titânio cp (49,23); sendo que entre elas não houve diferença estatística. Não houve interação entre os fatores avaliados. De acordo com a MO, houve predomínio de fraturas mistas. Segundo a MEV, os espécimes de Ni-Cr e titânio sinterizados a vácuo apresentaram maior rugosidade de superfície do que os sinterizados em argônio. Para a liga de Co-Cr não houve diferença na topografia de superfície. A sinterização em argônio influenciou negativamente a RUMC dos pares metalocerâmicos analisados. / The aim of this study was to evaluate the effect of firing atmospheres: vacuum and argon on the bond strength of ceramic to Ni-Cr (Fit Cast SB), Co-Cr (Star Loy C) and commercially pure titanium (Tritan) alloys. 60 wax/acrylic resin cylinder patterns (8 mm high and 5 mm in diameter) were prepared on a plastic custom mold for metalceramic bond strength (MCBS) test. The patterns were invested in phosphated investment and manipulated on vacuum. The rings were placed in a furnace to burn out patterns and thermally expand the molds. Then, the rings of Ni-Cr and Co-Cr were placed in an electronic machine to cast. The rings related to titanium were positioned in the casting machine with a voltaic arc. After the rings have cooled, the castings were divested manually and abraded with aluminum oxide particles (100 &mu;m). Then, the cylinders were prepared for applying of the ceramic veneering disks. The ceramic was applied and fired in vacuum and argon atmospheres. IPS-Classic ceramic was used for alternative alloys and for titanium, Triceram ceramic. Then, the cylinders composed of metal and ceramic disk (5 mm diameter and 2 mm height) (n=10) were submitted to metal-ceramic bond strength (MCBS) shear tests on an universal testing machine with load cell of 500 Kg at a crosshead speed of 0.5 mm/min. After the tests, there were made fracture analysis by optic microscopy (OM) and scanning electron microscopy (SEM). The MCBS data (MPa) were statistically analyzed by the ANOVA and Tukey test (&alpha;=0.05). The results indicated that the vacuum firing (76.58) promoted higher MCBS values than argon firing (51.31). Among the metals, Ni-Cr and Co-Cr alloys presented higher MCBS (71.32 e 71.28, respectively) than titanium (49.23); between two base alloys there was no statistical difference. There was no interaction between the evaluated factors. According to MO analysis, there was predominance of mixed fractures. According SEM, the Ni-Cr and titanium specimens submitted to vacuum presented higher surface roughness than the specimens submitted to argon. For Co-Cr, there was no difference of surface topography. The argon firing influenced negatively the MCBS of metal-ceramic evaluated pairs.

O objetivo do trabalho foi avaliar a influência do envelhecimento artificial acelerado e do fluorfosfato acidulado a 1,23% sobre a rugosidade superficial e alteração de cor de duas cerâmicas odontológicas de ultra-baixa fusão para titânio (Triceram- Dentaurum, e Noritake Ti22- Noritake), livre de metal ou com subestrutura em titânio comercialmente puro (Tritan- Dentaurum). A partir de uma matriz cilíndrica em teflon foram confeccionados, ao todo, 80 corpos-de-prova, com 15mm de diâmetro e 2,5mm de espessura, sendo 40 para cada cerâmica, 20 amostras livre de metal e 20 metalocerâmicas, que foram divididas em dois grupos de 10 amostras cada, sendo submetidas ao envelhecimento artificial acelerado (Sistema Acelerado de Envelhecimento para não-metálicos C-UV - Comexim Matérias Primas Ltda, São Paulo, Brasil) ou ao armazenamento em fluorfosfato acidulado a 1,23%. A rugosidade superficial foi realizada em rugosímetro SJ - 201P (Mitutoyo, Tokyo, Japão) em dois momentos: inicial (R1) foi aquela mensurada logo após obtidos os corpos-de-prova e a rugosidade superficial final (R2) aquela obtida após o envelhecimento artificial acelerado ou armazenamento em fluorfosfato acidulado a 1,23%. Para verificar as alterações de cor ocorridas nas cerâmicas odontológicas utilizou-se o Espectrofotômetro PCB 6807 BYK GARDNER (Columbia, Estados Unidos). Foram feitas leituras antes e após as etapas de envelhecimento artificial acelerado e armazenamento em fluorfosfato acidulado a 1,23%. Os resultados médios e desvios padrão para os corpos-de-prova livre de metal com envelhecimento artificial acelerado foram: a) rugosidade superficial: Triceram antes 0,390 ± 0,097, após 0,431 ± 0,100; Noritake Ti 22 antes 0,299 ± 0,075, após 0,312 ± 0,076; b) alteração de cor: Triceram 0,28 ± 0,14; Noritake Ti 22 0,33 ± 0,22; e para os corpos-de-prova submetidos ao armazenamento em fluorfosfato acidulado a 1,23% foram: a) rugosidade superficial: Triceram antes 0,325 ± 0,036 , após 2,199 ± 0,889; Noritake Ti 22 antes 0,317 ± 0,094, após 2,760 ± 0,833; b) alteração de cor: Triceram 5,39 ± 1,61; Noritake Ti 22 7,31 ± 0,71. Para as amostras metalocerâmicas com envelhecimento artificial acelerado foram: a) rugosidade superficial: Triceram antes 0,282 ± 0,06, após 0,315 ± 0,095; Noritake Ti 22 antes 0,269 ± 0,062, após 0,290 ± 0,075; b) alteração de cor: Triceram 0,57 ± 0,11; Noritake Ti 22 0,41 ± 0,08; e para os corpos-de-prova submetidos ao armazenamento em fluorfosfato acidulado a 1,23% foram: a) rugosidade superficial: Triceram antes 0,137 ± 0,026, após 2,560 ± 0,377; Noritake Ti 22 antes 0,125 ± 0,34, após 3,174 ± 0,565; b) alteração de cor: Triceram 7,56 ± 1,21; Noritake Ti 22 7,69 ± 1,26. Os resultados obtidos mostraram que o envelhecimento artificial acelerado simulando dez anos de uso clínico da restauração não afetou a rugosidade superficial de nenhuma das cerâmicas avaliadas, em nenhum grupo; que apenas o grupo da cerâmica Triceram com subestrutura em titânio comercialmente puro revelou valores de &Delta;E estatisticamente maiores que os demais, revelando que o envelhecimento artificial acelerado influenciou a coloração desse grupo. Entretanto, a alteração de cor apresentou-se menor que um, sendo considerada clinicamente indetectável; que após o armazenamento em fluorfosfato acidulado foi observado aumento de rugosidade superficial semelhante estatisticamente para ambas as cerâmicas estudadas, tanto em amostras livres de metal quanto metalocerâmicas; que a alteração total de cor, após armazenamento em fluorfosfato acidulado, todos os grupos revelaram valores inaceitáveis clinicamente (&Delta;E > 3,3) / The purpose of this study was to evaluate the influence of accelerated artificial aging and of 1.23% acidulated phosphate fluoride over superficial roughness and color stability of two low-fusing dental ceramics for titanium (Triceram- Dentaurum, and Noritake Ti22- Noritake), metal-free or metalceramics using commercially pure titanium (Tritan- Dentaurum). 80 cylindrical samples, with 15mm of diameter and 2.5mm of thickness, being 40 for each ceramic, 20 metal free and 20 metal-ceramics, which were divided into two groups of 10 samples, being submitted to the accelerated artificial aging (System Accelerated of Aging for not-metallic C-UV - Comexim Raw materials Ltda, São Paulo, Brazil) or storage in 1.23% acidulated phosphate fluoride. Superficial roughness was accomplished by roughness tester SJ - 201P (Mitutoyo, Tokyo, Japan) in two moments: initial measured after obtained the samples and final superficial roughness after the accelerated artificial aging or storage in 1.23% acidulated phosphate fluoride. Color changes were analyzed by a spectrophotometer PCB 6807 BYK GARDNER (Columbia, United States). The average results and standard deviations for the metal free over accelerated artificial aging were: a) superficial roughness: Triceram before 0.390 ± 0.097, after 0.431 ± 0.100; Noritake Ti22 before 0.299 ± 0.075, after 0.312 ± 0.076; b) color evaluation: Triceram 0.28 ± 0.14; Noritake Ti22 0.33 ± 0.22; and for samples submitted to the storage in 1.23% acidulated phosphate fluoride were: a) superficial roughness: Triceram before 0.325 ± 0.036, after 2.199 ± 0.889; Noritake Ti22 before 0.317 ± 0.094, after 2.760 ± 0.833; b) Color evaluation: Triceram 5.39 ± 0.61; Noritake Ti22 7.31 ± 0.71. The data were submitted to ANOVA and Duncan statistics analysis to p &le; .05. The obtained results showed that the accelerated artificial aging simulating ten years of clinical use of the restoration did not affect the superficial roughness of none of the evaluated ceramics, in no group; which only the group of the Triceram with substructure in commercially pure titanium revealed values statistically greater than the rest, revealing that the accelerated artificial aging influenced the color of this group. However, the values of color alteration was smaller than 1, being considered clinically acceptable ; which after the storage in 1.23% acidulated phosphate fluoride was observed increased values of superficial roughness with significant difference between both studied ceramics, as in metal-free samples as in metal-ceramics; which the color alteration, after storage in 1.23% acidulated phosphate fluoride, revealed to all the groups evaluated unacceptable values clinically (&Delta;E > 3.3).

O objetivo deste trabalho foi avaliar o efeito do ambiente de sinterização vácuo e argônio na resistência de união (RUMC) de cerâmicas às ligas de Ni-Cr (Fit Cast SB), Co-Cr (Star Loy C) e titânio comercialmente puro (Tritan). A partir de uma matriz de teflon, foram obtidos 60 padrões de resina/cera em forma de cilindro, com 8 mm de comprimento e 5 mm de diâmetro. Os padrões foram incluídos e os anéis foram levados ao forno e submetidos a ciclos térmicos para a expansão do revestimento. Em seguida, os anéis para fundição em Ni-Cr e Co-Cr foram levados à máquina de fundição por indução eletrônica. Os anéis referentes ao titânio foram levados à máquina de fundição por arco voltaico. Após resfriamento dos anéis, as fundições foram desincluídas e jateadas com óxido de alumínio (100 &mu;m). Depois de recortados dos canais de alimentação, os cilindros metálicos foram preparados para aplicação da cerâmica. Em seguida, foi realizada a aplicação e sinterização da cerâmica à vácuo ou em argônio. Para as ligas alternativas, foi utilizada a cerâmica IPS Classic V e para o titânio, a Triceram. Na sequência, os cilindros compostos pelo metal e disco cerâmico (5 mm de diâmetro e 2 mm de espessura) (n=10) foram submetidos aos ensaios de RUMC por cisalhamento na máquina de ensaios universais com célula de carga de 500 Kg e velocidade do travessão móvel de 0,5 mm/min. Após os ensaios, foram realizadas análises das fraturas por meio de microscopia óptica (MO) (15X) e microscopia eletrônica de varredura (MEV). Os dados de RUMC (MPa) obtidos foram analisados estatisticamente pelos testes ANOVA e Tukey (&alpha;=0,05). Os resultados demonstraram que a sinterização à vácuo propiciou obtenção de maiores valores (MPa) de RUMC (76,58) que a sinterização em argônio (51,31). Quanto às ligas avaliadas, as de Ni-Cr e Co-Cr apresentaram maiores valores de RUMC (71,32 e 71,28, respectivamente) que o titânio cp (49,23); sendo que entre elas não houve diferença estatística. Não houve interação entre os fatores avaliados. De acordo com a MO, houve predomínio de fraturas mistas. Segundo a MEV, os espécimes de Ni-Cr e titânio sinterizados a vácuo apresentaram maior rugosidade de superfície do que os sinterizados em argônio. Para a liga de Co-Cr não houve diferença na topografia de superfície. A sinterização em argônio influenciou negativamente a RUMC dos pares metalocerâmicos analisados. / The aim of this study was to evaluate the effect of firing atmospheres: vacuum and argon on the bond strength of ceramic to Ni-Cr (Fit Cast SB), Co-Cr (Star Loy C) and commercially pure titanium (Tritan) alloys. 60 wax/acrylic resin cylinder patterns (8 mm high and 5 mm in diameter) were prepared on a plastic custom mold for metalceramic bond strength (MCBS) test. The patterns were invested in phosphated investment and manipulated on vacuum. The rings were placed in a furnace to burn out patterns and thermally expand the molds. Then, the rings of Ni-Cr and Co-Cr were placed in an electronic machine to cast. The rings related to titanium were positioned in the casting machine with a voltaic arc. After the rings have cooled, the castings were divested manually and abraded with aluminum oxide particles (100 &mu;m). Then, the cylinders were prepared for applying of the ceramic veneering disks. The ceramic was applied and fired in vacuum and argon atmospheres. IPS-Classic ceramic was used for alternative alloys and for titanium, Triceram ceramic. Then, the cylinders composed of metal and ceramic disk (5 mm diameter and 2 mm height) (n=10) were submitted to metal-ceramic bond strength (MCBS) shear tests on an universal testing machine with load cell of 500 Kg at a crosshead speed of 0.5 mm/min. After the tests, there were made fracture analysis by optic microscopy (OM) and scanning electron microscopy (SEM). The MCBS data (MPa) were statistically analyzed by the ANOVA and Tukey test (&alpha;=0.05). The results indicated that the vacuum firing (76.58) promoted higher MCBS values than argon firing (51.31). Among the metals, Ni-Cr and Co-Cr alloys presented higher MCBS (71.32 e 71.28, respectively) than titanium (49.23); between two base alloys there was no statistical difference. There was no interaction between the evaluated factors. According to MO analysis, there was predominance of mixed fractures. According SEM, the Ni-Cr and titanium specimens submitted to vacuum presented higher surface roughness than the specimens submitted to argon. For Co-Cr, there was no difference of surface topography. The argon firing influenced negatively the MCBS of metal-ceramic evaluated pairs.

A higienização das próteses parciais ou totais removíveis é fundamental para a durabilidade do tratamento e prevenção de patologias orais. O objetivo deste estudo foi avaliar o efeito de agentes higienizadores de prótese na cor, corrosão e rugosidade superficial do titânio c.p., ligas metálicas e resina acrílica termopolimerizável, simulando um período de 180 dias de higienização. Espécimes em formato de discos (12 mm x 3 mm) foram confeccionados em: titânio comercialmente puro (Tritan - Ti c.p.), liga de níquel-cromo-molibdênio-titânio (Vi-Star), liga de níquel-cromo (Fit Cast-SB Plus) e liga de níquel-cromo-berílio (Fit Cast-V). Cada disco fundido foi incluído em mufla previamente preparada por matrizes retangulares de teflon (38 mm x 18 mm x 4 mm), incorporando-se o disco metálico à resina acrílica termopolimerizável. Os corpos-de-prova (n=5) foram imersos em soluções dos agentes higienizadores: hipoclorito de sódio a 0,05%, Periogard, Cepacol, pastilha Corega Tabs, pastilha Medical Interporous e pastilha Polident 3 Minute. Como controle, foi utilizada a água deionizada. Foram realizados ensaios de estabilidade de cor por meio de espectrocolorímetro (Color-guide 45/0), resistência à corrosão por meio da análise visual da presença de manchas no metal e análise da alteração de massa (balança eletrônica analítica), e rugosidade superficial por meio de rugosímetro (Surftest SJ-201P). Além disso, foi realizada análise quantitativa de liberação de íons metálicos por meio de espectrometria de massa com plasma indutivamente acoplado (ICP-MS - ELAN DRC II). Os resultados de estabilidade de cor, alteração de massa e rugosidade foram submetidos à ANOVA e teste de Tukey (p< 0,05). Quanto à estabilidade de cor da resina acrílica termopolimerizável (E), houve diferença estatisticamente significante entre o titânio c.p. e as ligas. A resina associada ao Ti c.p. apresentou menor alteração de cor, enquanto que a resina associada à Fit Cast-SB Plus apresentou a maior alteração de cor (1,33 ± 1,11 e 5,06 ± 1,96, respectivamente). Com relação à presença de manchas no metal, o hipoclorito de sódio causou manchamento nos espécimes das ligas Vi-Star e Fit Cast-V. Quando avaliada a alteração de massa (g), o Cepacol e a pastilha Corega Tabs propiciaram maior perda de massa. Entre os metais, a amostra do Ti c.p. apresentou maior perda de massa. Quanto à rugosidade (Ra, µm) da resina, o Cepacol causou maior rugosidade, enquanto que a pastilha Corega Tabs e o Periogard propiciaram maior lisura no corpo-de-prova. A resina associada ao Ti c.p. e ao Fit Cast-SB Plus apresentaram maior rugosidade. Quanto à rugosidade do metal, os produtos de imersão não influenciaram nos resultados, mas a liga Fit Cast-SB Plus apresentou maior rugosidade após a imersão. A liberação de íons mais expressiva foi constatada nas ligas Vi-Star e Fit Cast-V após a imersão na pastilha Medical Interporous. Pode-se concluir que as ligas Vi-Star e Fit Cast-V podem ser consideradas seguras para a confecção de aparelhos protéticos removíveis, mas com a condição de não utilizar o hipoclorito de sódio a 0,05% ou a pastilha Medical Interporous para a higienização, pois causaram corrosão e maior liberação de íons, respectivamente. / The hygiene care of the removable partial and complete dentures is required for the longevity of the treatment and prevention of oral diseases. The aim of this study was to evaluate the effect of denture cleansers on color, corrosion and surface roughness of the commercially pure titanium, metal alloys and heat-polymerized acrylic resin, simulating a period of 180 days of hygiene. Disk-shaped specimens (12 mm x 3 mm) had been fabricated with commercially pure titanium (Tritan - Ti c.p.), nickel-chromium-molybdenum-titanium alloy (Vi-Star), nickel-chromium alloy (Fit Cast-SB Plus) and nickel-chromium-beryllium alloy (Fit Cast-V). Each cast disc was invested in the flasks previously prepared by Teflon rectangular matrices (38 mm x 18 mm x 4 mm), incorporating the metal disk to the heat-polymerized acrylic resin. The specimens (n= 5) had been immersed in the solutions: sodium hypochlorite 0.05%, Periogard, Cepacol, Corega Tabs, Medical Interporous and Polident 3 Minute. As a control, it was used deionized water. It was accomplished assays of color stability by means of a colorimeter (Color-guide 45/0), corrosion resistance by means of visual analysis of tarnishes on the metal and mass alteration analysis (analytical electronic balance), and surface roughness by means of a surface analyzer (Surftest SJ-201P). Besides, the quantitative analysis of metal ions release was accomplished by means of inductively coupled plasma mass spectrometry (ICP-MS - ELAN DRC II). Color stability, mass alteration and roughness results were submitted to ANOVA and Tukey test (p<0.05). Considering the color stability of the heat-polymerized acrylic resin (E), there were statistically significant difference between the titanium c.p. and the alloys. The resin associated with the Ti c.p. showed lesser color alteration, whereas the resin associated with Fit Cast-SB Plus showed the higher color alteration (1,33 ± 1,11 e 5,06 ± 1,96, respectively). In relation to the presence of tarnishes on the metals, the sodium hypochlorite caused tarnishes on specimens of the Vi-Star and Fit Cast-V alloys. When evaluated the mass alteration (g), Cepacol and Corega Tabs propitiated higher weight loss. Between the metals, the Ti c.p. samples showed greater weight loss. Considering the resin roughness (Ra, µm), Cepacol caused higher roughness, whereas Corega Tabs and Periogard propitiated greater smoothness on the specimens. The resin associated with the Ti c.p. and Fit Cast-SB Plus showed higher roughness. Considering the metal roughness, the immersion products did not influence on the results, but the Fit Cast-SB Plus showed greater roughness after immersion. The ionic release most significant was with the Vi-Star and Fit Cast-V alloys after immersion in Medical Interporous. It could be concluded that the Vi-Star and Fit Cast-V alloys can be considered safe for removable prosthesis finish, but with the condition of do not use sodium hypochlorite 0.05% or Medical Interporous tablet for hygiene, because they caused corrosion and greater ionic release, respectively.

Le titane et ses alliages sont devenus des matériaux incontournables dans l'aéronautique, le domaine biomédical et l'industrie chimique et ce depuis le début des années 1950 en raison de haut rapport résistance/poids, une excellente biocompatibilité et une bonne résistance à la corrosion. La structure hexagonale du titane conduit à une anisotropie intrinsèque, due à la configuration atomique particulière et à une anisotropie extrinsèque, due à une texture marquée produite lors de leur élaboration. Le but de cette étude est d'améliorer la compréhension des mécanismes de déformation (glissement et maclage) dans le titane conduisant à cette anisotropie extrinsèque. Une technique d’essais interrompus in situ en MEB / EBSD a été utilisée lors la déformation plastique d’un alliage de titane T40 commercialement pur afin de suivre l'évolution de l'orientation cristalline et de la morphologie des grains au cours de la déformation sous différents types de chargement (traction, laminage, cisaillement). Cette technique permet de suivre l’apparition du maclage, la croissance et la forme des macles, l’interaction des variants de macles avec les grains voisins. Le Facteur de Schmid, l’orientation cristallographique, l'énergie de déformation plastique, et la déformation localisée liée à l’accommodation ont été calculés pour analyser l'activation du maclage, la croissance des macles, et la sélection de variant de macle. Des variants de macles avec un faible facteur Schmid, facteur qui exprime la force appliquée externe sur le plan de maclage et le long de la direction de maclage, ont été observés. Cela indique le facteur Schmid n'est pas très approprié pour prédire le maclage. Une règle de sélection de variant de maclage a été proposée sur la base de la consommation maximale d'énergie plastique. L'énergie plastique (on suppose le matériau comme étant rigide parfaitement plastique) consommée est calculée de la façon suivante : la déformation que produit chaque variant est exprimée du repère cristal au repère macroscopique ; la contrainte suit une loi de type Hall Petch, le diamètre des grains est alors défini comme la longueur maximale que peut prendre chaque variant dans le grain. Le variant qui consomme le plus d’énergie est activé le premier. Ces calculs sont en bon accord avec l'observation expérimentale : Les variants de macles sélectionnés étaient ceux conduisant à une consommation maximale de l'énergie plastique. Le libre parcours que peut prendre chaque variant est un critère pertinent puisque cela permet d’expliquer les différences observées dans un grain équiaxe ou un grain allongé en terme de nombre de variants présents et croissance des macles. Les essais interrompus in – situ montrent des chaines de macles ou paires de macles (propagation dans 2 ou plusieurs grains voisins). Une macle est activée en premier dans un grain, avec sa croissance, elle impose un champ de contrainte et un champ de déformation dans les grains voisins ce qui peut activer une macle dans les grains voisins. Les paires de macles ont un paramètre de Luster - Morris relativement élevé, ce qui traduit une bonne compatibilité entre les macles et une propagation facile de macle dans les grains voisins. Par une simple transformation du tenseur gradient de déplacement du variant utilisé dans le grain considéré on obtient la déformation imposée dans le grain voisin. Le variant de macle dans ce grain voisin pouvant accommoder le plus facilement la déformation imposée sera activé. Ceci montre que la déformation locale peut influencer l’activation et la sélection de variant de macle / Titanium and its alloys have become backbone materials for aerospace, biomedical field and chemical industries since the early 1950s because of the high strength-weight ratio, excellent biocompatibility, and good corrosion resistance. The hexagonal structure of titanium leads to an intrinsic anisotropy of the particular atomic configuration and extrinsic anisotropy of the texture to a product marked in their elaboration. The purpose of this study is to improve understanding of the deformation mechanisms (slip and twinning) in the titanium leading to the extrinsic anisotropy. Technical testing interrupted in situ SEM / EBSD was used in the plastic deformation of a commercially pure titanium alloy T40 to follow the crystal orientation and morphology of the grains during deformation under different types of loading (tension, rolling). This technique allows following the occurrence of twinning, growth and shape of the twins, the interaction of the twin variants with neighboring grains. Schmid factor, crystallographic orientation, plastic deformation energy, and localized strain accommodation were calculated to analyze the twin activation, the twin growth, and twin variant selection. Twinning variant with relatively low global Schmid factor, which resolves the externally applied force onto the twinning plane and along the twinning direction, were observed. That indicates the global Schmid factor is not very appropriate to predict twinning. A twinning variant selection rule was proposed based on the maximum plastic energy consumption. The plastic energy ( the material is assumed to be perfectly rigid plastic) consumed is calculated as follows: the deformation produced by each variant is expressed from crystal frame to macro frame; stress follows a Hall Petch type rule, the grain diameter is then defined as the maximum length that can take each variant in the grain. The variant which can consume the maximum of the externally imposed energy is expected to twin first. The calculation results show good agreement with the experimental observation: The selected twin variants were the one leading to maximum plastic energy consumption. The variant free path length relevant criterion so indicates the reason why the equiaxed grains and elongated grains have the difference in twin variant number and twinning variant growth. The interrupted in-situ investigation shows that the twin chains or twin pairs observed in this work are a sequential twinning behavior. A twin activated first, with its growth, it imposes a strain field and a stress field into its neighboring grains and possibly stimulate a twin in the neighboring grain. The twin pairs show a good alignment with a relatively high Luster-Morris parameter, which is a measure of the compatibility of twinning systems through a grain boundary. By the displacement gradient tensor transformation, the imposed strain into the neighboring grain was obtained. The twinning variant which can better accommodate the imposed strain can be activated. It indicates that the local strain can influence the twinning activation and variant selection