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Thesis (MScEng (Mechanical and Mechatronic Engineering))--University of Stellenbosch, 2011. / ENGLISH ABSTRACT: The purpose of this study is to investigate the machinability of commercially pure (CP) titanium, manufactured using the press-and-sinter PM process. To this end, CP titanium powder (-200 mesh) was compacted and sintered in vacuum (10-4 torr) for two hours at 1200°C. Small cylindrical samples were compacted at pressures varying from 350 to 600 MPa in order to determine the compressibility of the powder. Following these tests, four larger stepped-cylinder samples were compacted at pressures close to 400 MPa and sintered under similar conditions. These samples had sintered densities varying between 3.82 and 4.41 g/cm3. They were used to evaluate the machinability of the sintered titanium using face turning machining tests. The samples were machined dry, using uncoated carbide (WC-Co) cutting tool. Cutting speeds between 60-150 m/min were evaluated while keeping the feed rate and depth of cut constant at 0.15 mm/rev and 0.5 mm, respectively. The final machined surface finish and the tool wear experienced during the face turning machining tests were monitored in order to evaluate PM titanium’s machining performance. This study showed that it is possible to use the press-and-sinter PM process with CP titanium powder, with a particle size of less than 75 μm (-200 mesh), to manufacture sintered titanium. However, particle shape influences the compressibility of the powder and pressing parts of larger volume, such as the machining test sample shape, is challenging when using such small particle size powder. Processing conditions, such as compaction pressure, sintering temperature and sintering time, influence the sintered density. Results from the machinability tests show that tool wear increases with a decrease in the porosity of the sintered titanium. A more porous sintered material has both lower strength and thermal conductivity. As these factors have opposing effects on the machinability of materials, it is concluded that the strength of the sintered titanium has a stronger influence on its machinability than the thermal conductivity. The cutting tool wear was uniform but showed indications of crater wear. The machined surface of the denser parts had minimal defects compared to less dense parts. Chip shape is long for the dense parts, and spiral for the less dense parts. The chips formed were all segmented, which is typical for titanium. The machinability of the sintered CP titanium was compared to that of wrought titanium alloys. As expected, it was found that the machinability of the sintered titanium was poor in comparison. / AFRIKAANSE OPSOMMING: Die doel van hierdie studie is om die masjineerbaarheid van kommersieel suiwer (KS) titaan, wat deur die pers-en-sinter poeiermetallurgie (PM) metode vervaardig word, te ondersoek. Om hierdie doel te bereik, is KS titaan poeier (-200 ogiesdraad) gekompakteer en gesinter in ‘n vakuum (10-4 torr) teen 1200°C vir 2 ure. Klein silindriese monsters is tussen drukke van 350en 600 MPa gekompakteer om die samedrukbaarheid van die poeier te bepaal. Na aanleiding van hierdie toetse, is vier groter trapvormige-silinder monsters by drukke naby aan 400MPa gekompakteer en onder soortgelyke omstandighede gesinter. Hierdie monsters het gesinterde digthede tussen 3.82 en 4.41 g/cm3 gehad. Hulle is gebruik om die masjineerbaarheid van die gesinterde titaan te ondersoek deur middel van vlak-draai masjineringstoetse. Die monsters is sonder smeermiddel gemasjineer met onbedekte karbied (WC-Co) snygereedskap. Snysnelhede tussen 60 – 150 m/min is geëvalueer terwyl die voertempo en diepte van die snit konstant by 0.15 mm/rev en 0.5 mm, onderskeidelik, gehou is. Die finale gemasjineerde oppervlak afwerking en gereedskapsslytasie tydens die vlak-draai masjinering toets is van die faktore wat gemonitor is sodat PM titaan se optrede tydens masjinering geëvalueer kan word. Hierdie studie wys dat diepers-en-sinter metode wel met KS titaan poeier, met ‘n partikel grootte van minder as 75 μm (-200 maas), gebruik kan word om gesinterde titaan te vervaardig. Die partikelgrootte beïnvloed wel die samedrukbaarheid van die poeier. Die samedrukking van parte met groter volume, soos bv die masjinerings toetsmonster, is uitdagend wanneer klein partikelgrootte poeier gebruik word. Proses omstandighede, soos kompaksie druk, sinteringstemperatuur en sinteringstyd, beïnvloed die gesinterde digtheid. Resultate van die masjineerbaarheidstoetse wys dat beitelslytasie toeneem met ‘n afname in porositeit van die gesinterede titaan. ‘n Meer poreus gesinterde materiaal het beide laer sterkte en termiese geleidingsvermoë. Aangesien hierdie faktore teenoorgestelde uitwerkings op masjineerbaarheid het, word dit dan afgelei dat die sterkte van gesinterde titaan ‘n groter invloed het op sy masjineerbaarheid as die termiese geleidingsvermoë. Die beitel se slytasie is hoofsaahlik, maar het tekens van kraterslytasie getoon. Die gemasjineerde oppervlak van die meer digte onderdele of toetsmonters het min gebreke gehad in vergelyking met die minder digte dele. Die vorm van die spaanders is lank vir digte parte, en spiraalvormig vir minder digte toetsmonsters. Die spaanders wat gevorm het, was almal gesegmenteerd, wat tipies is vir titaan. Die masjineerbaarheid van die gesinterde KS titaan is met dié van gesmede titaanallooie vergelyk. Soos verwag is, is gevind dat die masjineerbaarheid van die gesinterde titaan in vergelyking swak is.

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.

Este trabalho tem como objetivo caracterizar as mudanças microestruturais durante o recozimento isotérmico de um fio de ferro trefilado a frio e de pureza comercial com ênfase no crescimento de grão. Os recozimentos foram realizados no intervalo de 823-1173 K por diversos tempos. As informações estatísticas do tamanho de grão foram obtidas por meio do método dos interceptos lineares. O mapeamento das orientações foi obtido por meio de difração de elétrons retroespalhados (EBSD). O material apresenta uma microestrutura ferrítica e totalmente recristalizada a partir de 873 K. Foram encontrados indícios de crescimento normal de grão a partir de 1023 K, porém este crescimento não evoluiu consideravelmente ao longo do tempo de tratamento. Os resultados obtidos a partir do método dos interceptos lineares demonstram que a distribuição de tamanho de grão segue uma curva próxima à log-normal. Nas amostras recozidas a partir de 1123 K, verificou-se a ocorrência de crescimento anormal de grão. O crescimento anormal de alguns grãos inicia-se na região central do fio, estendendo-se até uma região próxima à superfície do fio. Algumas modificações na dimensão da amostra e na atmosfera de recozimento foram realizadas a fim de se estudar a interação destas variáveis no desenvolvimento dos grãos anormais. Foram identificados indícios morfológicos de que o mecanismo para ocorrência de crescimento anormal foi o molhamento de contornos no estado sólido (solid-state wetting) que depois foram confirmados pelas análises de micro e mesotexturas. A análise de microtextura também revela que o material apresenta duas componentes preferenciais, as fibras || DT e || DT, onde DT é a direção axial de trefilação. A primeira orientação é a mais intensa, sendo que seu fortalecimento parece ser impulsionado pelo crescimento anormal de grão. A segunda é menos intensa e parece estar relacionada com as orientações dos grãos oriundos da recristalização primária. Aspectos teóricos e analíticos sobre o crescimento de grão são apresentados e associados aos resultados experimentais e à literatura. / This Dissertation aims follow the microstructural changes occurring during isothermal annealing of commercially-pure cold-drawn iron wire, with emphasys on grain growth phenomena. The grain size data were obtained by means of the linear intercept method. The orientations scanning were done by means of electron backscatter diffraction patterns (EBSD). Isothermal annealing was performed within the temperature range 823 - 1173 K for several times. The material displays full recrystallization at temperatures above 873 K. Normal grain growth was observed above 1023 K, although this growth did not evolve through longer annealing times. The results of the linear intercept method show the grain size distribution has a log-normal shape. For samples annealed above 1123 K, abnormal grain growth occurs. The first signs of secondary recrystallization appear close to the center of the wire, growing towards the surface. Changes in the wire diameter and annealing atmosphere were performed to assess the effect of these variables on abnormal grain growth. Results point out that abnormal grain growth is driven by solid-state wetting. These morphological observations were also confirmed by micro and mesotexture analyses. The microtexture also shows the presence of two major fiber texture components || WD and || WD, were WD is the axial wire-drawn direction. The first one is the most intense and its strengthening seems to be related with abnormal grain growth. The second one is weaker and it seems to be most related with small primary recrystallized grains. Theoretical and analytical features about grain growth are presented and discussed in light of literature and experimental results.

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.