Thesis (MScEng)--Stellenbosch University, 2014. / ENGLISH ABSTRACT: Surface seals are widely used in South Africa. There are a number of reasons which include affordability, versatility and durability. There are, however, in some cases problems with stone loss that can lead to a shortened lifespan of the pavement. The loss of aggregate chippings in surface seals poses a major problem in the seal pavement industry. This study aims to identify the influencing factors that lead to these adhesive failures as well as to find optimum combinations of binders and aggregates at various conditions. Various binders commonly used in South African surface seal construction will be tested using the Bitumen Bond Strength (BBS) test method. The binders used in the study include 80/100 penetration grade bitumen, elastomer modified bitumen, bitumen rubber, elastomer modified emulsion and cationic rapid setting emulsion. Aggregates used in the study include dolerite, granite and quartzite. The test samples were cured and tested at two temperatures, 15 °C and 35 °C. The samples were also cured for 2, 6 and 24 hours respectively. The study tackles a wide range of variables in order to obtain a good understanding of adhesion properties of surface seals used in South Africa. Tests were repeated at least once to ensure repeatability and in some cases up to four repeats were performed. The loading rate at which the tests were performed had a significant influence on the BBS results. This rate varied which complicated the process of comparing the results. It was therefore decided to unify the loading rates. The BBS results exposed the difference between hot applied binders and emulsions. The former having significant stronger adhesion properties. It was also confirmed by the results that temperature plays a key role in the BBS results due to the visco-elastic properties of bitumen. These influences will be discussed along with others such as aggregate types and curing times. The type of failure is also discussed. Failure can either be adhesive or cohesive, the former being a failure between the aggregate and the binder while the later refers to a failure in the binder itself. The results of other students will also be discussed and compared to the results of this study. These include results of predecessors that tested emulsions as well as results from tests done on fractured aggregate surfaces and precoated aggregates. This study showed very similar results as these from other students, except for tests done with emulsions. It was discovered that the method of curing of the emulsions must be adapted to ensure proper curing of the emulsions. It was found that aggregates did not influence the BBS properties to the same extent as temperature and binder application type. The BBS results of hot applied binders also did not significantly increase as the curing time increased, but the results of emulsions showed some increase. However, the emulsions needed more time to cure properly. / AFRIKAANSE OPSOMMING: Oppervlak seëls word algemeen gebruik in Suid-Afrika. Daar is verskeie redes hiervoor waaronder bekostigbaarheid,veelsydigheid en duursaamheid. Daar is egter in sommige gevalle probleme met klipverlies wat kan lei tot n verkorte leeftyd. Hierdie klipverlies ontstaan as gevolg van verskeie redes of kombinasies daarvan. Die studie beoog om hierdie faktore wat die adhesie eienskappe beïnvloed te identifiseer sowel as om optimum kobinasies van bindmiddels en klipsoorte te bewerkstellig by verkeie kondisies. ‘n Verskeidenheid van bindmiddels wat algemeen in Suid-Afrika gebruik word, word in die studie getoets met die Bitumen Bond Sterkte (BBS) toets metode. Die bindmiddels wat in die studie gebruik word sluit 80/100 penetrasie graad bitumen, elastomeer gemodifiseerde bitumen, bitumen rubber, elastomeer gemodifiseerde emulsie en kationiese snel settende emulsie. Die klipsoorte wat vir die studie gebruikword is doleriet, graniet en kwartsiet. Hierdie gesteentes word algemeen in die praktyk gebruik. Die toets monsters word ook by twee temperature gekuur en getoets. Hierdie temperature is 15 °C en 35 °C. Die toets monsters word ook onderskeidelik vir 2, 6 en 24 uur gekuur. Die studie ondersoek 'n wye verskeidenheid van veranderlikes om sodoende 'n goeie begrip van adhesie eienskappe van die oppervlak seëls wat in Suid-Afrika gebruik word te verkry. Elke toets was ten minste een maal herhaal om herhaalbaarheid te verseker. Sommige toetse was tot 4 keer herhaal. Die belasting tempo van die toetse het ‘n beduidende uitwerking op die BBS resultate as gevolg van die visko-elastiese eienskappe van bitumen. Hierdie tempo het gewissel en dit moeilik gemaak om die resultate te vergelyk. Daarom was daar besluit om die tempo van die toetse te verander na ‘n gelykvormige tempo. Daar was ‘n duidelike verskil in BBS resultate van die warm toegepaste bindmiddels en die emulsies. Die warm bindmiddels het baie hoër BBS resultate gelwer. Dit was ook bevestig in die resultate dat temperatuur ‘n beduidende rol speel in die BBS. Hierdie invloede sal bespreek word tesame met ander, soos klipsoorte en kuring tye. Die tipe versaking word ook bespreek. Versaking kan plaasvind as gevolg van adhesie of cohesie, waar adhesie versaking 'n versaking is tussen die klip en die bindmiddel terwyl cohesie versaking verwys na 'n versaking in die bindmiddel self. Die uitslae van die ander studente sal ook bespreek word en vergelyking word met die resultate van hierdie studie. Dit sluit die resultate van voorgangers in wat emulsies getoets het sowel as die resultate van toetse wat gedoen is op gebreekte klipoppervlaktes en bitumen behandelde klippe. Hierdie studie het baie soortgelyke resultate getoon as dié van ander studente, behalwe vir die toetse wat gedoen was met emulsies. Daar is vasgestel dat die metode van kuring van die emulsies moet aangepas word om behoorlike kuring van die emulsies te verseker. Daar is ook gevind dat klipsoorte nie die BBS eienskappe in dieselfde mate as temperatuur en bindmiddel toepassingstipe beïnvloed het nie. Die BBS resultate van warm aangewende bindmiddels het ook nie aansienlik verhoog soos die kuringstyd toegeneem het nie, maar die resultate van emulsies het wel 'n toename getoon. Die emulsies het wel meer tyd nodig gehad om behoorlik te kuur.

<p>U uvodnom delu doktorske disertacije opisuje se kompleksnost problematike kori&scaron;ćenja polimera za bazu zubne proteze, sa osvrtom na njihove op&scaron;te osobine, stepen biokompatibilnosti i njihove mehaničke karakteristike. Detaljno je opisana problematika ispitivanja stomatolo&scaron;kih materijala i napravljeno je poređenje i korelacija između in vitro i in vivo načina ispitivanja biokompatibilnosti. Drugi deo obuhvata ispitivanje čvrstoće polimera za bazu zubne proteze i analizu uticaja osobina materijala u odnosu na biolo&scaron;ku sredinu u kojoj obavljaju svoju funkciju, i u odnosu na sile kojima su tokom funkcije materijali izloženi. Cilj doktorske disertacije je utvrđivanje stepena biokompatibilnosti i mehaničkih karakteristika toplopolimerizujućih, hladnopolimerizujućih i termoplastičnih akrilata za bazu zubne proteze. Istraživanje je obuhvatilo 3 komercijalna materijala iz grupe akrilata, koji se razlikuju po hemijskom sastavu i načinu polimerizacije. Ispitivanje biokompatibilnosti rađeno je u in vitro i in vivo uslovima. Ispitivanje na ćelijskim kulturama obuhvatalo je dve ćelisjke linije (MRC 5 i L929) sa dva načina kontakta između ćelija i materijala (direktan, indirektan) i dva načina određivanja biolo&scaron;kog ishoda (MTT test, Agar difuzioni test). Istraživanje urađeno in vivo obuhvatalo je test subkutane implantacije, na animalnom modelu pacova, i test iritacije oralne sluzokože na animalnom modelu hrčka. Oba testa rađena su u skladu sa standardom ISO 10993. Cilj in vivo istraživanja bio je ispitivanje reakcije tkiva na implantirani materijal, računajući i zavr&scaron;nu integraciju ili dezintegraciju implantiranog materijala. Prednost in vivo istraživanja nalazi seu analizi uticaja materijala na sterilno živo tkivo, uz praćenje imunolo&scaron;ke reakcije, kao dopuna prethodnom istraživanju na ćelijskim kulturama. Dopunski deo in vivo ispitivanja biokompatibilnosti određen je prema kliničkoj upotrebi ispitivanih materijala, zbog čega je odabran test oralne iritacije sluzokože. Sluzokoža bukalne kesice sirijskog hrčka sastoji se od pločasto slojvitog epitela sa orožavanjem, &scaron;to je predstavljao dobar model za ispitivanje polimera za bazu zubne proteze, po&scaron;to zubna proteza naleže na sluzokožu nepca i rezidualnog alveolarnog grebena koja takođe orožava. Drugi deo disertacije obuhvatao je ispitivanje mehaničkih karakteristika, pri čemu su urađeni test zatezne čvrstoće, test savojne čvrstoće, test čvrstoće loma i mikrotvrdoće, uz dopunsku analizu pratećih parametara. Rezultati ispitivanja biokompatibilnosti pokazali su da su testovi biokompatibilnosti osetljivi na upražnjeni metodolo&scaron;ki postupak. Ispitivanjem na ćelijskim kulturama nisu utvrđene značajne razlike u citotoksičnosti između toplopolimerizujućih, hladnopolimerizujućih i termoplastičnih akrilata. Takođe, rezultati su se razlikovali u odnosu na tip ćelijske kulture i način provere biolo&scaron;kog ishoda, &scaron;to se slaže sa prethodnim navodima o kompleksnoj problematici njihovog međusobnog poređenja. Ispitivanjem biokompatibilnosti subkutanom implantacijom praćen je inflamatorni odgovor tkiva u vremenskom intervalu od 90 dana. Reakcija organizma na implantirani materijal posmatrana je kroz ćelijske i tkivne parametre, u skladu sa ISO 10993. Dodatno je urađena i analiza hrapavosti implantiranih materijala. Histolo&scaron;kom analizom utvrđena je razlika u inflamatornom odgovoru u odnosu na kori&scaron;ćeni materijal, kao i prema vremenskom intervalu implantacije. Test oralne iritacije sluzokože nije se pokazao kao dovoljno senzitivan za ispitivanje ovih vrsta materijala. Ispitivanjem mehaničkih karakteristika utvrđene su razlike između toplopolimerizujućih, hladnopolimerizujućih i termoplastičnih akrilata. Najveći stepen čvrstoće utvrđen je kod toplopolimerizujućih akrilata dok je najveća konzistentnost rezultata bila u grupi termoplastičnih akrilata. Prezentovano istraživanje predstavlja prvu detaljnu analizu biokompatibilnosti i mehaničkih karaktestistika polimera za bazu zubne proteze.</p> / <p>The introduction describes the complexity of use of denture base materials, with regard to their general characteristics, biocompatibility and mechanical properties. Issues related to the testing of dental materials is described in detail and comparison is made between in vitro and in vivo methods of biocompatibility testing. The second part further covers the determination of strength of previously used materials, in relation to biological environment in which their function is conducted and in relation to the influence of masticatory forces which can contribute to their mechanical failure. The aim of the presented research was to assess the degree of biocompatibility and mechanical properties of cold curing, hot curing and thermoformed denture base materials. The research included three denture base materials, which differed according to their chemical composition and polymerization protocols. The biocompatibility testing was carried out in in vitro and in vivo conditions. The in vitro experiments covered two different cell lines (MRC 5 human lung fibroblasts and L929 mouse fibroblasts) with two types of contact (direct, indirect) and two different types of quantification of biological outcome (MTT assay and Agar overley test). The in vivo assessment of biocompatibility covered the subcutaneous implantation test, on the animal model of Wistar rat, and oral mucosa irritation test, on the animal model of sirian hamster. Both tests were conducted according to the ISO 10993. The aim of the in vivo investigation was to evaluate tissue reactions to the implanted materials, including the final integration or disintegration of the tested materials. The advantage of in vivo investigation included the possibility of monitoring the materials influence on living tissues, with the analysis of imunological response as an addition to the previously conductedresearchon cell cultures. The supplemental part of in vivo investigation was chosen according to the clinical use of the tested materials, which included the oral mucosa irritation test.The mucosa of hamster buccal pouch consists of stratified squamos epithelium, which is considered to be an adequate replacement for the human denture supporting tissues, which also consist of the same type of epithelium. The second part of thesis includes the determination of mechanical properties of denture base materials. It consists of four types of tests: tensile strength test, bending strength test, fracture toughness test and microhardness tests, followed by the analysis of corresponding parameters. The results of the biocompatibility tests showed that the biological outcome of the applied method is highly depended on the methodological procedure. The investigation conducted in vitro, on two different cell lines, did not show significant difference in cytotoxicity between hot curing, cold curing and thermoformed denture base materials. Also, the results were influenced by the type of cell culture and the evaluation method of biological outcome, which agrees with the previous allegations about the complexicity of their mutual comparison. The subcutaneous implantation test covered the inflammatory response in the time period of 90 days. The organism reaction to the implanted material was determined through the cell and tissue parameters of organism response, evaluation of which was conducted according to the ISO 10993. Additionally, the surface roughness of the implanted specimens of materials was also measured. The inflammatory response of the ogranism was influenced by the type of the implanted material and the time interval of implantation. The oral mucosa irritation test has proven not to be sufficiently sensitive for testing of this type of materials. Testing of the mechanical properties od denture base materials, revealed the difference between the cold curing, hot curing and thermofomed denture base materials. The highest strength was observed in hot curing materials, while the highest consistency of the results was observed in thermoformed resins. The presented investigation presents the first detail analysis of the biocompatibility and mechanical properties of the denture base materials, and as such presents a novelty in the field of dental materials characterization.</p>

A utilização do titânio em odontologia tem aumentado devido suas propriedades mecânicas, biocompatibilidade, resistência à corrosão e baixo peso específico. Entretanto, o uso do titânio em próteses ainda não é rotineiro em virtude de dificuldades no processo de fundição. Uma das maneiras de superar estas dificuldades seria através do desenvolvimento de novas ligas cujo ponto de fusão fosse inferior ao do Ti cp. O objetivo deste estudo foi avaliar as propriedades mecânicas, biológicas e microestrutura de ligas experimentais de titânio para utilização em estruturas metálicas de próteses dentárias, após fundição odontológica, comparando-as ao Ti cp. As ligas experimentais avaliadas foram Ti-5Zr(%p), Ti-5Ta(%p) e Ti-5Ta-5Zr(%p). Os corpos-de-prova foram fundidos por arco voltaico em atmosfera de argônio e injeção por vácuo-pressão. Para avaliação das propriedades mecânicas, corpos-deprova em forma de halteres foram submetidos a ensaios de tração, barras foram submetidas a ensaios de flexão para avaliação do módulo de elasticidade, e hemi-esferas e discos foram submetidos ao teste de desgaste de dois corpos, sendo o perfil das amostras avaliado antes e após o teste para cálculo da perda de altura vertical. Discos foram utilizados para avaliação da microdureza e para caracterização microestrutural. Para avaliação das propriedades biológicas, células SCC9 foram cultivadas em meio de cultura D-MEM/HF12 suplementado sobre discos e poços sem discos foram usados como controle. Após períodos de 1, 4, 7, 10 e 14 dias, foi avaliada a proliferação celular pelo método histoquímico MTT. Aos 7 dias foi avaliada a viabilidade celular após marcação com azul de Trypan e contagem em hemocitômetro. A morfologia celular foi avaliada às 2, 12 e 24 horas através da visualização, em microscópio de fluorescência por epiluminação, do citoesqueleto de actina e dos núcleos, usando, respectivamente, faloidina e DAPI. Os resultados foram submetidos a testes estatísticos e a liga Ti-5Ta apresentou resistência à tração menor que as demais e módulo de elasticidade significativamente menor do que o Ti cp, embora não diferente das demais ligas experimentais. Com relação à resistência à abrasão, as ligas experimentais apresentaram desgaste significativamente menor do que o Ti cp e a liga Ti-5Zr apresentou microdureza significativamente maior do que os demais materiais. Não houve diferença na proliferação e na viabilidade celular entre os materiais. A avaliação da morfologia celular mostrou diferença na proporção de células nos diferentes estágios de desenvolvimento nos períodos de 2 e 12 horas, mas não em 24 horas. O Ti cp apresentou microestrutura do tipo feather-like com fase &alpha;, enquanto Ti-5Zr apresentou estrutura do tipo Widmanstätten com fase &alpha; e &alpha;´. As ligas Ti- 5Ta e Ti-5Ta-5Zr apresentaram as fases &alpha;, &alpha;´, &alpha;´´ e &beta;, com arranjos lamelar e acicular, respectivamente. Os resultados deste estudo sugerem que as ligas estudadas apresentam potencial para aplicação em próteses dentárias, uma vez que suas propriedades biológicas foram semelhantes às do Ti cp, comprovado por proliferação, viabilidade e morfologia celular; e suas propriedades mecânicas, como resistência à abrasão, microdureza e resistência à tração foram satisfatórias, ainda que o módulo de elasticidade possa e deva ser melhorado. / The use of titanium in dentistry have increased due to its mechanical properties, biocompatibility, corrosion resistance and density. However, titanium has not been routinely used because of the difficulties related to casting technique. One of the options to solve these difficulties would be to develop new titanium alloys whose melting point was lower than cp Ti. So, the aim of this study was to evaluate the mechanical and biological properties and microstructure of experimental titanium alloys for prosthesis frameworks, after dental casting, comparing to cp Ti. The experimental alloys evaluated were Ti-5Zr(%w), Ti-5Ta(%w) and Ti-5Ta-5Zr(%w). The samples were cast by voltaic arc in argon atmosphere and vaccum/pressure injection. To evaluate the mechanical properties, dumbbell-shaped samples were submitted to tensile test, slab-shaped were submitted to flexure for modulus of elasticity evaluation, and stylus tips and disks were submitted to two-body wear test, evaluating the profile of the samples before and after the test to calculate vertical height loss. Disks were used for microhardness evaluation and microstructural observation. For the biological properties evaluation, SCC9 cells were cultured in D-MEM/HF12 supplemented on the disks and wells without disks were used as control. After 1, 4, 7, 10 and 14-day period, cell proliferation was measured by MTT method. After 7 days, cell viability was evaluated after Trypan blue marking and counting in a hemacytometer. Cell morphology was evaluated in 2, 12 and 24-hour periods examining, in fluorescence microscope under epifluorescence, actin cytoskeleton and cell nuclei, using, respectively, phalloidin and DAPI. The results were submitted to statistical analysis and Ti-5Ta alloy presented ultimate tensile strength lower than the others and modulus of elasticity statistically lower than cp Ti, but no different to the other experimental alloys. In relation to wear resistance, the experimental alloys presented wear significantly lower than cp Ti and the Ti-5Zr alloy presented microhardness greater than other materials. Cell morphology evaluation showed difference in the proportion of cells in the different stages in 2 and 12-hour periods, but not in 24. The cp Ti presented feather-like structure with &alpha; phase while Ti-5Zr presented a Widmanstätten structure with &alpha; and &alpha;´ phases. The Ti-5Ta and Ti-5Ta-5Zr alloys presented &alpha;, &alpha;´, &alpha;´´ and &beta; phases with lamellar and acicular structures, respectively. The results of this study suggest that the studied alloys could be applied in dental prosthesis, once their biological properties were similar to cp Ti in cell proliferation, viability and morphology; and their mechanical properties, like wear resistance, microhardness and ultimate tensile strength were ideal, although the modulus of elasticity can and should be improved.

Nenhuma / A espectroscopia Mössbauer de 57Fe é uma técnica nuclear, não-destrutiva, utilizada na investigação das propriedades estruturais, magnéticas e hiperfinas de diferentes materiais sólidos. Trata-se, portanto, de uma poderosa ferramenta de caracterização de materiais na física, metalurgia, geologia e biologia, particularmente em materiais magnéticos, ligas metálicas e minerais contendo Fe. Na atualidade, a Espectroscopia Mössbauer de Elétrons de Conversão (CEMS) é amplamente utilizada no estudo de filmes finos e ultrafinos, bem como outros materiais nanoestruturados. No caso de nanoestruturas magnéticas, estudos a baixas temperaturas (LT) são particularmente importantes devido à possibilidade de efeitos oriundos do fenômeno do superparamagnetismo. Neste trabalho foi desenvolvido um sistema de medição CEMS a baixas temperaturas (< 20 K) utilizando um Channeltron (multiplicador de e-) e um Criostato ótico (Modelo SVT-400 da Janis Research Co, EUA) tendo como base um detector originalmente desenvolvido no Departamento de Física Aplicada / Espectroscopia Mössbauer da Universidade de Duisburg-Essen, Alemanha. O detector LTCEMS foi construído, testado e aplicado com sucesso num estudo preliminar de caracterização de bicamadas Fe/(EuxPb1-x)Te(111) com uso de camada sonda de 57Fe de apenas 15Å, obtendo resultados a temperaturas de até 8 K na amostra. / The 57Fe Mössbauer spectroscopy is a nuclear, non-destructive technique used for the investigation of structural, magnetic and hyperfine properties of several materials. It is a powerful tool in characterizing materials in physics, metallurgy, geology and biology field areas, especially magnetic materials, alloys and minerals containing Fe. Lately, the Conversion Electron Mössbauer Spectroscopy (CEMS) is widely used in making studies on ultra-thin magnetic films, as well as other nanoestructured materials. In case of magnetic nanostructures, low temperature (LT) studies are especially important due to the possibility of dealing with superparamagnetic effects. In this work it was developed a CEMS measurement system for low temperatures (< 20K) based on a solid-state electron multiplier (Channeltron) and an optical cryostat (Model SVT-400, Janis Research Co, USA), from which the project was originally conceived at the Applied Physics / Mössbauer Spectroscopy Department from University of Duisburg-Essen, Germany. The LT-CEMS system was fully built, tested and successfully applied in a preliminary characterization of Fe/(EuxPb1-x)Te(111) bilayers with use of a 15 Å, 57Fe probe layer, with reasonable results at sample temperatures as low as 8 K.

A utilização do titânio em odontologia tem aumentado devido suas propriedades mecânicas, biocompatibilidade, resistência à corrosão e baixo peso específico. Entretanto, o uso do titânio em próteses ainda não é rotineiro em virtude de dificuldades no processo de fundição. Uma das maneiras de superar estas dificuldades seria através do desenvolvimento de novas ligas cujo ponto de fusão fosse inferior ao do Ti cp. O objetivo deste estudo foi avaliar as propriedades mecânicas, biológicas e microestrutura de ligas experimentais de titânio para utilização em estruturas metálicas de próteses dentárias, após fundição odontológica, comparando-as ao Ti cp. As ligas experimentais avaliadas foram Ti-5Zr(%p), Ti-5Ta(%p) e Ti-5Ta-5Zr(%p). Os corpos-de-prova foram fundidos por arco voltaico em atmosfera de argônio e injeção por vácuo-pressão. Para avaliação das propriedades mecânicas, corpos-deprova em forma de halteres foram submetidos a ensaios de tração, barras foram submetidas a ensaios de flexão para avaliação do módulo de elasticidade, e hemi-esferas e discos foram submetidos ao teste de desgaste de dois corpos, sendo o perfil das amostras avaliado antes e após o teste para cálculo da perda de altura vertical. Discos foram utilizados para avaliação da microdureza e para caracterização microestrutural. Para avaliação das propriedades biológicas, células SCC9 foram cultivadas em meio de cultura D-MEM/HF12 suplementado sobre discos e poços sem discos foram usados como controle. Após períodos de 1, 4, 7, 10 e 14 dias, foi avaliada a proliferação celular pelo método histoquímico MTT. Aos 7 dias foi avaliada a viabilidade celular após marcação com azul de Trypan e contagem em hemocitômetro. A morfologia celular foi avaliada às 2, 12 e 24 horas através da visualização, em microscópio de fluorescência por epiluminação, do citoesqueleto de actina e dos núcleos, usando, respectivamente, faloidina e DAPI. Os resultados foram submetidos a testes estatísticos e a liga Ti-5Ta apresentou resistência à tração menor que as demais e módulo de elasticidade significativamente menor do que o Ti cp, embora não diferente das demais ligas experimentais. Com relação à resistência à abrasão, as ligas experimentais apresentaram desgaste significativamente menor do que o Ti cp e a liga Ti-5Zr apresentou microdureza significativamente maior do que os demais materiais. Não houve diferença na proliferação e na viabilidade celular entre os materiais. A avaliação da morfologia celular mostrou diferença na proporção de células nos diferentes estágios de desenvolvimento nos períodos de 2 e 12 horas, mas não em 24 horas. O Ti cp apresentou microestrutura do tipo feather-like com fase &alpha;, enquanto Ti-5Zr apresentou estrutura do tipo Widmanstätten com fase &alpha; e &alpha;´. As ligas Ti- 5Ta e Ti-5Ta-5Zr apresentaram as fases &alpha;, &alpha;´, &alpha;´´ e &beta;, com arranjos lamelar e acicular, respectivamente. Os resultados deste estudo sugerem que as ligas estudadas apresentam potencial para aplicação em próteses dentárias, uma vez que suas propriedades biológicas foram semelhantes às do Ti cp, comprovado por proliferação, viabilidade e morfologia celular; e suas propriedades mecânicas, como resistência à abrasão, microdureza e resistência à tração foram satisfatórias, ainda que o módulo de elasticidade possa e deva ser melhorado. / The use of titanium in dentistry have increased due to its mechanical properties, biocompatibility, corrosion resistance and density. However, titanium has not been routinely used because of the difficulties related to casting technique. One of the options to solve these difficulties would be to develop new titanium alloys whose melting point was lower than cp Ti. So, the aim of this study was to evaluate the mechanical and biological properties and microstructure of experimental titanium alloys for prosthesis frameworks, after dental casting, comparing to cp Ti. The experimental alloys evaluated were Ti-5Zr(%w), Ti-5Ta(%w) and Ti-5Ta-5Zr(%w). The samples were cast by voltaic arc in argon atmosphere and vaccum/pressure injection. To evaluate the mechanical properties, dumbbell-shaped samples were submitted to tensile test, slab-shaped were submitted to flexure for modulus of elasticity evaluation, and stylus tips and disks were submitted to two-body wear test, evaluating the profile of the samples before and after the test to calculate vertical height loss. Disks were used for microhardness evaluation and microstructural observation. For the biological properties evaluation, SCC9 cells were cultured in D-MEM/HF12 supplemented on the disks and wells without disks were used as control. After 1, 4, 7, 10 and 14-day period, cell proliferation was measured by MTT method. After 7 days, cell viability was evaluated after Trypan blue marking and counting in a hemacytometer. Cell morphology was evaluated in 2, 12 and 24-hour periods examining, in fluorescence microscope under epifluorescence, actin cytoskeleton and cell nuclei, using, respectively, phalloidin and DAPI. The results were submitted to statistical analysis and Ti-5Ta alloy presented ultimate tensile strength lower than the others and modulus of elasticity statistically lower than cp Ti, but no different to the other experimental alloys. In relation to wear resistance, the experimental alloys presented wear significantly lower than cp Ti and the Ti-5Zr alloy presented microhardness greater than other materials. Cell morphology evaluation showed difference in the proportion of cells in the different stages in 2 and 12-hour periods, but not in 24. The cp Ti presented feather-like structure with &alpha; phase while Ti-5Zr presented a Widmanstätten structure with &alpha; and &alpha;´ phases. The Ti-5Ta and Ti-5Ta-5Zr alloys presented &alpha;, &alpha;´, &alpha;´´ and &beta; phases with lamellar and acicular structures, respectively. The results of this study suggest that the studied alloys could be applied in dental prosthesis, once their biological properties were similar to cp Ti in cell proliferation, viability and morphology; and their mechanical properties, like wear resistance, microhardness and ultimate tensile strength were ideal, although the modulus of elasticity can and should be improved.

Os magnetos de Neodímio Ferro Boro (Nd2Fe14B) apresentam excelentes propriedades magnéticas e compatibilidade biológica, embora sejam frágeis e possuam baixa resistência à corrosão. As forças de atração magnética de magnetos de terras raras têm sido empregadas em sistemas de retenção, principalmente associadas aos implantes osseointegráveis, em próteses bucais e próteses faciais, bem como em aparelhos ortodônticos. Este estudo avalia o comportamento das forças de repulsão magnética, em função do volume e comprimento do eixo magnético, quando submetidos a afastamentos, de modo que esta propriedade física seja empregada em odontologia. Vinte e quatro corpos de prova, com um ou dois pares de magnetos de Nd2Fe14B, com diferentes formas e volumes variados, foram submetidos a ensaio mecânico para mensuração das forças de repulsão magnética, em condições de afastamentos que variaram entre 0,0 e 20,0 mm. Os dados observados mostram que, considerando-se uma mesma área superficial de polo, a força de repulsão magnética varia em função do comprimento do eixo magnético. Os dados relativos ao afastamento foram submetidos a análise de variância (p0,05), tendo-se observado que o aumento da distância entre os magnetos diminui significantemente a força de repulsão magnética na maioria dos corpos de prova. No afastamento 0,0 mm as forças magnéticas de repulsão dos subgrupos mantêm uma sequência crescente a partir do subgrupo de menor volume de magnetos ao subgrupo de maior volume de magnetos, os quais permanecem nessa sequência nos afastamentos iniciais. A força de repulsão magnética gerada por magnetos pequenos varia menos em função do aumento do afastamento. Conclui-se que a variação da força de repulsão magnética, dada a mesma área superficial de polo, apresenta uma relação direta com o volume e com o eixo magnético onde, quanto maior o volume ou o comprimento do eixo magnético, maior a força de repulsão magnética. A relação direta entre volume e força de repulsão magnética não se altera frente aos afastamentos inicais, tendendo a se tornar imensurável com o aumento da distância. A força de repulsão magnética mantém uma relação inversa com a distância entre os pares de magnetos. Este ensaio mecânico indica que a força de repulsão magnética apresenta, assim como a força de atração magnética, uma curva hiperbólica de redução frente ao aumento do afastamento. / Neodymium Iron Boron (Nd2Fe14B) magnets exhibit excellent magnetic properties and demonstrate biological compatibility, despite of their fragility and low resistance to corrosion. The magnetic attraction forces of rare earth magnets have been used in retention systems mainly associated with osseointegrated implants, in oral and facial prostheses, as well as orthodontic appliances. This study evaluates the repulsion forces of magnets, varying volume and length of magnetic axis when subjected to vertical distance, in order to assess the usefulness of such physical property in clinical situations. Twenty-four specimens, with one or two pairs of Nd2Fe14B magnets, presenting different shapes and various volumes, were subjected to mechanical testing so as to measure magnetic repulsion forces, under conditions of vertical pole face separation ranging from 0.0 to 20.0 mm. Repulsive magnetic force varies depending on the length of the magnetic axis, when considering the same surface area of a pole. Analysis of Variance - (p0.05) indicated that by increasing the distance between the pairs of magnets, magnetic repulsion force significantly reduces in most of the specimens. Starting at a 0.0 mm distance, the magnetic repulsion forces keep an enhancing sequence from lower to higher magnetic volume, holding these characteristics during initials distances. Repulsion magnetic forces generated by small magnets varies less as the distance increases. The results indicate the repulsion magnetic force variation, fixing the same pole surface area, presenting a direct relationship between volume and magnetic axis, since the increase of the volume or of the magnetic axis length leads to a higher magnetic repulsive force. The relationship between volume and magnetic repulsion force does not vary at initial distance. Nevertheless, when such distance increases, the force between the magnets significantly decreases. The magnetic repulsion force holds an inverse relationship with respect to the distance between magnets pairs. This mechanical test indicates that the magnetic repulsion force, as well the magnetic attraction force, present a hyperbolic curve of force reduction due to the increasing vertical distance.

Orientador: Paulo Sérgio Cerri / Banca: Lea Assed Bezerra da Silva / Banca: Mario Tanomaru Filho / Resumo: Perfurações radiculares acidentais ocorrem em cerca de 2-12% dos dentes tratados endodonticamente. Estas perfurações causam injúria aos tecidos periodontais adjacentes e, frequentemente, promovem a invasão bacteriana culminando com a inflamação do ligamento periodontal e reabsorção óssea podendo levar a perda do elemento dental. Dentre os materiais indicados para o selamento destas perfurações, o MTA tem sido largamente usado. O MTA é basicamente composto por silicatos de cálcio (80%) e óxido de bismuto (Bi2O3; 20%), usado como agente radiopacificador. Silicato tricálcico (STC) é um biomaterial utilizado associado ao óxido de zircônio (ZrO2) e o óxido de nióbio (Nb2O5) é um radiopacificador alternativo. O objetivo deste estudo foi avaliar a resposta dos tecidos periodontais promovida pelo silicato tricálcico puro (Mineral Research Processing, Meyzieu, França) associado ao ZrO2 ou ao Nb2O5 comparando-os ao MTA-Angelus, em perfuração de furca de molares de ratos. Foram utilizados 80 ratos, distribuídos em 4 grupos: GS (sham), STC+ZrO2, STC+Nb2O5 e GMTA, de acordo com o material de selamento. No grupo GS, as perfurações no assoalho da câmara pulpar não foram seladas. O acesso da cavidade foi restaurado com cimento de ionômero de vidro fotopolimerizável. Os 1os molares esquerdos, sem perfurações no assoalho da câmara pulpar, foram usados como controle (GC). Após os períodos de 7, 15, 30 e 60 as maxilas foram removidas, fixadas, descalcificadas e incluídas em parafina. Os cortes c... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Accidental radicular perforation occurs in about 2-12% of endodontically treated teeth. These perforations lead to injury of periodontal tissues and frequently promote bacterial invasion inducing to periodontal ligament inflammation and bone resorption may lead to tooth loss. Among the materials suitable for the sealing of these perforations, the MTA has been widely used. MTA is basically composed of calcium silicate (80%) and bismuth oxide (Bi2O3, 20%), a radiopacifying agent. Tricalcium silicate (TCS) is a biomaterial used associated with zirconium oxide (ZrO2) and niobium oxide (Nb2O5) is an alternative radiopacifier. Our purpose was to evaluate response of the periodontium adjacent to furcation perforations in rat molars filled with pure tricalcium silicate (Mineral Research Processing, Meyzieu, France) associated with ZrO2 or Nb2O5 and MTA-Angelus. Eighty rats were distributed into four groups: SG (sham), TCS+ZrO2, TCS+Nb2O5 and MTAG according to the sealing material. In the SG group, the perforations in the pulp chamber floors were not sealed. The access cavity was restored with light-cure glass-ionomer cement. The left upper first molars, without perforations in the pulp chamber floors, were used as controls (CG). After 7, 15, 30 and 60 days, fragments of maxilla were fixed, decalcified and embedded in paraffin. In the HE-stained sections, the volume density of inflammatory cells (VvIC), fibroblasts (VvFb) and blood vessels (VvBV) was obtained. The width of the periodo... (Complete abstract click electronic access below) / Mestre

Reembasadores resilientes temporários contendo fármacos antifúngicos foram sugeridos como um tratamento adjunto para estomatite protética. No entanto, antes de utilizar clinicamente estes reembasadores modificados em humanos, é importante avaliar a sua biocompatibilidade em modelos animais. Este estudo avaliou a biocompatibilidade in vivo de um reembasador resiliente temporário para base de prótese (Trusoft) modificado por agentes antimicrobianos em suas mínimas concentrações inibitórias (MCIs) para biofilme de Candida albicans. Dispositivos acrílicos intra-orais (DIOs) foram confeccionados individualmente para 60 ratos Wistar. Os ratos foram divididos em 6 grupos (n=5): 3 grupos controle (Negativo: sem DIO; Geral: DIO sem reembasamento; Positivo: DIO reembasado com Trusoft sem fármacos) e 3 grupos experimentais (DIOs reembasados com Trusoft modificados por fármacos em suas respectivas MCIs: 0,032 g de nistatina, 0,064 g de diacetato de clorexidina e 0,128 g de cetoconazol). Os ratos com ou sem os DIOs foram eutanasiados após 7 e 14 dias de avaliação. A análise histopatológica qualitativa foi realizada comparando-se fotomicrografias de secções histológicas, que foram obtidas utilizando um microscópio óptico que abrangeu transversalmente a região intermolares. As alterações morfológicas no epitélio e queratina foram analisadas quantitativamente através da realização de planimetria computadorizada. Os dados quantitativos foram analisados utilizando ANOVA 2-fatores e teste de Tukey (=0,05). A análise quantitativa mostrou que apenas o grupo com DIO contendo cetoconazol diminuiu significativamente a espessura e a área do estrato córneo em comparação com os outros grupos (p<0,05), que não apresentaram diferenças significativas entre si (p>0,05). Estes resultados estiveram de acordo com os obtidos para análise qualitativa. A incorporação de MCIs de nistatina e diacetato de clorexidina no Trusoft não induziram alterações histopatológicas na mucosa palatina de ratos, sugerindo a biocompatibilidade in vivo deste protocolo para o tratamento de estomatite protética. / Temporary resilient denture liners containing antifungal drugs have been suggested as an adjunct treatment for denture stomatitis. However, before clinically using these modified liners in humans, it is important to assess their biocompatibility in animal models. This study evaluated the in vivo biocompatibility of a temporary soft denture liner (Trusoft) modified by antimicrobial agents at their minimum inhibitory concentrations (MICs) for biofilm formation by Candida albicans. Methods: Acrylic intraoral devices (IODs) were individually made for 60 Wistar rats. The rats were divided into the following 6 groups (n=5): 3 control groups (Negative: without IOD; General: IOD without relining; Positive: IOD relined with Trusoft without drugs) and 3 experimental groups (IOD relined with Trusoft modified by drugs at MICs: 0.032 g for nystatin, 0.064 g for chlorhexidine diacetate, and 0.128 g for ketoconazole). The rats with or without the IODs were sacrificed after 7 or 14 days of evaluation. Histopathological qualitative analysis was performed by comparing photomicrographs of histological sections, which were obtained using an optical microscope that transversely covered the inter-molar region. Morphological changes in the epithelium and keratin were quantitatively analyzed by performing computerized planimetry. Quantitative data were analyzed using 2-way ANOVA and Tukey\'s test (=0.05). Quantitative analysis showed that only the group with IOD containing ketoconazole significantly decreased the thickness and area of the stratum corneum compared with the other groups (p<0.05), which showed no significant differences between each other (p>0.05). These results were in accordance with those obtained for qualitative analysis. Incorporation of MICs of nystatin and chlorhexidine diacetate in Trusoft did not induce histopathological changes in the palatal mucosa of rats, suggesting the in vivo biocompatibility of this protocol for treating denture stomatitis.

Introduction: The aim of this study was to evaluate some of the physico-chemical properties of a new root canal sealer. Methodology: The sealers tested were Sealer Plus (MKLife, Porto Alegre, Rio Grande do Sul, Brazil), compared as AH Plus (Dentsply, DeTrey GmbH, Konstanz, Alemanha). For the radiopacity, flow, solubility and fabrication of test specimens relative to setting times the ANSI/ADA No. 57 (2000) and ISO 6876 (2012) specifications were followed. To measure the initial and final setting times the ASTM C266/2008 standard was used. pH was evaluated in the time intervals of 3, 24, 72 and 168 hours). Statistical tests were applied to the results obtained at a level of significance of 5%. Results: The results demonstrated that the Sealer Plus sealer showed a lower radiopacity value than AH Plus sealer (p<0.05), however, this was higher than the minimum value recommended by the specifications; that is 3 mm Al. Relative to flow, the value for Sealer Plus was 19.19 mm and for AH Plus, 19.81 mm (p>0.05). Sealer plus presented initial and final setting times of 138 min. and 210 min., respectively, while the values for AH Plus were 437 min. and 849 min., respectively, (p<0.05). Relative to solubility, Sealer Plus presented 0.21% and AH Plus, 0.27% (p>0.05). None of the sealers showed a significant increase in pH (p>0.05). Conclusion: Sealer Plus sealer presented physico-chemical properties in accordance with ANSI/ADA (2000) No.57 and ISO 6876 (2012) specifications. / Introdução: Este estudo objetivou avaliar algumas propriedades físico-químicas de um novo cimento obturador de canais radiculares. Metodologia: Para os testes de radiopacidade, escoamento, solubilidade e confecção dos corpos de prova para os tempos de presa foram seguidas as especificações nº57 da ANSI/ADA (2000) e ISO 6876 (2012). Para a medição dos tempos de presa, inicial e final, foi empregada a norma ASTM C266/2008. O pH foi avaliado nos períodos de 3, 24, 72 e 168 horas. Sobre os resultados foram aplicados testes estatísticos com nível de significância de 5%. Resultados: Os resultados demonstraram que o cimento Sealer Plus apresentou menor radiopacidade do que o cimento AH Plus (p<0.05), porém, superior ao mínimo recomendado pelas especificações, ou seja, de 3 mm de Al. Com relação ao escoamento, o do Sealer Plus foi 19,19 mm e do AH Plus 19,81 mm (p>0.05). O Sealer Plus apresentou tempos de presa inicial e final de 138 min. e 210 min., respectivamente, enquanto o AH Plus, 437 min. e 849 min., respectivamente, (p<0.05). Em relação à solubilidade, o Sealer Plus apresentou 0,21% e o AH Plus 0,27% (p>0.05). Nenhum dos cimentos apresentou aumento significativo do pH (p>0.05). Conclusão: O cimento Sealer Plus apresentou propriedades físico-químicas de acordo com as especificações nº 57 da ANSI/ADA (2000) e ISO 6876 (2012).

A challenging application space exists for high-aspect-ratio, high-fidelity dielectrics in micro-electro-mechanical system (MEMS), microelectronic, and photonic applications. Photosensitive polymers are widely used in these fields because they are relatively easy to process and pattern, and have good mechanical properties. Photosensitive polynorbornene (PNB)-based dielectrics have been shown to have high sensitivity, excellent photodefinition properties, and high mechanical strength making them suitable for MEMS, microelectronic packaging, and photonic applications. PNB-based dielectrics can be functionalized with epoxide, carboxylic acid, or fluorinated alcohol groups. Epoxy or carboxylic acid groups can be used to provide cross-linkable sites, resulting in improved chemical and thermal properties while fluorinated alcohol groups can provide solubility in aqueous base. The focus of this study has been on the epoxy-based cross-linking of ultraviolet and electron beam (e-beam) sensitive negative-tone PNB-based dielectrics. The impact of multifunctional epoxy-based additives on the cross-linking, photolithographic properties, and adhesion properties of the photosensitive PNB dielectric was investigated. High aspect ratio features of 13:1 (height:width) were produced in 40 µm thick films (a single coat) with straight side-wall profiles and high fidelity. Contrast values as high as 33.4 were obtained at doses below 15 mJ/cm2. To evaluate the polymer's suitability to MEMS and microelectronics applications, epoxy cross-linking reactions were studied as a function of processing condition through Fourier transform infrared spectroscopy (FTIR), nanoindentation, swelling and dielectric measurements. The fully cross-linked films had an elastic modulus of 2.9 GPa and hardness of 0.18 GPa which can improve the mechanical compliance of the packaging device. To explore the feasibility of the PNB dielectric as a highly sensitive e-beam resist for nano scale fabrication, the e-beam initiated reaction between PNB cross-linking sites and the multifunctional epoxy cross-linkers was investigated. In this study, the interaction of an e-beam with the PNB mixture and its compounds was investigated. The contrast, photodefinability, and e-beam activation of the components in the PNB formulations were studied. The PNB polymer had very high e-beam sensitivity and contrast. It was shown that the addition of a photoacid generator (PAG) to the polymer-epoxy mixture enhanced the contrast and sensitivity. Formulations with the additional cross-linker showed improved contrast, sensitivity, and substrate adhesion. 100 nm structures with 13.5 nm line edge roughness (LER) were fabricated. The influence of the developing time, the developer concentration, PEB, and film thickness on the contrast and sensitivity were studied. Structures with contrast values as high as approximately 8 were fabricated at doses as low as 0.38 µC/cm2. The acid-catalyzed epoxy ring opening reaction of the PNB dielectric was studied using FTIR spectroscopy. The photo and thermal acid generation initiated epoxy ring opening reactions and subsequent cross-linking of polymer. Additionally, polymer properties were characterized as a function of processing conditions for this polymer system. It was shown that thermal cure conditions have a substantial impact on the mechanical and electrical properties of the polymer. The rate and ultimate conversion of the epoxy ring opening reaction increased with increasing cure temperature, resulting in a higher degree of cross-linking at cure temperatures above 140°C. Degradation reactions occurred at temperatures above 160°C, indicating loss of epoxide cross-linking groups and linkages. These hypotheses were supported by electrical and mechanical property studies. It was shown that curing the PNB polymer at 160°C for 1 h after develop resulted in full epoxy ring opening and highest cross-link density. This sample showed lower dielectric constant (3.9), residual stress (20 MPa), and solvent swelling (3.1%). Variable frequency microwave (VFM) processing of the PNB dielectric was studied to investigate the rapid curing of the polymer at lower temperatures. The FTIR results showed that the microwave reaction rates were higher at each isothermal cure temperature compared to convective heating, indicating that the rapid VFM curing of PNB at low temperatures is feasible. The PNB film was fully cross-linked after 15 min VFM cure at the low temperature of 150˚C. The shortest time to fully cure the polymer was found to be 5 min at 160°C. Also, the feasibility of rapid VFM curing of PNB in air was studied. All samples VFM-cured (140˚C-180˚C) in air showed no signs of oxidation. The electrical and mechanical properties of VFM-cured films were characterized and compared with thermally cured films to determine the effectiveness of the VFM processing. VFM-cured samples showed higher degree of cross-linking than thermally-cured samples, which was congruent with the FTIR results. Improved or equivalent properties were obtained for VFM-cured samples at shorter cure cycles and lower cure temperatures compared to thermally-cured films. The PNB dielectric was also used as an overcoat material to make micro and nano fluidic channels. In this work, incorporation of advanced micro/nano fluidics with high-sensitivity photonic sensors was demonstrated. 500 nm to 50 µm channels were fabricated by thermal decomposition of epoxy-based PNB polymers. Microdisks with quality factors of over 106 were presented in complementary metal-xide-semiconductor (CMOS) compatible SiN on oxide technology. These ultra-high quality factor SiN resonators were demonstrated in the visible range for the first time. The fluidic structures were interfaced with photonics for index and florescence sensing. This study was a collaboration with Dr. Ehsan Shahhosseini from the Photonics Group at Georgia Tech.