Submitted by ANA CAROLINA DE OLIVEIRA SOUZA null (carol.odonto@yahoo.com.br) on 2016-03-30T18:03:40Z No. of bitstreams: 1 TESE DOUTORADO ANA CAROLINA SOUZA.pdf: 3241026 bytes, checksum: 2c360076e32b60dc4d62310a77a7e869 (MD5) / Approved for entry into archive by Juliano Benedito Ferreira (julianoferreira@reitoria.unesp.br) on 2016-04-01T14:37:32Z (GMT) No. of bitstreams: 1 souza_aco_dr_sjc.pdf: 3241026 bytes, checksum: 2c360076e32b60dc4d62310a77a7e869 (MD5) / Made available in DSpace on 2016-04-01T14:37:32Z (GMT). No. of bitstreams: 1 souza_aco_dr_sjc.pdf: 3241026 bytes, checksum: 2c360076e32b60dc4d62310a77a7e869 (MD5) Previous issue date: 2016-02-19 / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / O objetivo deste trabalho foi avaliar o comportamento de cimentos resinosos experimentais reforçados com fibras de nylon (N6) e de nylon com nanotubos de carbono de parede múltipla (N6+CNT). A hipótese testada foi de que a distribuição das fibras seria capaz de melhorar as propriedades mecânicas dos compósitos, resultando em um efetivo reforço dos cimentos resinosos. As fibras foram produzidas pela técnica da eletrofiação para caracterização e para a imersão na matriz resinosa e posterior obtenção das partículas, utilizadas em quatro diferentes frações de massa (2,5; 5,0; 10,0 e 20,0%). Também foi preparado um grupo controle, sem adição de partículas e um grupo matriz, onde as partículas sem nanofibras foram utilizadas. Foram realizados os testes de resistência à flexão, módulo de elasticidade, contração de polimerização, grau de conversão e espessura do cimento. Também foi realizada a caracterização das fibras obtidas. Os resultados mostraram que todos os grupos apresentaram espessura de cimentação aceitáveis de acordo com a norma ISO 4049. As fibras de N6+CNT apresentaram distribuição bimodal, com fibras de maior diâmetro em relação as fibras de N6. As partículas de todos os grupos mostraram-se irregulares, aglomeradas e com grande variação de tamanho, entretanto as fibras de N6 +CNT mantiveram-se mais alinhadas, o que pode ter levado aos maiores valores de resistência, de maneira que as menores concentrações (2,5 e 5,0%) parecem ser mais favoráveis. O acréscimo de partículas sem nanofibras foi capaz de aumentar a resistência dos cimentos resinosos devido a um significativo aumento do grau de conversão. Com relação aos valores do módulo de elasticidade, todos os grupos apresentaram valor de módulo estatisticamente maior, quando comparados com o grupo controle, porém não apresentaram diferenças entre si em relação ao tipo e concentração de partícula. Podemos concluir que com a utilização de cargas orgânicas de nylon associadas a nanotubos de carbono foi possível obter a melhoria das propriedades mecânicas dos cimentos resinosos. / The aim of this study was to evaluate the behavior of experimental resin cement reinforced with nylon fibers (N6) and nylon with multiwalled carbon nanotubes (CNT + N6). The hypothesis was that the distribution of fibers would be able to improve the mechanical properties, reinforcement the resin cements. The fibers were produced by electrospinning technique for characterization and for immersion of fibers in the resin matrix and obtainment of the particles used in four different mass fractions (2.5, 5.0, 10.0 and 20.0%). It was also prepared a control group without addition of particles and the matrix group, where the particles without nanofibers were used in different concentrations to eliminate the effect of pre-polymerized matrix. Were tested the flexural strength, elastic modulus, shrinkage, degree of conversion and thickness of the cement. It also were characterized the fiber obtained. The results showed that all groups had acceptable cement thickness in accordance with ISO 4049 and that the selected parameters for the electrospinning, the fibers showed no beads. The fibers with N6 + CNT had a bimodal distribution, with the larger diameter fibers than the N6 fiber. The particles of all groups were irregular, agglomerated and with great size variation, however the fibers N6 + CNT remained more aligned, which might explain the higher values of flexural strength and the lower concentrations (2.5 and 5.0%) appear to be more favorable. The particles without fibers was able to increase the resistance of the resin cement due to a significant increase in the degree of conversion. All groups showed statistically higher elastic modulus value than the control group, but did not differ among themselves with respect to the type and particle concentration. It is possible to conclude that the use of organic fillers with nylon and carbon nanotubes improved mechanical properties of the resin cements. / FAPESP: 2014/00668-4

Submitted by Lucas Jorge Affonço (lucas_jorgeaffonco@yahoo.com.br) on 2018-09-25T18:16:47Z No. of bitstreams: 1 Dissertação_POSMAT_LucasJorgeAffonco.pdf: 1122070 bytes, checksum: 3aa8bf900f18ab0cc3c2d9fdbbc0ce2e (MD5) / Rejected by Lucilene Cordeiro da Silva Messias null (lubiblio@bauru.unesp.br), reason: Solicitamos que realize uma nova submissão seguindo as orientações abaixo: 1 - Inserir no corpo do texto uma cópia da ata de defesa, pois é um item obrigatório. Agradecemos a compreensão on 2018-09-26T13:33:08Z (GMT) / Submitted by Lucas Jorge Affonço (lucas_jorgeaffonco@yahoo.com.br) on 2018-09-26T13:39:25Z No. of bitstreams: 1 Dissertação_POSMAT_LucasJorgeAffonco.pdf: 1731555 bytes, checksum: 7c7c9ba43b8b832af33307bef8e74d22 (MD5) / Approved for entry into archive by Lucilene Cordeiro da Silva Messias null (lubiblio@bauru.unesp.br) on 2018-09-26T17:02:25Z (GMT) No. of bitstreams: 1 affonço_lj_me_bauru.pdf: 1731555 bytes, checksum: 7c7c9ba43b8b832af33307bef8e74d22 (MD5) / Made available in DSpace on 2018-09-26T17:02:25Z (GMT). No. of bitstreams: 1 affonço_lj_me_bauru.pdf: 1731555 bytes, checksum: 7c7c9ba43b8b832af33307bef8e74d22 (MD5) Previous issue date: 2018-07-26 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / O nitreto de titâno apresenta uma vasta gama de aplicações. Entre elas destacam-se as aplicações em recobrimento de superfícies que exploram características mecânicas tais como dureza e módulo de elasticidade do material para aplicações em biomateriais. Essas características e suas correlações com a microestrutura são investigadas, nesse trabalho, em função dos parâmetros de deposição de filmes de TiN. Os filmes foram depositados pela técnica de magnetron sputtering reativo em rádio frequência, sobre substratos de titânio, de sílica, de silício e de uma liga de titânio-nióbio. Nas deposições, foi utilizado um alvo de titânio puro e misturas gasosas de argônio e nitrogênio, com diferentes fluxos de nitrogênio. As potências empregadas foram de 240 W e 300 W, com diferentes tempos de deposição. Medidas de taxa de deposição e emissão óptica do plasma auxiliaram na escolha dos parâmetros de deposição. As análises das difrações de raios X mostraram que com o aumento do fluxo de nitrogênio os cristalitos tendem a apresentar uma orientação preferencial com os planos (200) do TiN paralelos à superfície do substrato, além de indicar a presença de strain nos filmes. Medidas de nanoindentação foram realizadas nas amostras, com o intuito de obter a dureza e o módulo de elasticidade dos filmes depositados com diferentes fluxos de nitrogênio. Buscando assim determinar a influência do fluxo sobre as propriedades mecânicas e a microestrutura dos filmes. Verificou-se que a dureza nas amostras depositadas a 10 sccm foi a maior, variando de 10 a 18 GPa de acordo com a profundidade de penetração, sendo essa amostra a que apresentou maior textura de orientação favorecendo os planos (200). O módulo de elasticidade foi maior para a amostra de 8 sccm, em torno de 140 GPa, sendo essa a amostra que apresentou maior strain compressivo. Verificou-se que a técnica de sputtering reativo é versátil para o crescimento dos filmes de nitreto de titânio, e que o fluxo de nitrogênio usado nas deposições é um parâmetro de grande impacto nas características mecânicas e estruturais dos filmes obtidos. / The titanium nitride (TiN) has mechanical properties that are useful in a wide range of applications. In special, it is being investigated to improve the surfaces of bone implants. The mechanical properties of TiN films deposited by reactive magnetron sputtering and their correlations with microstructure will be investigated in this dissertation as a function of the deposition parameters. The films were deposited in titanium, silica, silicon and titanium-niobium substrates. A pure titanium target and a mix of argon and nitrogen gases were used in the depositions. The influence of the variation of the reactive gas fluxes on the mechanical properties and in the microstructure of the films were investigated, for applied powers of 240 W and 300 W at 13.6 MHz. Deposition rate and plasma optical emission measurements helped to control the deposition parameters. X ray diffraction analysis show that all films present compressive strain and, at high nitrogen fluxes, a preferred crystallite orientation of planes (200) parallel to the substrate surface occurs. Nanoidentation measurements were performed, for different nitrogen fluxes, to obtain the hardness and elastic modulus of TiN films. The hardness of films deposited at 10 sccm, varied between 10 and 18 GPa, as a function of the penetration depth, and is higher than the observed in other samples. These films also showed the higher (200) plane texture. The elastic modulus is higher on films deposited at 8 sccm N2 flow (around 140 GPa). These films also showed the higher compressive strain. It was checked that the reactive sputtering is a resourceful technique for titanium nitride deposition, and nitrogen flux present a high impact in the structure and mechanical properties of the deposited films.

O objetivo deste trabalho foi avaliar a dureza e o módulo de elasticidade da região de adesão quando utilizados diferentes sistemas adesivos e uma resina composta imediatamente após o procedimento adesivo e após 6 meses de armazenamento, correlacionando esses valores com a resistência adesiva à dentina humana. Para isso foram medidos a dureza e o módulo de elasticidade da resina composta junto à área de união, da camada de adesivo, da camada híbrida, e da dentina adjacente utilizando testes de nanoendentação. Foram utilizados 40 molares humanos hígidos (n=10). Os dentes foram preparados de modo a obterem-se superfícies planas em dentina, sobre as quais os sistemas adesivos foram aplicados seguindo as instruções dos fabricantes. Foram utilizados quatro sistemas adesivos de diferentes formas de aplicação (Adper Scotchbond Multiuso, Adper Single Bond 2, Adper SE Plus e Clearfil SE Bond). Sobre essas superfícies foram inseridos incrementos de resina composta perfazendo 5 mm de altura. Após 24h de armazenamento em água destilada à 37ºC. Os dentes restaurados foram seccionados para obterem-se corpos-de-prova com área aderida de 1mm2. Dos corpos de prova viáveis, 2 palitos centrais de cada dente foram selecionados para análise da nanodureza e do módulo de elasticidade da interface adesiva. Os demais tiveram a resistência de união testada através do teste de microtração, sendo metade desses corpos de prova armazenados durante 6 meses em água à 37ºC. Foi aplicado o teste estatístico ANOVA para dois fatores para todas as variáveis do estudo. Para o fator tempo foi detectada diferença estatística entre os grupos para a resistência adesiva (p=0,042), para o módulo de elasticidade do adesivo (p=0,000) e nanodureza do adesivo (p=0,000), sendo os valores mais baixos observados após 6 meses de armazenamento. Para o fator adesivo, todos os grupos apresentaram diferenças estatísticas (p=0,000), exceto para a variável nanodureza da camada híbrida (p=0,255). O sistema adesivo Clearfil SE Bond apresentou os melhores valores para resistência adesiva e módulo de elasticidade da camada híbrida, juntamente com o sistema Scothbond Multiuso. Os piores desempenhos foram demonstrados pelo sistema adesivo Adper SE Plus. Para a interação, apenas a variável nanodureza do adesivo apontou diferença entre os grupos (p=0,028). O teste de correlação de Pearson detectou correlação significante para as variáveis de módulo de elasticidade, sendo negativa para o módulo de elasticidade do adesivo e positiva para o módulo de elasticidade da camada híbrida. A metodologia e os resultados apresentados permitem-nos concluir que as propriedades mecânicas estudadas (resistência adesiva, módulo de elasticidade do sistema adesivo e da camada híbrida, nanodureza do sistema adesivo e da camada híbrida) podem variar dependendo do sistema adesivo utilizado e do tempo de armazenamento após o procedimento adesivo ter sido realizado. Além disso, quanto maior o módulo de elasticidade da camada híbrida apresentado por um sistema adesivo maior será sua resistência adesiva e menor será o módulo de elasticidade apresentado pela camada de adesivo. / The aim of this study is to evaluate hardness and elasticity module of adhesive region of adhesive systems of different formulations immediately and 6 moths after the adhesive procedures. Those values will be compared to microtensile bond strength to human dentin. The hardness and elasticity module of composite resin next to adhesion region, adhesive layer, hybrid layer and dentin were evaluated. Forty sound human molars were used and prepared in order to obtain flat dentin surfaces in which the adhesive systems were applied following manufactures instructions (n=10). The groups were divided according the four adhesive systems: Adper Scotchbond Multipurpose, Adper Single Bond 2, Adper SE Plus and Clearfil SE Bond. Resin blocks of 5mm were constructed in those surfaces. After 24h of storage in distilled water at 37°C restored teeth were sectioned in order to obtain specimen with a bonded area of around 1mm2. Two specimen of each tooth were submitted to nanohardness and elasticity module test of adhesive interface. Half of the specimen were immediately submitted to the test with a crosshead speed of 0,5mm/min until fracture, the other specimen were stored for additional 6 month in 37ºC water prior to the test. The values resulting of all variables of the study were compared using ANOVA two-way. For the time factor, it was detected statiscal difference between groups in microtensile bond strength values (p=0,042), adhesive elastic modulus (p=0,000) and adhesive nanohardnes (p=0,000), the lowest values were observed in 6 months of storage. For adhesive factor, all groups presented statistical difference (p=0,000), except hybrid layer nanohardness (p=0,255). Clearfil SE bond and Scothbond systems presented the best values of bond strength and hybrid layer elastic modulus. The worse performance was demonstrated by Adper SE Plus adhesive system. For the interaction, only the adhesive nanohardness presents difference between groups (p=0,028). The Pearson correlation test detected positive correlation with microtensile bond strength tests and hybrid layer elastic modulus and negative correlation with bond strength and adhesive elastic modulus. The methodology and the results allow us to conclude that the studied mechanical properties (bond strength, modulus of elasticity of the adhesive and hybrid layer, nanohardness adhesive system and the hybrid layer) may vary depending on the adhesive system and time storage after the bonding procedures have been performed. Moreover, when an adhesive system presents a high elastic modulus of hybrid layer, it will present a high bond strength and low elastic modulus of adhesive layer.

O objetivo principal foi investigar se o osso cortical apresenta comportamento bimodular, ou seja, se os valores de módulo de elasticidade (E) dependem do tipo de carregamento que o método utiliza. Para alcançá-lo foi preciso: (1) \"calibrar\" os diferentes métodos em um material conhecidamente unimodular, para afastar a possibilidade de erros ligados à execução de um método. (2) Depurar os métodos já calibrados para torná-los exequíveis em osso cortical. O que foi feito em espécimes de resina composta, que é um material unimodular e com E parecido com o do osso cortical. Foi investigado se o método de medida interfere no valor do E obtido neste material (pois, pelas informações da literatura, existia uma dúvida consistente). Finalmente, (3) foi avaliado se o método de medida, a região anatômica e o indivíduo interferem nos valores de E em espécimes de osso cortical. Adicionalmente, (4) verificou-se a possibilidade de se encontrar e validar uma correlação entre E e dureza Knoop (KH), para medir o E de resinas compostas indiretamente. Espécimes de latão (n = 5) tiveram o seu E calculado por quatro métodos estáticos diferentes (flexão em três pontos; tração; compressão e método de Marshall), que foram calibrados até que todos medissem o valor esperado; os valores de cada método foram comparados por análise de variância de medidas repetidas (o método foi o fator vinculado e o nível de significância foi de 5%). Espécimes (n = 4) de cinco marcas diferentes de resina composta, também foram submetidos aos quatro métodos, fazendo as adaptações pertinentes (depuração), e tiveram o seu E calculado. Estes valores foram submetidos à análise de variância de medidas repetidas (o método foi o fator vinculado e o nível de significância foi de 5 %). Espécimes (n = 48) obtidos em diferentes regiões (periósteo, endósteo e \"transversal\") de fêmures de quatro bois diferentes tiveram seu E calculado através dos métodos devidamente depurados (flexão em três pontos, tração indireta e compressão). Os valores de E foram submetidos a análises de variâncias (nível de significância de 5 %) para avaliar a influência do método, da região e do indivíduo (bois diferentes) sobre os valores de E. O método experimental de tração não foi utilizado para analisar o comportamento bimodular, porque durantes os ensaios com osso cortical, ele apresentou valores com viés. Por isso, os valores de tração foram calculados de forma indireta (Eti) através de uma equação e dos valores experimentais de flexão em três pontos (Eb) e compressão (Ec). Para validar o uso de valores de Eti, eles foram comparados com os respectivos valores de tração experimental (Et) calculados previamente nos espécimes de resinas compostas por análise de variância de medidas repetidas, e não foram achadas diferenças significantes (p > 0,05). Para encontrar e validar a correlação entre E e KH, os valores médios de E em cada espécime de resina (média do E obtido nos 4 métodos em cada espécime) foram submetidos ao teste de correlação de Pearson (nível de significância de 5%) com os respectivos valores experimentais de dureza Knoop (KH) e foi obtida uma equação de regressão linear. Para validar a equação foi confeccionado um segundo grupo de espécimes de resina (de marcas diferentes das utilizadas anteriormente) que teve seu E calculado pelo ensaio de flexão (Eb) e pela equação de regressão proposta previamente (Er); verificou-se então se a correlação entre estes valores (Eb x Er) era significante (nível de significância de 5 %), e se a nova reta de regressão apresentava coeficiente angular não diferente de 1, e coeficiente constante não diferente de zero (critérios de validação). A análise de variância não apontou diferença significante (p > 0,05) entre os valores de E calculados para o metal pelos 4 métodos, e os valores obtidos não diferiram do E conhecido do latão (ao redor de 100 GPa). As depurações necessárias foram realizadas e com elas os diferentes métodos calcularam o E dos espécimes de resina composta de modo consistente: a análise de variância encontrou diferenças significantes (p < 0,05) entre marcas (cujos E médios cobriram a faixa entre 3 e 20 GPa) e não significantes entre os 4 métodos (p > 0,05). Nos espécimes de osso cortical o valor de E foi significantemente dependente (p < 0,05) do método de obtenção (Eti > Eb > Ec). O E dos espécimes obtidos na região \"transversal\" foi menor que o E dos espécimes obtidos na região do endósteo (p < 0,05); no entanto, não houve diferença significante (p > 0,05) entre o E dos espécimes obtidos nas regiões do endósteo e periósteo e entre o E dos espécimes obtidos nas regiões do periósteo e \"transversal\". Ao considerar somente os valores obtidos no ensaio de compressão (Ec), um dos indivíduos apresentou valores de E maiores que os demais (p < 0,05). As médias de E (dos quatro métodos) em cada espécime de resina apresentaram correlação significante com os respectivos valores de KH (p < 0,05) e a equação de regressão linear: E = 0,1602 KH. Também foi significante (p < 0,05) a correlação dos valores de Eb com os respectivos valores de Er (calculados pela regressão E = 0,1602 KH); além disso, a reta de regressão linear desta nova correlação (Eb = 1,0088Er + 0,0475) apresentou coeficiente angular não diferente de 1 e coeficiente constante não diferente de zero. Pode-se concluir que: (1) Quatro métodos de medir o E apresentaram resultados semelhantes em um material metálico. (2) Estes mesmos métodos foram depurados com sucesso para sua utilização em espécimes de osso cortical ao constatar que também não interferiram no valor do E obtido em espécimes semelhantes aos de osso, confeccionados com resinas compostas. (3) Os valores de E de osso cortical dependem do método de medida, o que demonstra seu comportamento bimodular. A região anatômica e o indivíduo também afetam os valores de E dos espécimes de osso cortical (o indivíduo só foi um fator significante ao considerar somente os valores obtidos no ensaio de compressão). (4) Foi encontrada e validada uma correlação entre E e KH em resinas compostas, que permite calcular o E deste material através da regressão E = 0,1602 KH. / The main objective was to investigate whether the cortical bone has a bimodular behavior, that is, if the values of elastic modulus (E) depend on the load type used by the method. To achieve this, it was necessary: (1) \"calibrate\" the different methods in a material with well-known unimodular behavior, for excluding the possibility of systematic errors in the execution of the methods. (2) Depurate the calibrated methods to make them executable in cortical bone. This was made on specimens of composite resin, which is a unimodular material and has an E similar to that of cortical bone. It was also investigated if the method of measuring the E influences the obtained value in this material (because there was a consistent doubt in the literature). Finally (3), we assessed whether the E values in cortical bone are influenced by the measurement method, by the anatomical region and by the individual. Additionally, (4) it was verified if it would be possible suggesting and validating a correlation between E and Knoop hardness (KH), to indirectly measure the E of composite resins. Brass specimens (n = 5) had their E calculated by four different static methods (three point bending, tensile, compression and Marshall\'s method), which were calibrated until all the methods were capable of measuring the expected value; the E values of each method were compared by analysis of variance of repeated measures (the method was the linked factor and the significance level was 5%). Specimens (n = 4) of five different composite resins were also subjected to the four methods, making the relevant adjustments (depuration), and had their E calculated. These values were subjected to analysis of variance of repeated measures (the method was the linked factor and the significance level was 5%); Specimens (n = 48) obtained in different regions (periosteum, endosteum and \"transverse\") of bovine femurs from four different individual had their E calculated using the depurated methods (three point bending, indirect tensile and compression). The E values were subjected to analyzes of variance (significance level of 5%) to evaluate the influence of the method, of the region and of the individual (different cattle) in the E values. The experimental tensile method was not used to analyze the bimodular behavior because during tests on cortical bone, this method showed values with bias. Therefore, the tensile values were indirectly calculated (Eti) by a formula and by the experimental values of E calculated by three point bending (Eb) and compression (Ec). To validate the use of Eti values, they were compared with the corresponding tensile experimental values (Et) previously measured in the composite resins specimens by analysis of variance (repeated measures), and no significant difference was found (p > 0.05). For suggesting and validating the correlation between E and KH, the average values of E of each composite specimen (mean of E obtained considering the values of the four methods in each specimen) were submitted to the Pearson\'s correlation test (significance level of 5 %) with the corresponding experimental KH values and it was obtained the linear regression equation. To validate this equation, it was made a second group of composite resins specimens (with different brands of the previously used) in which the E was calculated by three point bending test (Eb) and by regression equation previously proposed (Er); then it was checked whether the correlation between these values (Eb x Er) was significant (significance level of 5 %), and if the new regression line showed angular coefficient no different from one, and constant coefficient no different from zero (validation criteria). The analysis of variance showed no significant difference (p > 0.05) among the E values calculated for the metal specimens by the four methods; the obtained values did not differ from the known E of the brass (about 100 GPa). The necessary adjustments (depuration) were made and then the different methods calculated the E of the composite resin specimens consistently: the analysis of variance found significant difference (p < 0.05) between composite brands (whose E mean covered the range between 3 and 20 GPa) and no significant difference among the four methods (p> 0.05). In the specimens of cortical bone, the E values were significantly dependent (p < 0.05) of the obtainment method (Eti > Eb> Ec). The E values of the \"transversal\" specimens were lower than the endosteum specimens (p < 0.05); but there was no significant difference (p > 0.05) between the E of endosteum specimens and periosteum specimens and between the E of periosteum specimens and \"transversal\" specimens. When considering just E values of the compression method, one cattle showed higher E values than the others (p < 0.05). The mean of the four methods for each specimen composite resin exhibited a significant correlation with the respective KH values (p < 0.05) and the linear regression equation: E = 0.1602 KH. It was also significant (p < 0.05) the correlation between Eb and the respective Er values (calculated by the regression E = 0.1602 KH); furthermore, the linear regression of this new correlation (Eb = 1.0088Er + 0.0475) presented angular coefficient no different from 1, and constant coefficient no different from zero. It can be concluded that: (1) Four methods of E measuring showed similar results in a metallic material. (2) The same methods were successfully depurated for their execution in cortical bone specimens, since the measurement method did not affect the obtained E value in resin composites (that is a material with E value similar to cortical bone); (3) The E values of cortical bone depend on the measurement method, which demonstrates its bimodular behavior. The anatomical region and the individual also affect the E values of the cortical bone specimens (the individual was a significant factor only when considering just the E values obtained in the compression test). A correlation between E and KH that allows the E estimation by the regression E = 0.1602 KH was suggested and validated in composite resins.

Le tendon transmet les forces musculaires aux os et permet le mouvement. C'est un tissucomplexe et organisé, formé de cellules et d’une matrice extracellulaire (fibres collagènes,élastiques et substance fondamentale). Les fibres lui confèrent son élasticité et résistance et lasubstance fondamentale sa viscosité.La tendinopathie est souvent lié au sport, de morbidité élevée qui affecte laperformance des sportifs. Elle associe dégénérescence, douleur, rigidité et oedème local.L’imagerie quantifie et qualifie les changements morphologiques du tendon. L’homéostasietendineuse et sa physiopathologie restent peu connues, mais un changement des liaisons desfibrilles lors de la cicatrisation diminue sa résistance.L’objectif de l’étude est: mettre en place un modèle de tendinopathie chirurgicale chezla chèvre avec suivi clinique transposable (homme et cheval); développer un dispositifd’évaluation du comportement mécanique des tendons; et valider la chèvre comme modèleanimal pour l’étude de la tendinopathie. L’étude a été faite sur 84 jours avec un suivi cliniqueet échographique suivi d’un test de traction.La chèvre est un ongulé facile à héberger et manipuler. La technique chirurgicalepermet la résection de quelques fibres causant une lésion identifiable par échographie et dessymptômes cliniques. La grande variabilité du comportement mécanique ne se corrèle pas aupoids, morphologie des animaux ou section transversale du ses tendon, ce qui complique laréduction de l’effective. Notre modèle semble pouvoir être utilisé pour évaluer des traitementsde tendinopathies destinés à l’homme et/ou au cheval. Ce que n’exclue pas sondéveloppement pour renforcer sa pertinence / Tendons transmit muscles forces to bone and allow movement. It is a complexorganized tissue, composed by few cells and an extracellular matrix (collagen fibers, elasticfibers, and a ground substance. Fibers give to tendon its elastic characteristic and resistanceand ground substance its viscosity.Tendinopathy is a medical problem associated with sport, with a high morbidity whichaffects performance. It is an association of degeneration, pain, stiffness and local edema.Imaging can be used to quantify and qualify the changes in the morphology of the tendon.The tendon homeostasis and physiopathology remain poorly understood, but a change at theconnections of the fibrils, decreasing its strength.The purpose of this study is: development of surgical model of induced localtendinopathy in goats with clinical follow up transposable for humans and horses;development of a device to evaluate the mechanical properties of tendons, and demonstratethat the goat is a good experimental animal model for the study of tendinopathy. The studyhas been performed in 84 days with a clinical follow up, US imaging and tensile test.Goat is an ungulate easy to house and handle. The modified splitting allows easy andreproducible resection of some tendon fibers with an identifiable lesion in US imaging andclinical symptoms. The variability of mechanical behavior is not correlated with"macroscopic" aspects (weight, animal morphology or cross sectional area), thus reducing theeffective is difficult. However, our model appears in the state, can be used to evaluatetreatments for human and horse’s tendinopathy. The development of our model couldstrengthen its relevance.

Ce travail de thèse a pour objectif de caractériser le comportement anisotrope des mousses acoustiques. Ces matériaux, couramment employés pour lutter contre les nuisances sonores et vibratoireset sont modélisés à l'aide du modèle de Biot. Celui-ci est basé sur le formalisme de lamécanique des milieux continus à deux champs couplés, l'un associé au solide et l'autre au fluidesaturant. Nous nous intéresserons plus particulièrement dans ce travail aux paramètres du solideet aux matériaux présentant une anisotropie (c'est-à-dire des propriétés qui varient suivant lesdirections) du squelette solide. Ici, deux types d'anisotropie sont distingués, l'anisotropie naturelledu matériau et celle induite par une action extérieure, cette dernière ayant pour principale cause lacompression statique des échantillons. Par ailleurs, trois types de symétries naturelles sont considérés : isotropie, isotropie transverse avec et sans rotation de direction principale. Celles-ci sont leplus couramment rencontrées.L'analyse expérimentale du type de symétrie des mousses se fait au moyen d'un dispositif, appelé rigidimètre, qui permet de déterminer la raideur mécanique d'échantillons cubiques de moussesous hypothèse quasi-statique. Celui-ci est couplé à une mesure au vibromètre laser à balayage, permettantde mesurer le déplacement normal des faces des cubes. Des lignes de niveaux des champsde déplacements normaux surfaciques sont ainsi obtenues. Il est alors possible de classer les différentstypes d'anisotropie en analysant ces courbes de niveaux. Ainsi, avec ces a-priori, une méthodea été élaborée pour déterminer les coefficients de Poisson à l'aide de techniques de minimisationà partir des autres constantes élastiques préalablement déterminées. Ce problème est construit àpartir d'indicateurs expérimentaux et d'indicateurs provenant d'un modèle éléments finis.L'influence de la compression statique sur les modules élastiques est ensuite étudiée. Toutd'abord, la variation du module d'Young en fonction du taux de compression est caractérisée àpartir de mesures au rigidimètre. Ensuite, la variation du module de cisaillement en fonction de lacompression statique est caractérisée par une méthode d'ondes guidées (en collaboration avec laKULeuven). Il a été montré que les variations de modules élastiques pouvaient être importantespuisqu'elles peuvent atteindre 50 %. A partir de ces déterminations expérimentales, quatre zones decomportement de la mousse ont été mises en évidence. Ces quatre zones correspondent respectivementà des effets de compression, de flambement, de densification et de réarrangement des cellules.Un modèle éléments-finis microstructural, dans lequel la cellule élémentaire est modélisée par untétrakaidécaèdre de Kelvin, est enfin proposé. Celui-ci permet de modéliser les trois premièreszones, qui correspondent aux compressions statiques usuelles dans les applications acoustiques. / This thesis deals with the characterization of the anisotropic behavior of acoustic foams. Thesematerials, which are commonly used to reduce noise and vibration, are modeled by the Biot model.This model is based on the formalism of continuum mechanics of two coupled elds, one associated to the solid, and the other one associated to the saturating fluid. This work is more particularly focused on the solid parameters and on the materials having an anisotropy (i.e. properties which vary according to directions) of the solid skeleton. Here, two types of anisotropy are distinguished,the natural anisotropy of the material, and the induced anisotropy, which is due to an external action and principally caused by a static compression samples. Furthermore, three types of natural symmetries (which are the most commonly encountered) are considered : isotropy, transverseisotropy with and without rotation of principal direction.The experimental analysis of the type of the foam symmetry is performed with the device calledrigidimeter, which allows to determine the mechanical stiness of cubic samples of foam underquasi-static assumption. This device is coupled with a laser scanning vibrometer, which measures the normal displacement of the faces of cubes. Isovalues of the displacement fields of the normal surface are obtained. According to these results, it is possible to classify the different types of anisotropy by the analysis of the isovalues of the displacement fields. Thus, with these a-priori, a method was developed to determine the Poisson's ratios with minimization techniques from theother elastic constants already determined. This problem is constructed from experimental indicators and indicators taken from a finite element model.The influence of static compression on the elastic moduli is then studied. First, the variation of Young's modulus as a function of compression ratio is characterized from the rigidimeter measurement. Then, the variation of shear modulus as a function of static compression has been characterized by a method of guided waves (in collaboration with KULeuven). It was shown that variations of elastic moduli could be important because they can reach 50 %. From these experimental determinations, four areas of behavior of the foam have been identified. These four areas correspond, respectively, to effects of compression, buckling, densification and rearrangement of cells. A microstructural finite element model, in which the unit cell is modeled by a Kelvin tetrakaidecahedron,is finally proposed. This one models successfully the first three areas, which correspond to the common static compression in the acoustic applications.

The master thesis deals with the possibilities of using waste aggregate from main rock production to hydraulically bound mixtures, witch are used in base and sub base pavement. The theoretical part describes conditions and properties of bound mixtures, aggregates and cement. The practical part describes the process of design, mixture preparing and laboratory test carried out on them. The bound mixtures are testing in compressive strength, frost and water resistace and resilient modulus.

This diploma thesis deals with the application of basalt reinforcement in lightweight concretes. In the practical part, the comparison of steel and basalt reinforcement in concrete from agloporite and steel reinforcement in concrete from Liapor is performed experimentally.

Oxygen strengthened biomedical beta titanium alloys Beta titanium alloy Ti-35Nb-6Ta-7Zr-0.7O (wt. %) exhibits a low Young's modulus and high strength thanks to interstitial strengthening effect of oxygen. These mechanical properties are promising for implant production. In this thesis, the aforementioned alloy is thoroughly studied in conditions prepared by various thermomechanical treatments, namely: material after casting, hot compression testing, die-forging, hot rolling and finally, cold-swaged and annealed condition. Mechanical properties and microstructure of prepared conditions are studied with special interest of enhancing the fatigue performance that is poor after casting due to porosity and large grains. The hot rolling was shown to improve the fatigue performance significantly, mainly through grain refinement. It is shown that by combining the effects of cold-swaging and recrystallization annealing, extensive refinement of grain structure can be achieved. Industrial aspects of implant production by the studied methods were discussed. In the second part of the thesis, the possibility of lowering the Young's modulus by reducing the beta phase stability (by reducing of Nb and Ta content), while retaining high strength caused by high interstitial oxyen content is explored. Several alloys were...

Over the past 50 years, several advancements have been made in the research area of the mechanics of unsaturated soils. These advancements can be categorized into two groups; (i) development (or improvement) of testing techniques (or apparatus) to determine the mechanical properties of unsaturated soils and (ii) development of (numerical, empirical or semi-empirical) models to estimate the variation of mechanical properties of unsaturated soils with respect to suction based on the experimental results. Implementation of the mechanics of unsaturated soils in conventional geotechnical engineering practice, however, has been rather limited. The key reasons for the limited practical applications may be attributed to the lack of simple and reliable methods for (i) measuring soil suction in the field quickly and reliably and (ii) estimating the variation of mechanical properties of unsaturated soils with respect to suction. The main objective of this thesis research is to develop simple and reliable techniques, models or approaches that can be used in geotechnical engineering practice to estimate sol suction and the mechanical properties of unsaturated soils. This research can be categorized into three parts. In the First Part, simple techniques are proposed to estimate the suction values of as-compacted unsaturated fine-grained soils using a pocket penetrometer and a conventional tensiometer. The suction values less than 300 kPa can be estimated using a strong relationship between the compressive strength measured using a pocket penetrometer and matric suction value. The high suction values in the range of 1,200 kPa to 60,000 kPa can be estimated using the unique relationship between the initial tangent of conventional tensiometer response versus time behavior and suction value. In the Second Part, approaches or semi-empirical models are proposed to estimate the variation of mechanical properties of unsaturated soils with respect to suction, which include: - Bearing capacity of unsaturated fine-grained soils - Variation of bearing capacity of unsaturated fine-grained soils with respect to matric suction - Variation of initial tangent elastic modulus of unsaturated soils below shallow foundations with respect to matric suction - Variation of maximum shear modulus with respect to matric suction for unsaturated non-plastic sandy soils (i.e. plasticity index, Ip = 0 %) In the Third Part, approaches (or methodologies) are suggested to simulate the vertically applied stress versus surface settlement behavior of shallow foundations in unsaturated coarse-grained soils assuming elastic-perfectly plastic behavior. These methodologies are extended to simulate the stress versus settlement behavior of both model footings and in-situ plates in unsaturated coarse-grained soils. The results show that there is a reasonably good comparison between the measured values (i.e. soil suction, bearing capacity, elastic and shear modulus) and those estimated using the techniques or models proposed in this thesis research. The models (or methodologies) proposed in this thesis research are promising and encouraging for modeling studies and practicing engineers to estimate the variation of mechanical behavior of unsaturated soils with respect to matric suction.