Esta dissertação insere-se nas áreas de qualidade laboratorial e de ensaios de controle de concreto, especificamente quanto à propriedade módulo estático de deformação ou módulo de Young. A motivação do trabalho é a elevada variabilidade de resultados experimentais observada pelo meio técnico nacional em ensaios interlaboratoriais, cujos resultados indicam desvios-padrão totais da ordem de 3,5 GPa, valor significativo para o controle tecnológico de obras de construção civil. Os objetivos buscados foram a identificação das parcelas da variabilidade oriundas da produção e do ensaio, com especial atenção àquela originada na instrumentação para medida das deformações durante o ensaio, e a discussão da aplicabilidade do conceito semiprobabilístico normativo à propriedade módulo de deformação do concreto. Além disso, a própria discussão da aplicabilidade da sistemática de pesquisa e análise sobre este tipo de ensaio e de material constou como um objetivo do trabalho. Para tal, desenvolveu-se um programa experimental em duas etapas: a primeira foi destinada às avaliações de acurácia (precisão e exatidão) do método de ensaio. As avaliações se deram segundo roteiros da área metrológica para validação de métodos e sistemas de medida. De quatro instrumentações para medida das deformações testadas, uma se mostrou mais precisa (identificada como clip gages) e outra se mostrou a mais suscetível a erros sistemáticos e aleatórios entre as testadas (identificada como compressômetro com dois relógios comparadores). Recomendou-se a ampliação do programa experimental para o âmbito interlaboratorial, pois, a rigor, o método de ensaio vigente não poderia ser considerado validado em termos de acurácia baseando-se unicamente nos resultados deste programa experimental. Porém, concluiu-se pela possibilidade de aceitação prática do método independentemente da utilização de três de um total de quatro tipos de instrumentação para medida das deformações testados em ensaio, sem que houvesse prejuízo para a produção ou o controle tecnológico usual desta propriedade. Na segunda etapa, obteve-se um Diagrama de Dosagem e estudou-se um cenário de fornecimento de concreto sob critérios estatísticos diferentes de atendimento à especificação de módulo de deformação: utilização do valor característico e do valor médio, com diferença de 4 GPa entre eles. Estimou-se um aumento da ordem de 9% no deslocamento vertical de uma viga simples bi-apoiada quando executada com o concreto de menor módulo em relação à execução com o de maior módulo. Por sua vez, o concreto de maior módulo exigiria um aumento no consumo de cimento da ordem de até 200 kg/m3, se conservados todos os insumos materiais e os demais parâmetros tecnológicos contidos nos traços. Concluiu-se pela aplicabilidade do uso da sistemática empregada na avaliação da acurácia do método de ensaio e do uso do conceito semiprobabilístico para esta propriedade. / This work is developed into the areas of laboratorial quality and concrete control tests, specifically focusing on the static modulus of elasticity or Young´s modulus. The motivation of this work is the high variability of experimental results observed by national technicians in interlaboratorial tests. These results show total standard deviations of around 3.5 GPa, a significant value for the technological control for civil construction. The main objectives are the identification of the variability fragments derived from the production and test, specially the ones related to the instrumentation for measuring deformations during the test, and the discussion of the semi-probabilistic concept applicability on the concrete Young´s modulus control. Moreover, the discussion of the applicability of the procedure used in this work and its analysis are also objective pursued here. The experimental program was developed in two steps: the first step covered the accuracy assessments (precision and exactness) of test method. The assessments were carried out according to instructions from Metrology concepts for the validation of the methods and the measure systems. One out of four instrumentations for measuring the tested deformations proved to be more precise (identified as clip gages) and another one proved to be more susceptible to systematic and random errors (identified as a compressometer with two dial indicators). The extension of the experimental program to an interlaboratorial scope is recommended because the current test method could not be considered valid based only on the results of this experimental program. However, it was shown that the practical acceptance of the test method for three among the four kinds of instrumentations analyzed, without damaging the production or the usual technological control of this property, is possible. On the second step, a mix design diagram was obtained and a case of supply of concrete under different statistical criteria (fulfillment the modulus of elasticity specification): the use of the characteristic value and the average value, with difference of 4 GPa between them. An increase of 9% on the vertical transference of a simple dual supported beam was observed when using a lower modulus concrete, when compared to another one with a higher modulus. On the other hand, the modulus increase would require an increment in the cement consumption up to 200 kg per cubic meter, if all the material inputs and further technological parameters is maintained. The final conclusion was that the procedure used on the assessment of the test method accuracy and the semi-probabilistic concept on this material property is applicable.

A contração de polimerização das resinas compostas é uma característica indesejável que compromete a integridade da interface dente/restauração. O objetivo deste estudo foi avaliar in vitro a influência de diferentes materiais usados em restaurações classe II de resina composta, quanto ao grau de conversão, tensão de contração, resistência a flexão, módulo de elasticidade e formação de fenda marginal. Foram realizados preparos classe II com dimensões de 4x4x2mm em terceiros molares recém-extraídos para a avaliação da formação de fenda marginal. As cavidades foram niveladas com cimento de ionômero de vidro Riva Light Cure (SDI) (CIV), resina de baixa contração SureFilSDR (Dentsply) (SDR), resina flow FiltekZ350Flow (3M/ESPE) (Z350F) e resina composta FiltekP90 (3M/ESPE) (P90). As restaurações (n=3) foram avaliadas com lupa estereoscópica. A resistência a flexão foi avaliada por meio de ensaio de flexão em três pontos. Para este ensaio foram confeccionados dez corpos de prova (n=10) de cada material com dimensões de 10x2x1mm. Para o teste de tensão de contração foram utilizados cilindros de polimetacrilato com 5 mm de diâmetro e 13 ou 28mm de comprimento. Os bastões foram fixados na EMIC com um espaço de 2mm entre eles, onde os materiais foram inseridos. Foram realizadas cinco repetições para cada grupo (n=5) e a tensão proveniente da contração foi medida por até 10 minutos após o início da fotopolimerização. O Grau de Conversão (GC) foi determinado por espectroscopia no infravermelho com transformada de Fourier (FTIR). Os resultados foram tratados estatisticamente por análise de variância (ANOVA) e Teste de Tukey (p<0,05). Fenda marginal: Z350F = CIV > SDR = P90. Tensão de contração: Z350F > SDR > CIV = P90. Resistência a flexão: P90 > SDR = Z350F > CIV. Módulo de Elasticidade: P90 > CIV = SDR = Z350F. GC: Z350F = SDR > P90 > CIV. Conclusões: existe correlação entre a formação de fenda marginal e as propriedades físico químicas dos materiais testados, sendo as resinas de baixa contração que proporcionaram melhor adaptação marginal; existe correlação entre resistência a flexão, módulo de elasticidade, tensão de contração e a composição dos materiais, já que os compósitos com melhores resultados foram os que apresentaram os maiores percentuais de carga, no entanto, maior grau de conversão não representou melhores propriedades mecânicas. / The shrinkage of composite resin polymerization is an undesirable characteristic that compromises the integrity of the tooth / restoration interface. The aim of this study was to evaluate in vitro the influence of different materials used in composite resin class II restorations in terms of contraction stress, flexural strength, degree of conversion and marginal gap formation. Class II preparation were performed with 4x4x2mm dimensions in third molars freshly extracted for the evaliation of marginal gap formation. The cavities were filled with Riva Light Cure (SDI) glass ionomer cement (CIV), SureFil SDR (Dentsply) low shrinkage resin (SDR), Filtek Z350Flow (3M/ESPE) flowable composite (Z350F) and Filtek P90 (3M/ESPE) composite resin (P90). The restorations (n = 3) were evaluated with magnifying stereoscopic. The flexural strength was assessed by means of three point bending test. For this test ten specimens (n = 10) of each material were made, each with 10x2x1mm dimensions. For the shrinkage stress test polymethacrylate cylinders with 5 mm in diameter and 13 or 28mm in length were used. Bats were attached to the EMIC with a 2mm space between them, where the materials were inserted. The test were repeated five times for each group (n = 5) and the contraction stress was measured for up to 10 minutes after initiation of photopolymerization. The Degree of Conversion (DC) was determined by Fourier transform infrared (FTIR). The results were statistically analyzed by the variance analysis (ANOVA) and Tukey test (p <0.05). Marginal gap: Z350F = CIV > SDR = P90. Contraction stress: Z350F > SDR> CIV = P90. Flexural strength: P90 > SDR = Z350F > CIV. Elasticity Modulus: P90 > CIV = SDR = Z350F. DC: Z350F = SDR > P90 > CIV. Conclusion: There is a correlation between formation of marginal gap and physicochemical properties of the materials tested whereas low shrinkage resins provided better marginal adaptation; correlation exists between flexural strength, elastic modulus, shrinkage stress and material composition, since better results were obtained from composites with larger quantity of load; higher conversion degree did not represent better mechanical properties.

Este trabalho apresenta dois tipos de ensaios não destrutivos para a correlação do módulo dinâmico com a resistência à compressão para elementos de concreto. Os métodos de ensaio são a ultrassonografia e o método de excitação por impulso utilizando o equipamento Sonelastic®. Neste trabalho estão descritos seus funcionamentos, aplicações e limitações. A ultrassonografia, através da propagação de ondas sonoras, fornece, indiretamente, o módulo de elasticidade dinâmico. Com o método de excitação por impulso obtêm-se as frequências naturais e os modos de vibração do elemento estudado, o que permite determinar seu módulo dinâmico. Primeiramente, estes ensaios foram utilizados em corpos-de-prova cilíndricos e lajes alveolares produzidas em laboratório para a obtenção das curvas de correlação e, em seguida, estes mesmos ensaios foram realizados na fábrica de concreto pré-moldado. Para elementos de geometria complexa, como é o caso das lajes alveolares, apresenta-se uma metodologia para a obtenção de uma equação analítica para o cálculo do módulo dinâmico no ensaio de excitação por impulso. Estes métodos tiveram o objetivo final de avaliar a resistência à compressão do concreto na pista de protensão da fábrica, e então determinar o melhor momento para a desforma e corte do cabo de protensão. Com ambos os métodos, obteve-se ótimas correlações do módulo dinâmico com a resistência à compressão dos elementos em laboratório. Na fábrica de concreto pré-moldado não foi possível obter uma curva de correlação representativa de toda a laje na pista de protensão, porém foi possível registrar um bom indicativo de que é possível obter boas correlações para futuras pesquisas no assunto / This work presents two types of non-destructive testing for the correlation of the dynamic elastic modulus with the compressive strength. The test methods are the ultrasonography and the impulse excitation using the Sonelastic® equipment. In this work the equipaments operations, applications and limitations are also described. The ultrasound test indirectly supplies the dynamic elastic modulus through the propagation of sound waves. The natural frequencies and the vibration modes of the studied elements are obtained through impulse excitation method allowing to determine its dynamic modulus. To start, these tests were used in cylindrical specimens and hollow core slabs produced in the laboratory to obtain the correlation curves, and then these same methods were performed in the pre-cast concrete plant. As for complex geometric elements, as in the case of hollow core slabs, a methodology is applied in order to obtain an analytic equation to calculate the dynamic modulus in the impulse excitation test. These methods had the final goal the evaluation of the strength of prestressed concrete lying on track of the plant, so as to determine the best moment to demold and cut the prestressed cable. Excellent correlations of the dynamic modulus with compressive strength of the elements made in laboratory were obtained using both methods. It was not possible to obtain in the precast concrete plant a representative correlation curve of the whole slab on the track, nevertheless, it was possible to record a good indication that it is possible to obtain good correlations for future research.

Esse trabalho tem como objetivo estabelecer um método simples de ensaio que permita determinar a resistência à tração e módulo elástico de partículas individuais de agregados graúdos naturais submetidas à carga de compressão. O método de ensaio foi desenvolvido baseado no ensaio de carga pontual (Point Load Test) que permite obter a resistência à tração de partículas. Para a determinação do módulo de elasticidade foi acoplado ao método um LVDT e foi satisfeita a condição para aplicação da teoria de contato de Hertz (contato curvo-plano entre as partículas e as fixações de aplicação da carga). Inicialmente a metodologia foi avaliada utilizando como material de referência partículas de vidro (com geometrias similares aos agregados). Após a validação no vidro, o método de ensaio foi aplicado em agregados graúdos de granito. Propôs-se um método de seleção de partículas com base na sua distribuição de frequência de absorção, com o intuito de reduzir a quantidade de partículas testadas mecanicamente necessárias para obter a distribuição de Weibull da resistência à tração (e módulo de elasticidade). Para tanto, foi feita a determinação da absorção de água individual de centenas de partículas selecionadas por amostragem a esmo da população de agregados. Com base nos resultados, foi possível determinar a distribuição de Weibull da resistência à tração e módulo de elasticidade das partículas. Observou-se que as resistências à tração variaram de 3 a 15 MPa. Os agregados possuíam aproximadamente 10% da população de partículas com resistência à tração inferior a 5 MPa, o que pode influenciar as classes de resistência à compressão de concretos >50MPa. Os módulos elásticos dos agregados também foram variáveis (18-67 GPa) e aproximadamente 10% da população de partículas com módulo elástico <30 GPa. Isso pode limitar o módulo de elasticidade do concreto (que geralmente é em torno de 27 GPa), dependendo do processo de escolha dos agregados. As funções exponenciais inversas fundamentais entre essas propriedades mecânicas e a porosidade foram confirmadas (para valores médios). / The aim of this work is to establish a simple test method to determine the tensile strength and elastic modulus of individual natural aggregate particles subjected to a compression load. The test method was developed based on the Point Load Test, that allows to obtain the tensile strength of particles. For the determination of the elastic modulus, an LVDT was coupled to the method and the condition for application of Hertz contact theory (curved-plane contact between the particles and the load application fixations) was satisfied. Initially, the method was evaluated using glass particles as reference (with geometries similar to aggregates). After validation on the glass, the test method was applied to coarse granite aggregates. A method of particle selection was proposed based on its absorption frequency distribution, in order to reduce the amount of mechanically tested particles required to obtain the Weibull distribution of tensile strength (and elastic modulus). For this purpose, the determination of the individual water absorption of hundreds of particles selected by random sampling of the population of aggregates was made. Based on the results, it was possible to determine the Weibull distribution of the tensile strength and elastic modulus of the particles. The tensile strengths ranged from 3 to 15 MPa. The aggregates had approximately 10% of the particles population with tensile strength less than 5 MPa, which may influence the classes of concrete with compressive strength > 50MPa. The elastic modulus of the aggregates was also variable (18-67 GPa), with approximately 10% of the particle population with elastic modulus <30 GPa. This may limit the elastic modulus of the concrete (usually around 27 GPa) depending on how the aggregates are selected. The fundamental inverse exponential functions between these mechanical properties and the porosity were confirmed (for mean values).

The mechanical properties of boron carbide (B4C) with 10 and 20 vol% particulate inclusions of commercially available nano-sized alpha-phase silicon carbide (a-SiC) or micron-sized titanium diboride (TiB2) were investigated so as to produce a fine-grained material with high hardness, toughness, and overall strength in order to increase the effectiveness of B4C as a structural ceramic, whose use in the field has been limited because of the extreme brittle nature of the material. Full density sintering of the ceramics (≥99% theoretical) was completed using the novel Plasma Pressure Compaction (P²C®) technique, which limited grain growth due to a reduced processing temperature and a significantly reduced consolidation time. The reinforced ceramic composites had particulate grains homogeneously distributed within the B4C matrix. X-ray diffraction patterns confirmed that the constituents did not interdiffuse. The four-point flexure strength for the monolithic B4C ceramic was found to be significantly larger than any recorded value found in scientific literature, and was most likely attributed to the fine-grained microstructure resulting from the P²C® processing. The mechanical properties of the nano-sized a-SiC-B4C ceramics showed a slight increase in the Chevron-notched four-point bend fracture toughness due to the crack deflection toughening mechanism. A slight decrease in the Vickers microhardness and the static elastic modulus values were also observed. A significant increase in the fracture toughness as well as a slight increase in the microhardness and elastic modulus of the micron-sized TiB2-B4C materials was found. The toughening mechanism of this composite was attributed to the slight chemical bond between the B4C matrix and the ultra-small, ultra-tough TiB2 particulates, which forced a propagating crack to completely rip apart the TiB2 reinforcing particles. This cleaving nature resulted in significant amounts of energy being absorbed by the micron-sized particulates. It was concluded that the composite with 20 vol% TiB2 allowed for the largest gain in toughness because it possessed the largest number of ultra small, ultra tough particulate-cracktip interactions.

Η κατανόηση των φαινομένων που λαμβάνουν χώρα κατά την αλληλεπίδραση κυττάρου βιοϋλικού και η συσχέτιση μηχανικών παραμέτρων του κυττάρου με πολύπλοκες διεργασίες στο εξωκυττάριο (ECM) περιβάλλον οδηγεί το μέλλον στο σχεδιασμό των βιοϋλικών. Σκοπός της διατριβής ήταν η διερεύνηση της προσκόλλησης και των μεταβολών των μηχανικών ιδιοτήτων οστεοβλαστών στους αρχικούς χρόνους προσκόλλησης σε υπόστρωμα του βιοπολυμερούς χιτοζάνης. Η προετοιμασία υποστρωμάτων χιτοζάνης έγινε με ομοιοπολική πρόσδεση του βιοπολυμερούς σε επιφάνεια γυαλιού (επιφάνεια ελέγχου). Με φασματοσκοπία φωτοηλεκτρονίων από ακτίνες Χ επιβεβαιώθηκε η μεταβολή της επιφανειακής χημικής σύστασης. Η μέση επιφανειακή τραχύτητα, με χρήση Μικροσκοπίας Ατομικής Δύναμης, βρέθηκε 4 φορές μεγαλύτερη στη χιτοζάνη σε σύγκριση με το γυαλί, ενώ η μέση γωνία διαβροχής ήταν περίπου 3 φορές μεγαλύτερη στη χιτοζάνη. Ο αριθμός και η μέση επιφάνεια εξάπλωσης των προσκολλημένων κυττάρων, προσδιορίστηκαν από φωτογραφίες ηλεκτρονιακού μικροσκοπίου σάρωσης και χρήση λογισμικού ανάλυσης εικόνας. Μέχρι τα 30 λεπτά, ο αριθμός ήταν μεγαλύτερος στη χιτοζάνη, ενώ μετά τα 45 λεπτά, στο γυαλί. Σε όλους τους χρόνους, η μέση επιφάνεια εξάπλωσης ήταν μεγαλύτερη στη χιτοζάνη. Για την ποσοτικοποίηση της προσκόλλησης, χρησιμοποιήθηκε η τεχνική της μικροπιπέττας σε πειράματα αποκόλλησης μεμονωμένων οστεοβλαστών. Υπολογίστηκε η “ώθηση αποκόλλησης”, I, ως το ολοκλήρωμα της εφαρμοζόμενης δύναμης στο χρόνο (I=SFdt) για την πλήρη αποκόλληση ενός κυττάρου και βρέθηκε στατιστικά μεγαλύτερη στη χιτοζάνη σε όλους τους χρόνους. Με την τεχνική Ποσοτικής Αλυσιδωτής Αντίδρασης Πολυμεράσης, η έκφραση των γονιδίων ιντεγκρινών αν, α4, β1 και β3 βρέθηκε σημαντικά αυξημένη στη χιτοζάνη από τα 30 στα 120 λεπτά. Με συνεστιακό μικροσκόπιο σάρωσης, παρατηρήθηκε αυξημένη έκφραση της κινάσης εστιακής προσκόλλησης στη χιτοζάνη στα 30 και στα 120 λεπτά. Τέλος, χρησιμοποιήθηκε η τεχνική της μικροπιπέττας σε πειράματα εφελκυσμού και ερπυσμού των οστεοβλαστών και υπολογίστηκαν οι μεταβολές του μέτρου Young, Ε, και του φαινόμενου ιξώδους, η. Οι μέσες τιμές βρέθηκαν αυξημένες στην πορεία της προσκόλλησης στις δύο επιφάνειες, παρουσιάζοντας υψηλότερες τιμές στη χιτοζάνη. Η παρούσα διατριβή είναι μια ολοκληρωμένη φαινομενολογική προσέγγιση της μηχανικής συμπεριφοράς της οστεοβλάστης κατά την προσκόλληση. Η προσκόλληση στη χιτοζάνη συνοδεύεται από μεταβολές στη μηχανική συμπεριφορά και συνδέεται με κρίσιμες βιοχημικές διεργασίες. / The understanding of the phenomena that take place during cell-biomaterial interaction and the correlation of cell mechanical parameters with complicated processes at the extracellular environment (ECM) is driving the future of biomaterial design. The aim of the present study was the investigation of attachment and of alterations of mechanical properties of osteoblasts during the initial phase of attachment on chitosan biopolymer substrate. The preparation of the chitosan substrates was done with covalent immobilization of the biopolymer on glass surface (control substrate). X-Ray photolelectron spectroscopy confirmed the alteration of the surface chemical composition. Mean surface roughness, as measured by Atomic Force Microscopy, was increased 4-fold compared to glass, while the mean contact angle was found 3 times higher on chitosan substrate. The mean number and spreading area of the attached cells, were determined by Scanning Electron Microscopy images and the use of image processing program. Up to 30 minutes, the number of attached cells was higher on chitosan, while after 45 minutes, it was on glass. At all time points, the mean spreading area was greater on chitosan. To quantify attachment, the micropipette aspiration technique was used at experiments of detachment of individual osteoblasts. The ‘’detachment impulse’’, I, was calculated, as the integral of the applied force at time required (I=SFdt) for complete detachment of one cell, and it was found statistically higher on chitosan at all attachment times. With the quantified Polymerase Chain Reaction, the αν, α4, β1 and β3 gene integrin expression was found significantly increased from 30 to 120 minutes of attachment on chitosan. Using confocal scanning microscopy, higher expression of focal adhesion kinase was observed on chitosan at 30 and 120 minutes of attachment. Additionally, the micropipette aspiration technique was used at stretching and creep experiments so as to calculate the alterations of cell’s Young modulus, E, and apparent viscosity, η. Mean values were increased at the course of spreading for both surfaces, demonstrating greater values on chitosan. The present study is a complete phenomenological approach of the mechanical behavior of osteoblasts during attachment. Attachment on chitosan is accompanied by alterations of the mechanical behavior and is associated with critical biochemical processes.

In order to evaluate a methane gas productivity of methane hydrate reservoirs, it is necessary to develop a numeric simulator predicting gas production behavior. For precise assessment of long-term gas productivity, it is important to develop a mathematical model which describes mechanical behaviors of methane hydrate reservoirs in consideration of their time-dependent properties and to introduce it into the numeric simulator. In this study, based on previous experimental results of triaxial compression tests of Toyoura sand containing synthetic methane hydrate, stress-strain relationships were formulated by variable-compliance-type constitutive model. The suggested model takes into account the time-dependent property obtained from laboratory investigation that time dependency of methane hydrate bearing sediment is influenced by methane hydrate saturation and effective confining pressure. Validity of the suggested model should be verified by other laboratory experiments on time-dependent behaviors of methane hydrate bearing sediment.

Šiame baigiamajame magistro darbe nagrinėjama polistireninio putplasčio stiprumo savybės. Teorinėje dalyje pateikta literatūros analizė, bendros žinios apie polistireninį putplastį, gamybos būdai, panaudojimo galimybės. Išnagrinėta trijų didžiausių gamintojų Lietuvoje siūloma produkcija. Apžvelgti reikalavimai pastatų atitvarų šiluminei varžai, išnagrinėta termoizoliacinio sluoksnio storio pokytis nuo TSRS laikų iki dabar. Eksperimentinėje dalyje aprašomos naudotos medžiagos; jų charakteristikos; gniuždomasis stipris; šliejamasis stipris; išnagrinėta skirtingo tankio bandinių mikrostruktūra ir makrostruktūra. Aprašomi rezultatai, naudojant statistinės analizės programą atliekama jų analizė, suformuluojamos išvados. / The present work of Master degree studies analyzes the properties of expanded polystyrene.Theoretical par of this work introduces analysis of references, general information on expanded polystyrene, manner of production and fields of application. The work analyzes production offered by three biggest manufacturers in Lithuania, reviews the requirements applicable to thermal resistance of enclosures of the building, analyses alteration of thickness of a heat insulation layer comparing the situation in Soviet Union time and nowadays. Experimental part describes the used material, their properties, compressive strength, shear strength; analyses microstructure and macrostructure of samples of different density. The work presents the results and analysis of the results by applying software of statistical analysis; formulation of conclusions.

Carbon forms the basis of a variety of compounds. The allotropic forms of carbon include graphene, fullerenes, graphite, carbon nanotubes and diamond. All these structures possess unique physical and chemical properties. This work focusses on the usage of carbon nanotubes (CNT), especially iron-filled CNT. An industrial application of CNT requires the understanding of the growth mechanism and the control of the synthesis process parameters. Regarding iron-filled CNT the shell formation as well as the filling process has to be understood in order to control the CNT morphology and distribution and dimension of the iron filling. The thesis involves two topics - synthesis of CNT and characterization of their mechanical properties. Chapter 2 of the present work deals with the synthesis of iron-filled CNT. In this thesis all experiments and the discussion about the growth process were conducted with respect to the demands of magnetic force microscopy probes. The experimental work was focused on the temperature profile of the furnace, the aluminum layer of the substrate, the precursor mass flow and their impact on the morphology of in-situ iron-filled CNT. By selecting appropriate process parameters for the temperature, sample position, gas flow and by controlling the precursor mass flow, CNT with a continuous filling of several microns in length were created. Existing growth models have been analyzed and controversially discussed in order to explain the formation of typical morphologies of in-situ filled CNT. In this work a modified growth model for the formation of in-situ filled CNT has been suggested. The combined-growth-mode model is capable to explain the experimental results. Experiments which were conducted with respect to the assumptions of this model, especially the role of the precursor mass flow, resulted in the formation of long and continuous iron nanowires encapsulated inside multi-walled CNT. The modified growth model and the synthesis results showed, that besides the complexity of the parameter interaction, a control of the morphology of in-situ iron-filled CNT is possible. In chapter 3 the measurements of mechanical properties of in-situ iron-filled CNT are presented. Two different experimental methods and setups were established, whereby one enabled a static bending measurement inside a TEM and another a dynamical excitation of flexural vibration of CNT inside SEM. For the first time mechanical properties and in particular the effective elastic modulus Eb of in-situ iron-filled CNT were determined based on the Euler-Bernoulli beam model (EBM). This continuum mechanic model can be applied to describe the mechanical properties of CNT and especially MWCNT in consideration of the restriction that CNT represent a macro molecular structure built of nested rolled-up graphene layers. For evaluation and determination of the elastic modulus the envelope of the resonant vibrating state was evaluated by fitting the EBM to the experimental data. The experiments also showed, that at the nanoscale the properties of sample attachment have to be taken into account. Thus, instead of a rigid boundary condition a torsion spring like behavior possessing a finite stiffness was used to model an one side clamped CNT. The extended data evaluation considering the elastic boundary conditions resulted in an average elastic modulus of Eb = 0.41 ± 0.11 TPa. The low standard deviation gives evidence for the homogeneity of the grown material. To some extend a correlation between the formation process, the morphology and the mechanical properties has been discussed. The obtained results prove the usability of this material as free standing tips for raster scanning microscopy and especially magnetic force microscopy. The developed methods provide the basis for further investigations of the CNT and the understanding of mechanical behavior in greater detail.

Incorporation of monoacetylferrocene to the sulfonated polystyrene ionomers imparted some changes in the properties of sulfonated polystyrene. Sulfonation was carried out by acetic anhydride and concentrated sulphuric acid. The sulfonation reaction and the degree of sulfonation were determined by analytical titration and adiabatic bomb calorimeter . For this purpose, sulfonated polystyrene (SPS) samples with varying percentages of sulfonation were prepared between 0.85% and 6.51%. Monoacetyl ferrocene was used in equivalent amount of sulfonation through addition procedure. FTIR Spectroscopy was one of the major techniques used to support the successful addition of AcFe to the SPS samples. Altering the sulfonation degree did not change the characteristic peak positions, but increased the peak intensities with increasing the degrees of sulfonation. Mechanical properties of resultant polymers were investigated. As a result, elastic modulus of polymers decreased by the amount of monoacetylferrocene. Thermal characteristic were found by Differential Scanning Calorimeter (DSC). Thermal analysis revealed that sulfonated polystyrene samples after addition of monoacetylferrocene displayed lower values of Tg. Microscopic analysis were made by Scanning Electron Microscopy (SEM) and single phase for each sample was observed. Besides, energy dispersed micro analysis showed an increase in the intensity of the iron (II) peaks that is related to the amount of monoacetylferrocene added to the SPS samples. Flame retardancy for each polymer was also examined and found that addition of monoacetylferrocene to sulfonated polystyrene does not change the Limiting Oxygen Index value (LOI)(17). However, LOI value for polystyrene is 18.