Made available in DSpace on 2014-10-09T12:38:21Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:07Z (GMT). No. of bitstreams: 1 05678.pdf: 6012797 bytes, checksum: fe9d7fe0fee771d558f91a7bffb7cfa3 (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Made available in DSpace on 2014-10-09T12:41:14Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:08:34Z (GMT). No. of bitstreams: 0 / O objetivo deste trabalho foi desenvolver um software, de fácil operação e eficiente, para determinar a difusividade térmica de biomateriais. A necessidade de se conhecer a difusividade térmica de materiais como, por exemplo, esmalte e dentina, é essencial para o estabelecimento de protocolos de utilização clínica laser, para evitar danos colaterais ao paciente. O software desenvolvido, denominado CZ ThermaDiff, baseia-se no processamento de imagens térmicas adquiridas por uma câmera termográfica no infravermelho (ThermaCam SC3000, FLIR System, EUA). Foi desenvolvido em ambiente LabView, o que permitiu criar um painel de controle de fácil operação, contendo apenas duas funções básicas (Start e Stop). O software arquiva os dados em formato de tabela contendo todas as medidas de difusividade térmica, suas médias para intervalos de 10 °C e suas respectivas temperaturas, para uma amostra. Foi observado, tanto para o esmalte quanto para a dentina, que os valores de difusividade não são constantes e aumentavam em função da temperatura. Os valores encontrados foram aplicados a um modelo de transferência de calor, simulando um dente molar humano com as seguintes estruturas: esmalte, dentina e polpa. O modelo baseia-se no método de resistores térmicos, sendo que para a polpa foi utilizado o modelo de difusão de calor, considerando a circulação sanguínea. Os valores de temperatura obtidos neste modelo teórico, utilizando difusividades dependentes da temperatura foram maiores que as obtidas com um valor constante de difusividade, medido à temperatura ambiente. Este fato realça a importância da mensuração da difusividade em função da temperatura e da interface desenvolvida neste trabalho. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

L'usage des matériaux composites dans les différents domaines technologiques (microélectronique, aéronautique, transports…) ne cesse de croître. Une telle augmentation vient du fait qu'il est possible de développer de nouveaux matériaux avec des propriétés adaptées à une application bien préc ise en combinant les propriétés physiques des différents constituants. Dans le travail de thèse, nous nous intéressons à l'étude des propriétés thermophysiques, électriques et diélectriques de composites à base de matrice polymère chargée avec des fibres naturelles et/ou de particules minérales. L'objectif final étant d'une part d'accroître notre connaissance sur le mécanisme de transfert (thermique, électrique et diélectrique) au sein des matériaux composites et d'autre part, de développer une méthode de mesure des propriétés thermophysiques des matériaux à différentes températures (-20°C etlt; T etlt; 180°C) / The use of composite materials in various fields of technology (microelectronics, aerospace, transportation ...) continues to grow. Such an increase is that it is possible to develop new materials with properties tailored to a specific application by combining the physical properties of different constituents.In the thesis, we focus on the study of thermophysical properties, electrical and dielectric of composites based on polymer matrix loaded with natural fibers and/or mineral particles.The final goal is to increase our knowledge on the mechanism of transfer (thermal, electrical and dielectric) in composite materials and secondly, to develop a method for measuring thermophysical properties of materials at different temperatures (-20°C etlt; Tetlt; 180°C)

Les matériaux composites à matrice céramique (CMCs) à matrice auto-cicatrisantes (MAC) sont développées depuis plusieurs années pour leurs possibilités d'application dans le domaine de la propulsion aéronautique où ils se révèlent trés intéressants en termes de résistance à des conditions sévères et de légèreté. Dans le cadre d'un programme d'étude du comportement des CMC-MAC et de leurs mécanismes d'endommagement, l'objectif de ces travaux est de construire un modèle numérique multi-physique permettant de déterminer la durée de vie d'un échantillon d'un tel matériau soumis à une contrainte mécanique dans un environnement oxydant. L'étude porte sur la mise en place d'un couplage entre deux codes de calcul : un code d'endommagement mécanique et un code physico-chimique qui a été développé au cours de cette thèse. De façon inédite, on se place dans la géométrie 2D d'un plan de fissure, partant d'une image détaillée de l'arrangement des constituants (fibres, interphases, matrice multi-couche). Les différentes parties du programme ont été validées indépendamment et des résultats du calcul complet sont présentés et discutés. / Self-Healing Ceramics Matrix Composites (HT-CMC) are developed since several years for theirapplication in aeronautic applications and are interesting for their good resistance to criticalenvironments. As part of a study program of the HT-CMC behavior and their damagemechanisms, the objective of this thesis is to build a multi-physics numerical model todetermine the lifetime of a sample such a material subjected to a mechanical stress in anoxidizing environment. The study focuses on the establishment of a coupling between twocomputer codes: a code of mechanical damage and a physical-chemical code that wasdeveloped during this thesis. In an unprecedented way, we place ourselves in the 2D geometryof a crack plane, starting from a detailed picture of the arrangement of the components (fiber,interphase, multi-layer matrix). The different parts of the code have been independentlyvalidated and the results of the complete calculation are presented and discussed.

Les recherches portant sur le développement des composites réfractaires de type SiCf/SiC pour application gainage du combustible des réacteurs de géneration IV ont conduit le CEA à s’intéresser aucomportement thermique de ces matériaux. En particulier, la connaissance des propriétés thermiques représente un des points cles dans la conception des composants. Au regard du concept sandwichdont la complexité de structure et la géométrie cylindrique s'éloigne de celle d'éprouvettes planes classiquement utilisées, les méthodes de mesures usuelles ne conviennent pas.Ce travail de thèse s’intéresse à la caractérisation et à la modélisation du comportement thermiquede ces structures. Une première partie du travail concerne l'identification des paramètres thermiquesglobaux des différentes couches constitutives d'une gaine sandwich . Pour cela, une méthodeash est employée et un banc d’expériences adapte aux géométries tubulaires a pu être développe.L’écriture d'un nouveau modèle d'estimation, fonde sur le couplage des signaux recueillis à la fois enface avant et en face arrière, permet aujourd'hui d’accéder par la mesure a la diffusivité thermiquedes composites tubulaires via la thermographie infrarouge. Dans une seconde partie de la thèse,une démarche matériau virtuel a été mise en place pour décrire le comportement thermique d'unegaine sandwich à partir des propriétés des constituants élémentaires (bres et matrice). Cespropriétés, obtenues avec deux méthodes d'estimation différentes permettant d'exploiter les mesuresde deux expériences distinctes basées sur la thermographie infrarouge, sont utilisées comme donnéespour la modélisation du transfert thermique au sein de ces gaines. Les confrontations réalisées entrecampagnes de mesures et expériences numériques permettent normalement d’appréhender le poids desdifférents facteurs d'influence qui régissent les transferts thermiques. / Researches on the development on SiCf/SiC refractory composites for generation IV nuclear fuel cladding led the CEA to focus on the thermal behavior of these materials. In particular, knowingthe thermal properties is essential for their components design. Regarding the development of the sandwich" concept, whose complexity and geometry differ from the conventionally used at tubes,usual measurement methods are unsuitable.This PhD reports on the characterization and modeling of the thermal behavior of these structures. The first part concerns the identification of the global thermal parameters of the diferent layers of a"sandwich" sheath. To do so, a ash method is used and an experimental bench suitable for tubular geometries was developed. A new estimation method based on the combination of both collectedsignals in front and rear faces allows the identification of the thermal diffusivity of tubular composites using infrared thermography. The second part focuses on a virtual material approach, established todescribe the thermal behavior of a "sandwich" cladding, starting from the properties of the elementary components (bers and matrix). These properties, obtained using two different estimation methods,allows exploiting the measurements of two separate experiments based on infrared thermography.They are then used as data for the heat transfer modeling in these ducts. Confrontations betweenexperimental measurements and numerical results finally allow gaining insight into the in uence ofthe different key parameters governing the heat transfer.

A Physalis peruviana Linnaeus é uma fruta considerada exótica que possui elevado custo de comercialização, principalmente nos mercados internacionais. Suas propriedades nutracêuticas e o aumento da sua produtividade no Estado do Rio Grande do Sul, associados à sua elevada perecibilidade definiram o objetivo deste trabalho: estudar o processo de transferência de massa durante a desidratação osmótica de physalis. Diversos trabalhos que avaliam as propriedades dos compostos bioativos da physalis através de ensaios in vitro e in vivo estão disponíveis na literatura, no entanto, há uma carência de informações a respeito de processos de industrialização desta fruta. Neste trabalho foi realizada a desidratação osmótica da physalis avaliando os efeitos da temperatura (variando de 40 a 70 C), da concentração da solução osmótica de sacarose (variando de 40 a 70 g por 100 g de solução) e da interação dessas variáveis através de planejamento experimental 22 com três repetições no ponto central (em duplicata). Análises de umidade (método gravimétrico), sólidos solúveis (refratômetro), açúcares totais (cromatografia líquida de alta eficiência) foram realizadas ao longo do processo de desidratação osmótica, enquanto que, as análises de carotenoides totais (espectrofotômetro), atividade de água (método higrométrico) e cor (escala CIELAB) foram realizadas para a fruta in natura e após 10 horas de processamento. Adicionalmente, testes utilizando uma sonda de ultrassom (frequência de 20 KHz, amplitude de 80 % durante 30 minutos) como pré-tratamento ao processo de desidratação osmótica foram realizados, a fim de aumentar a permeabilidade da casca cerosa desta fruta. Além disso, foram realizadas análises de atividade de água e da viscosidade das soluções osmóticas utilizadas neste trabalho. Os resultados mostraram que a utilização da sonda de ultrassom como pré-tratamento não apresentou diferenças estatisticamente significativas para nenhum dos parâmetros estudados, dentro da faixa de temperatura e concentração avaliadas. O modelo de Rastogi & Raghavarao mostrou-se adequado para a determinação do conteúdo de umidade e de sacarose no equilíbrio, assim como a utilização do modelo de difusão da Segunda Lei de Fick para a determinação da difusividade mássica efetiva da água e da sacarose na physalis usando os cinco primeiros termos da série. A difusividade mássica efetiva da água variou de 2,44 - 7,60 x 10-10 m2 s-1, enquanto que a da sacarose variou de 2,13 - 3,20 x 10-10 m2 s-1. Dentre todas as condições estudadas no planejamento experimental, o processo de desidratação osmótica mostrou-se mais eficiente quando realizado na temperatura de 70 C e concentração da solução osmótica de 70 g por 100 g de solução. Nessa condição experimental houve uma elevada perda de água (aproximadamente 83 %), além de uma redução estatisticamente significativa na atividade de água da fruta (passando de 0,979 para 0,872 após 10 horas), no entanto, ocorreu a maior perda de carotenoides totais (aproximadamente 50 %). Nessa condição experimental, a matriz do tecido da physalis sofreu alterações que foram comprovadas através da análise microestrutural realizada por Microscopia Eletrônica de Varredura (MEV). Adicionalmente, verificou-se que nenhum dos tratamentos realizados promoveu modificações visualmente perceptíveis na diferença global de cor (ΔE*) devido ao processo de desidratação osmótica. / Physalis peruviana Linnaeus is considered to be an exotic fruit, with a high cost of commercialization, especially in international markets. Its nutraceutical properties and increased productivity in the state of Rio Grande do Sul, associated with its high perishability defined the goal of this work is the following: to study the process of mass transfer during the osmotic dehydration of physalis. It is noteworthy that several studies have evaluated the properties of the bioactive compounds of physalis both in vitro and in vivo; however, there is a shortage of information in the literature regarding the industrialization of physalis. In this work the osmotic dehydration of physalis was carried out evaluating the effects of temperature (ranging from 40 to 70 °C), osmotic sucrose solution concentration (ranging from 40 to 70 g per 100 g solution) and the interaction of these variables by a 22 experimental design, with three replicates at the center point (in duplicate). Analyses of moisture content (gravimetric method), soluble solids (refractometer) and total sugars (high performance liquid chromatography - HPLC) were performed along the osmotic dehydration process. Content of total carotenoids (spectrophotometer), water activity (hygrometric method) and color (CIELAB scale) were analyzed for the fresh fruit and after 10 hours of processing. In addition, tests using an ultrasound probe (frequency 20 kHz, amplitude of 80 % for 30 minutes) as a pretreatment for the process of osmotic dehydration were performed to increase the permeability of the waxy skin of this fruit. Furthermore, analyses of the water activity and viscosity of the osmotic solutions used were carried out. The results show that the use of the ultrasound probe as a pre-treatment did not yield statistically significant differences for any of the parameters studied within the temperature range at the concentrations assessed. The model of Rastogi & Raghavarao proved to be suitable for the determination of equilibrium content; Fick's Second Law was satisfactorily used to determine the effective diffusivity of water and sucrose for a spherical geometry. Thus, the effective diffusivity of water was calculated and ranged from 2.44 to 7.60 x 10-10 m2 s-1, while that of sucrose ranged from 2.13 to 3.20 x 10-10 m2 s-1. Among all conditions studied in the experimental design, the osmotic dehydration process was more efficient when performed at a temperature of 70 °C and an osmotic solution concentration of 70 g per 100 g of solution. In these conditions, there was a high water loss (approximately 83 %) and a statistically significant reduction in the water activity of this fruit (from 0.979 to 0.872 after 10 hours); however, the greatest loss of total carotenoids (approximately 50 %) was observed. Under this experimental condition, the tissue matrix of physalis suffered structural changes, as proven through Scanning Electron Microscopy (SEM) analysis. Additionally, it was found that none of the treatments performed promoted visually perceptible changes in the overall color difference (ΔE*) due to processing.

The purposes of this research were to determine the efficacy of using the Ogawa® passive sampling device (PSD) to measure ammonia and to identify significant ammonia sources adjacent to Hillsborough and Tampa Bay. Ninety-four samplers were deployed over a 180-km2 area for two weeks in October 2001. Within the area sampled were located suburbs, an urban center, major highways, port activities, fertilizer manufacturing, wastewater treatment, coal-combustion power plants, warehousing and dairy farming. The sampled locations were arranged in a triangular grid pattern spaced 1.5 km apart. The pattern was designed to locate circular hot spots with a minimum radius of 0.75 km. The minimum, maximum, mean, and median ammonia concentrations were 0.06, 15, 2.0, and 1.5 mg/m3, respectively, and the estimated precision was 16%. Hot spots identified from kriged concentration data coincided with inventoried ammonia sources. The relative bias and precision of the PSD based on collocation with an annular denuder system were (plus or minus) 30 % and 20 %.

Zeolite membranes have great potential in gas separation applications because of their unique selective properties. The main challenge is in synthesizing defect-free zeolite membranes. In this study, we synthesized silicalite-1 zeolite membranes on ceramic supports composed of Al2O3 and TiO2 using the pore-plugging method. We investigated the effect of the fill-level in the autoclave during the synthesis on the membrane performance. In particular, we were interested in determining the conditions at which the defects' contribution to the total transport is minimized. We adopted and further developed the approach proposed by Carter (2019) to quantify the permeance contribution through defects. Comparing the membrane performance before and after calcination, we proposed several modifications to the original analysis of Carter (2019). Knowing the defect transport contribution, we determined the corrected diffusivity, an intrinsic property of zeolite crystals at a given temperature, of several adsorbed gases on silicalite-1 crystals. The defect's contribution decreased as the autoclave fill-level increased from 94 to 98%. A further increase in the autoclave fill-level introduced more defects and caused the autoclave lid to rupture. Despite the differences in the membranes' performance arising from the autoclave fill-level, the corrected diffusivities of CO2, CH4, and N2 in silicalite-1 showed minimal variation from membrane to membrane. This proves the validity of the proposed characterization method. Moreover, the reported corrected diffusivities are comparable to the literature's values, found using other characterization methods. However, none of the previously used methods is as simple and straightforward as the one we further developed in this study.

No description available.

This study focuses on factors that affect the structural integrity of wood-based composites. Wood-based composites exposed to fire may decompose due to the elevated temperatures, resulting in a degradation in performance. Thermal modelling can only predict the structural integrity of construction materials in fire if it is given accurate inputs. Consequently, methods for the characterization of the thermal, physical, and mechanical behaviors of wood and wood-based composites are selected, designed, and benchmarked. The relevant thermal and physical responses characterized includes porosity, permeability and thermal diffusivity. Common construction materials (white pine board, medium density fiberboard and spruce 24) are characterized from room temperature to complete decomposition. The characterization techniques and processes are based on existing literature and relevant ASTM standards. To reduce the number of experiments required for future material characterization, estimates based upon the degree of decomposition and the measured values for the virgin and charred materials are used. For porosity and thermal diffusivity, these models allow values at intermediate temperatures to be estimated with measurements at room temperature and complete decomposition and thermogravimetric analysis (TGA). We find that permeability depends heavily on the microstructure of materials and should be measured independently at the conditions of interest. An additional important aspect of the performance of wood-based composites is the fracture behavior of wood/adhesive systems. Adhesive bonding enables many engineered wood products such as furniture and structural wood joints and the adhesive fracture toughness often determines the durability. The conventional characterization method for wood/adhesive fracture resistance relies on samples with machined grain angles designed to funnel cracks to the adhesive interface. This method of sample preparation is difficult and time-consuming for certain wood species. In this work, a practical and efficient method is developed to characterize adhesive fracture energy of adhesively bonded veneer systems. In the method, auxiliary aluminum adherends are bonded to the veneers in an effort to drive the crack to the wood/adhesive interface. The method is applied to rotary-peeled veneers and saw-cut veneers produced from three species of wood bonded with three commonly used adhesives. The new tests method yields a high interfacial failure rate and successfully identifies differences in the performance of the three adhesives. SPG (one species of the rotary-peeled veneers) demonstrates a rising R-curve behavior (an increase in the fracture toughness with crack length) when bonded on the loose side. This increase in fracture toughness is observed to be a result of adhesive-substrate interaction, which is a developing process zone behind the crack tip consisting of bridged wood ligaments. / Doctor of Philosophy / Construction materials exposed to elevated temperatures from fires may reach temperatures where the material decomposes from the original material to a char. Protected and unprotected structural timber products exposed to fires may exhibit this behavior resulting in a degradation of performance. Understanding the thermal and physical responses of these materials is crucial in evaluating the materials behavior in fire. Additionally, many wood-based products (such as furniture) rely on adhesive bonds. Consequently, their usefulness is determined by the performance of those bonds. In this work, methods are developed to measure key properties impacting the behavior of wood-based systems at elevated temperatures, such as that experienced in fires and when they are subjected to forces attempting to debond one wood material from another. These techniques are demonstrated on common building materials (white pine board, medium density fiberboard and spruce 24) and wood veneers from three different species bonded with three different adhesives. Mathematical models are developed to expand the use of the data beyond the specific conditions for which it is measured.