Orientador: Priscila Lupino Gratão / Resumo: As plantas estão expostas a adversidades no ambiente que as circundam, como a contaminação por cádmio (Cd). Este metal pesado tem aumentado na atmosfera devido a atividades humanas. As plantas podem absorver o Cd, causando sérias alterações estruturais, fisiológicas e bioquímicas. As plantas desenvolveram sistemas de defesa complexos, incluindo mecanismos não enzimáticos e enzimáticos para evitar uma cascata de oxidação descontrolada causada pelo estresse oxidativo. Alguns elementos, como o selênio (Se), se utilizados em concentração adequadas, podem induzir uma melhora no sistema antioxidante, no crescimento e nos atributos fotossintéticos. Ainda é pouco conhecido o papel do Se nas respostas das plantas ao estresse. O objetivo deste trabalho foi obter novas informações sobre o papel do selenato e selenito no sistema de desintoxicação das plantas, incluindo a avaliação da nutrição mineral, atividade de enzimas antioxidantes e conteúdo de compostos não enzimáticos, pigmentos, alterações estruturais e o papel do Se na modulação do etileno, com o uso de mutantes hormonais como ferramenta. Nossos dados indicam que o Se é uma estratégia interessante para melhorar o metabolismo da planta sob condições normais ou estressantes. O selênio pode induzir aumento da ação do metabolismo de defesa antioxidante, provavelmente devido a alterações na sinalização do etileno. Além disso, em condições normais, o Se induz alterações estruturais nas células, o que pode contribuir para o desenvolvim... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Cadmium (Cd) contamination is a worldwide concern and one of the most severe causes of abiotic stress in plants, triggering losses in crop production and contamination risks to human health. This heavy metal increased in atmosphere due to human activities. Plants can uptake Cd, causing serious changes in structural, physiological and biochemical processes. Plants developed a complex defence systems including non-enzymatic and enzymatic mechanism to avoid oxidative stress and prevent an uncontrolled oxidation cascade. Some elements, such as selenium (Se), if used in adequate concentration, may induce an improvement in antioxidant system, growth and photosynthetic attributes. It is still unknown the mechanisms of Se in stress responses. The aim of this work was get new insights about the role of selenate and selenite-mediated detoxification strategies, including the evaluation of mineral nutrition, the activity of antioxidant enzymes and non enzymatic compounds, pigments, structural alterations and the role of Se in modulate ethylene, with the use of hormonal mutants as a tool. Our data indicates that Se is an interesting strategy to improve plant metabolism under normal or Cd stressful-condition. Selenium may induce enhancement in antioxidant defence metabolism, probably due to alterations in ethylene signalling. Moreover, under normal condition Se induce structural alterations in cells, which may contribute to plant development. Thus, the information available in this work is... (Complete abstract click electronic access below) / Doutor

This dissertation is focused on understanding heterogeneous metal catalysts supported on oxides using a model catalyst system of SiO2 thin film supported metal nano-clusters. The primary technique applied to this study is scanning tunneling microscopy (STM). The most important constituent of this model catalyst system is the SiO2 thin film, as it must be thin and homogeneous enough to apply electron or ion based surface science techniques as well as STM. Ultra-thin SiO2 films were successfully synthesized on a Mo(112) single crystal. The electronic and geometric structure of the SiO2 thin film was investigated by STM combined with LEED, Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS). The relationship between defects on the SiO2 thin film and the nucleation and growth of metal nano-clusters was also investigated. By monitoring morphology changes during thermal annealing, it was found that the metal-support interaction is strongly dependent on the type of metal as well as on the defect density of the SiO2 thin film. Especially, it was found that oxygen vacancies and Si impurities play an important role in the formation of Pd-silicide. By substituting Ti atoms into the SiO2 thin film network, an atomically mixed TiO2-SiO2 thin film was synthesized. Furthermore, these Ti atoms play a role as heterogeneous defects, resulting in the creation of nucleation sites for Au nano-clusters. A marked increase in Au cluster density due to Ti defects was observed in STM. A TiO2-SiO2 thin film consisting of atomic Ti as well as TiOx islands was also synthesized by using higher amounts of Ti (17 %). More importantly, this oxide surface was found to have sinter resistant properties for Au nano-clusters, which are desirable in order to make highly active Au nano-clusters more stable under reaction conditions.

This dissertation is focused on understanding heterogeneous metal catalysts supported on oxides using a model catalyst system of SiO2 thin film supported metal nano-clusters. The primary technique applied to this study is scanning tunneling microscopy (STM). The most important constituent of this model catalyst system is the SiO2 thin film, as it must be thin and homogeneous enough to apply electron or ion based surface science techniques as well as STM. Ultra-thin SiO2 films were successfully synthesized on a Mo(112) single crystal. The electronic and geometric structure of the SiO2 thin film was investigated by STM combined with LEED, Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS). The relationship between defects on the SiO2 thin film and the nucleation and growth of metal nano-clusters was also investigated. By monitoring morphology changes during thermal annealing, it was found that the metal-support interaction is strongly dependent on the type of metal as well as on the defect density of the SiO2 thin film. Especially, it was found that oxygen vacancies and Si impurities play an important role in the formation of Pd-silicide. By substituting Ti atoms into the SiO2 thin film network, an atomically mixed TiO2-SiO2 thin film was synthesized. Furthermore, these Ti atoms play a role as heterogeneous defects, resulting in the creation of nucleation sites for Au nano-clusters. A marked increase in Au cluster density due to Ti defects was observed in STM. A TiO2-SiO2 thin film consisting of atomic Ti as well as TiOx islands was also synthesized by using higher amounts of Ti (17 %). More importantly, this oxide surface was found to have sinter resistant properties for Au nano-clusters, which are desirable in order to make highly active Au nano-clusters more stable under reaction conditions.

Conselho Nacional de Desenvolvimento CientÃfico e TecnolÃgico / Uma parcela significativa da pesquisa cientÃfica hodierna baseia-se na sÃntese, caracterizaÃÃo ou aplicaÃÃo de materiais nanoestruturados. No intuito de possibilitar um maior entendimento das intrigantes propriedades destes materiais, muitas tÃcnicas com resoluÃÃo nanomÃtrica e atà subnanomÃtrica foram criadas nos Ãltimos 50 anos e tÃm passado por um processo de contÃnuo aprimoramento. Apesar do grande desenvolvimento tÃcnico e cientÃfico da instrumentaÃÃo disponÃvel, a caracterizaÃÃo Ãtica com resoluÃÃo nanomÃtrica destes materiais tem se mostrado um desafio para pesquisadores do mundo inteiro. Nesse contexto, as tÃcnicas baseadas em radiaÃÃo de campo prÃximo tÃm despontado como uma boa alternativa para quebra do limite de difraÃÃo, que constitui um limite natural para os instrumentos Ãticos convencionais. AlÃm disso, a microscopia de campo prÃximo em modo de iluminaÃÃo e contato adquire simultaneamente informaÃÃes Ãticas e topogrÃficas do material, o que permite fazer uma distinÃÃo entre as propriedades Ãticas nanomÃtricas reais e as induzidas por topografia. O fenÃmeno de domÃnios cristalogrÃficos tem sido um assunto de interesse da cristalografia desde que ela comeÃou a se desenvolver como ciÃncia. As razÃes Ãbvias para isso sÃo a beleza de formas externas de algumas estruturas de domÃnios, assim como as evidentes e desafiantes relaÃÃes de simetria entre os seus constituintes. Os domÃnios ferroelÃsticos sÃo um dos importantes tipos de domÃnios apresentados por cristais. Tais domÃnios apresentam, algumas vezes, dimensÃes muito reduzidas sem manifestar uma considerÃvel alteraÃÃo na estrutura topogrÃfica da amostra. Por outro lado, o comportamento Ãtico de domÃnios distintos pode ser bem diferente quando sujeitos a uma mesma condiÃÃo de medida. Tais caracterÃsticas tornam esta classe de materiais ideais para um estudo baseado na microscopia de campo prÃximo em modo de iluminaÃÃo e contato. Imagens de domÃnios ferroelÃsticos, utilizando microscopia de campo prÃximo em modo de iluminaÃÃo e contato, foram obtidas com resoluÃÃo nanomÃtrica. Tais imagens, em geral, apresentaram pouquÃssima relaÃÃo com a estrutura topogrÃfica do material, revelando importantes caracterÃsticas Ãticas (ocorrÃncia do efeito de guias de onda nos domÃnios) e estruturais (dimensÃes dos domÃnios ferroelÃsticos, presenÃa de defeitos de deslocamento na rede cristalina). / A significant part of the nowadays scientific research is based on the synthesis, characterization and application of the nanostructured materials. In order to make possible a further understanding of the intriguing properties of these materials, many techniques with nanometric and even subnanometric resolution have been created during the last 50 years and are passing through a process of continuous improvement. In spite of the great scientific and technical development on the available instrumentation, the optical characterization with nanometric resolution of these materials remains a challenge for researchers from all over the world. In this context, techniques based on near field radiation have emerged as a great alternative for the diffraction limit break which is a nature imposed limit for conventional optical instruments. Besides this, contact near field microscopy in illumination mode acquires optical and topographical information of the material simultaneously. This capability permits the distinction between the real and topographic induced nanometric optical features. The domain phenomenon in crystals has been a subject of interest for crystallographers since crystallography started to develop as a scientific branch. The obvious reasons are the beauty of some domain patterns as well as evident and challenging symmetry relations between their constituents. The ferroelastic domains are one of the important kinds of domains presented by crystals. They have, sometimes, very small dimensions without inducing any topographic element on the sample. On the other side the optical behavior of different domains under almost the same measurement condition may be very dissimilar. Such characteristics make then an ideal class of materials for contact near field microscopy in illumination mode based studies. Ferroelastic domains images, using near-field optical microscopy in illumination and contact mode, were obtained with a nanometric resolution. Such images, in general, presented very little relation with the topographical structure of the material, revealing optical and structural features such as occurrence of the waveguide effect in the domains, domainÂs dimensions and presence of dislocations on the crystalline structure.  

The mechanisms linking deposits of insoluble fibrils of amyloid proteins to the debilitating neuronal cell death characteristic of neurodegenerative diseases remain enigmatic. Recent findings suggest that transiently formed intermediate aggregates, and not the prominent neuronal plaques, represent the principal toxic agent. Evaluating the neurotoxicity of intermediate aggregates, however, requires unambiguous characterization of all aggregate structures present, their relative distributions, and how they evolve in time. Hen-egg white lysozyme represents an attractive model for studying intermediate aggregate formation since it is an extensively characterized globular protein, and its human variants can lead to systemic amyloidosis. Combining in-situ dynamic light scattering (DLS) with atomic force microscopy (AFM), we have characterized the morphologies and growth kinetics of intermediate aggregates formed during lysozyme fibrillogenesis. Upon incubation at elevated temperatures, small uniform oligomers form with their numbers increasing for several hours. After a variable lag period protofibrils spontaneously nucleate. The heights and widths of protofibrils closely match those of oligomers. This match in physical dimensions, combined with the delayed onset of protofibril nucleation vs. the continuous formation of oligomers, suggest that protofibrils both nucleate and grow from oligomers. Protofibril morphologies and structures, visualized with AFM, are quite distinct from subsequently emerging mature fibrils. Overall, the evolution of aggregate morphologies during lysozyme fibrillogenesis follows a clear hierarchical pathway: amyloid monomers initially coalesce into oligomers of uniform size. Their steadily increasing numbers eventually induce nucleation and growth of protofibrils. Protofibrils, in turn, nucleate and grow via oligomer addition until they start to self-assemble into micron-sized double-stranded fibrils.

DANTAS, Saulo Maia. Microscopia de campo próximo aplicada ao estudo dos domínios ferroelásticos. 2011. 116 f. Dissertação (Mestrado em Física) - Programa de Pós-Graduação em Física, Departamento de Física, Centro de Ciências, Universidade Federal do Ceará, Fortaleza, 2011. / Submitted by Edvander Pires (edvanderpires@gmail.com) on 2015-10-16T20:43:18Z No. of bitstreams: 1 2011_dis_smdantas.pdf: 2227981 bytes, checksum: 19c007c3550b22fce922a346d6f4508f (MD5) / Approved for entry into archive by Edvander Pires(edvanderpires@gmail.com) on 2015-10-21T20:37:21Z (GMT) No. of bitstreams: 1 2011_dis_smdantas.pdf: 2227981 bytes, checksum: 19c007c3550b22fce922a346d6f4508f (MD5) / Made available in DSpace on 2015-10-21T20:37:21Z (GMT). No. of bitstreams: 1 2011_dis_smdantas.pdf: 2227981 bytes, checksum: 19c007c3550b22fce922a346d6f4508f (MD5) Previous issue date: 2011 / A significant part of the nowadays scientific research is based on the synthesis, characterization and application of the nanostructured materials. In order to make possible a further understanding of the intriguing properties of these materials, many techniques with nanometric and even subnanometric resolution have been created during the last 50 years and are passing through a process of continuous improvement. In spite of the great scientific and technical development on the available instrumentation, the optical characterization with nanometric resolution of these materials remains a challenge for researchers from all over the world. In this context, techniques based on near field radiation have emerged as a great alternative for the diffraction limit break which is a nature imposed limit for conventional optical instruments. Besides this, contact near field microscopy in illumination mode acquires optical and topographical information of the material simultaneously. This capability permits the distinction between the real and topographic induced nanometric optical features. The domain phenomenon in crystals has been a subject of interest for crystallographers since crystallography started to develop as a scientific branch. The obvious reasons are the beauty of some domain patterns as well as evident and challenging symmetry relations between their constituents. The ferroelastic domains are one of the important kinds of domains presented by crystals. They have, sometimes, very small dimensions without inducing any topographic element on the sample. On the other side the optical behavior of different domains under almost the same measurement condition may be very dissimilar. Such characteristics make then an ideal class of materials for contact near field microscopy in illumination mode based studies. Ferroelastic domains images, using near-field optical microscopy in illumination and contact mode, were obtained with a nanometric resolution. Such images, in general, presented very little relation with the topographical structure of the material, revealing optical and structural features such as occurrence of the waveguide effect in the domains, domain´s dimensions and presence of dislocations on the crystalline structure. / Uma parcela significativa da pesquisa científica hodierna baseia-se na síntese, caracterização ou aplicação de materiais nanoestruturados. No intuito de possibilitar um maior entendimento das intrigantes propriedades destes materiais, muitas técnicas com resolução nanométrica e até subnanométrica foram criadas nos últimos 50 anos e têm passado por um processo de contínuo aprimoramento. Apesar do grande desenvolvimento técnico e científico da instrumentação disponível, a caracterização ótica com resolução nanométrica destes materiais tem se mostrado um desafio para pesquisadores do mundo inteiro. Nesse contexto, as técnicas baseadas em radiação de campo próximo têm despontado como uma boa alternativa para quebra do limite de difração, que constitui um limite natural para os instrumentos óticos convencionais. Além disso, a microscopia de campo próximo em modo de iluminação e contato adquire simultaneamente informações óticas e topográficas do material, o que permite fazer uma distinção entre as propriedades óticas nanométricas reais e as induzidas por topografia. O fenômeno de domínios cristalográficos tem sido um assunto de interesse da cristalografia desde que ela começou a se desenvolver como ciência. As razões óbvias para isso são a beleza de formas externas de algumas estruturas de domínios, assim como as evidentes e desafiantes relações de simetria entre os seus constituintes. Os domínios ferroelásticos são um dos importantes tipos de domínios apresentados por cristais. Tais domínios apresentam, algumas vezes, dimensões muito reduzidas sem manifestar uma considerável alteração na estrutura topográfica da amostra. Por outro lado, o comportamento ótico de domínios distintos pode ser bem diferente quando sujeitos a uma mesma condição de medida. Tais características tornam esta classe de materiais ideais para um estudo baseado na microscopia de campo próximo em modo de iluminação e contato. Imagens de domínios ferroelásticos, utilizando microscopia de campo próximo em modo de iluminação e contato, foram obtidas com resolução nanométrica. Tais imagens, em geral, apresentaram pouquíssima relação com a estrutura topográfica do material, revelando importantes características óticas (ocorrência do efeito de guias de onda nos domínios) e estruturais (dimensões dos domínios ferroelásticos, presença de defeitos de deslocamento na rede cristalina).

The integration of sensors, actuators, and control systems is an ongoing process in a wide range of applications covering automotive, medical, military, and consumer electronic markets. Four major families of ceramic and metallic actuators are under development: piezoelectrics, electrostrictors, magnetostrictors, and shape-memory alloys. All of these materials undergo at least two phase transformations with coupled thermodynamic order parameters. These transformations lead to complex domain wall behaviors, which are driven by electric fields (ferroelectrics), magnetic fields (ferromagnetics), or mechanical stress (ferroelastics) as they transform from nonferroic to ferroic states, contributing to the sensing and actuating capabilities. This research focuses on two multiferroic crystals, Pb(Mg1/3Nb2/3)O3-PbTiO3 and Fe-Ga, which are characterized by the co-existence and coupling of ferroelectric polarization and ferroelastic strain, or ferro-magnetization and ferroelastic strain. These materials break the conventional boundary between piezoelectric and electrostrictors, or magnetostrictors and shape-memory alloys. Upon applying field or in a poled condition, they yield not only a large strain but also a large strain over field ratio, which is desired and much benefits for advanced actuator and sensor applications. In this thesis, particular attention has been given to understand the structure-property relationships of these two types of materials from atomic to the nano/macro scale. X-ray and neutron diffraction were used to obtain the lattice structure and phase transformation characteristics. Piezoresponse and magnetic force microscopy were performed to establish the dependence of domain configurations on composition, thermal history and applied fields. It has been found that polar nano regions (PNRs) make significant contributions to the enhanced electromechanical properties of PMN-x%PT crystals via assisting intermediate phase transformation. With increasing PT concentration, an evolution of PNRï  PND (polar nano domains)-> micron-domains-> macro-domains was found. In addition, a domain hierarchy was observed for the compositions near a morphotropic phase boundary (MPB) on various length scales ranging from nanometer to millimeter. The existence of a domain hierarchy down to the nm scale fulfills the requirement of low domain wall energy, which is necessary for polarization rotation. Thus, upon applying an E-field along <001> direction(s) in a composition near the MPB, low symmetry phase transitions (monoclinic or orthorhombic) can easily be induced. For PMN-30%PT, a complete E-T (electric field vs temperature) diagram has been established. As for Fe-x at.% Ga alloys, short-range Ga-pairs serve as both magnetic and magnetoelastic defects, coupling magnetic domains with bulk elastic strain, and contributing to enhanced magnetostriction. Such short-range ordering was evidenced by a clear 2theta peak broadening on neutron scattering profiles near A2-DO3 phase boundary. In addition, a strong degree of preferred [100] orientation was found in the magnetic domains of Fe-12 at.%Ga and Fe-20 at.%Ga alloys with the A2 or A2+DO3 structures, which clearly indicates a deviation from cubic symmetry; however, no domain alignment was found in Fe-25 at.%Ga with the DO3 structure. Furthermore, an increasing degree of domain fluctuations was found during magnetization rotation, which may be related to short-range Ga-pairs cluster with a large local anisotropy constant, due to a lower-symmetry structure. / Ph. D.

En este trabajo se ha desarrollado un microscopio de fuerzas (SFM) provisto de microscopía electrostática (ESFM) y microscopía Kelvin (KPM) especialmente diseñado para integrarse en un microscopio óptico invertido de forma que combine simultáneamente las técnicas de campo cercano con las técnicas ópticas. Tras una introducción (capítulo 1) y la descripción de las técnicas experimentales (capítulo 2), se detallan las características del diseño de un primer prototipo, así como las medidas realizadas con él con el fin de comprobar su correcto funcionamiento (capítulo 3). El capítulo 4 muestra el diseño de un segundo prototipo con las mejoras que incorpora respecto al primero, que lo convierten en un sistema más completo, versátil y fácil de manejar. También figuran las medidas realizadas con él. El capítulo 5 muestra un estudio de fotodegradación en polímeros conductores en función de la radiación incidente, combinando microscopía electrostática y Kelvin con técnicas ópticas. / In this work we have developed an Scanning Force Microscope (SFM) equipped with Electrostatic and Kelvin Probe Microscopy (ESFM, KPM), specially designed for integration into an inverted optical microscope in order to combine near-field techniques with optical techniques. After an introduction (Chapter 1) and the description of the experimental techniques (Chapter 2), are described the features of the design of a first prototype, as well as the measurements made with it in order to verify proper operation (Chapter 3). The Chapter 4 shows the design of a second prototype that incorporates the improvements over the first, making it more comprehensive, versatile and easy to handle. Also are shown the measurements performed with it. The Chapter 5 shows a photodegradation study of conductive polymers as a function of incident radiation combining KPM with optical techniques.

Apesar do alto e significativo índice de sucesso dos implantes osseointegráveis, fracassos podem ser acarretados por diversos fatores, tais como falhas cirúrgicas, protéticas, trauma oclusal e por infecções nos tecidos ao redor do implante. As lesões inflamatórias desenvolvidas ao redor de implantes são conhecidas coletivamente como doença peri-implantar, que possui um papel muito importante na falência de implantes, sendo considerada uma das principais causas. O objetivo deste trabalho foi analisar a ação antibacteriana de filme nanoestruturado com partículas de prata aplicado em superfície de titânio de componentes protéticos conectados a implantes, em relação às bactérias predominantes na infecção peri-implantar. Para avaliar a ação antibacteriana do filme nanoestruturado com partículas de prata foi realizado teste microbiológico com cepas de Aggregatibacter actinomycetemcomitans (ATCC 43719), Fusobacterium nucleatum (ATCC 25586) e Porphyromonas gingivalis (ATCC 33277). Discos de titânio sem tratamento formaram o grupo controle (Ti) e discos com filme nanoestruturado com partículas de prata, o grupo teste (NT-Ag). Cada teste foi realizado em triplicata e repetido por três ocasiões separadas. Após 48 horas de incubação dos discos em caldo de infusão de cérebro e coração (BHI), previamente inoculado com as cepas, a 37 °C, em anaerobiose, os discos foram então retirados e colocados em um tubo contendo solução tampão fosfato-salina (PBS) e centrifugados por 1 minuto em aparelho tipo vortex. O PBS foi diluído em série até 1:100.000, distribuído em placas de ágar sangue e essas foram incubadas por 48 horas, a 37ºC, em anaerobiose e então foi feita a contagem de colônias sobre as placas para posterior calculo das unidades formadoras de colônia (UFC). A análise da adesão bacteriana foi realizada com cepas de Aggregatibacter actinomycetemcomitans (ATCC 43719), Fusobacterium nucleatum (ATCC 25586) e Porphyromonas gingivalis (ATCC 33277), através da leitura dos discos em microscópio eletrônico de varredura Leo 43, após imersão dos discos em BHI inoculado. O teste antibacteriano, realizado com Aggregatibacter actinomycetemcomitans, apresentou valor médio de UFC/mL do grupo teste (NT-Ag) semelhante ao obtido do grupo controle (Ti), não havendo diferença estatística (p<0,01) entre eles. Os testes realizados com Fusobacterium nucleatum e Porphyromonas gingivalis não apresentaram crescimento bacteriano, na etapa de leitura das placas, para os dois grupos, controle (Ti) e teste (NT-Ag). As imagens obtidas, através do microscópio eletrônico de varredura (MEV), demonstraram uma notável redução da adesão bacteriana, nos discos com filme nanoestruturado com partículas de prata (NT-Ag), em comparação com as imagens do grupo controle (Ti), para todas as cepas, porém não são conclusivas. O filme nanoestruturado com partículas de prata não foi efetivo na redução da adesão de A. actinomycetemcomitans. / Despite the high and significant success rate of dental implants, failures can be posed by various factors such as surgical and prosthetic failures, oclusal trauma and infections in the tissues around the implant. The inflammatory lesions developed around implants are collectively known as peri-implant disease, which has a very important role in implant failure and is considered one of the main causes. The aim of this study was to evaluate the antibacterial activity of nanostructured film with silver particles, applied on abutments connected to implants, in relation to the predominant bacteria in peri-implant infection. To evaluate the antibacterial activity of the nanostructured film, microbiological tests were performed with strains of Aggregatibacter actinomycetemcomitans (ATCC 43719), Fusobacterium nucleatum (ATCC 25586) and Porphyromonas gingivalis (ATCC 33277). Untreated titanium discs were the control group (Ti) and discs with the nanostructured film with silver particles formed the test group (NT-Ag). Each test was run in triplicate and repeated on three separate occasions. After 48 hours of discs incubation in brain heart infusion broth (BHI), previously inoculated with the strains, at 37 °C, under anaerobic conditions, the discs were then removed and placed in a tube containing phosphate buffered saline solution (PBS) and vortexed for 1 minute. The PBS was serially diluted up to 1:100,000, distributed in blood agar plates and incubated for 48 hours, at 37 ° C in anaerobiosis and then colonies were counted for subsequent calculation of colony forming units (CFU). The analysis of bacterial adhesion was performed with strains of Aggregatibacter actinomycetemcomitans (ATCC 43719), Fusobacterium nucleatum (ATCC 25586) and Porphyromonas gingivalis (ATCC 33277) by reading the discs surface in a scanning electron microscope Leo 43, after immersion of the discs on inoculated BHI. The antibacterial test, performed with Aggregatibacter actinomycetemcomitans, obtained CFU/mL medium value from the test group (NT-Ag) similar to the obtained in the control group (Ti), showing no statistical difference (p <0.01) between them. The tests performed with Fusobacterium nucleatum and Porphyromonas gingivalis showed no bacterial growth, in plates reading step, for both groups, control (Ti) and test (NT-Ag). The images obtained by scanning electron microscopy showed a remarkable reduction of bacterial adhesion, on discs with nanostructured film with silver particles (NT-Ag), when compared to the images of the control group (Ti), for all strains, but they were not conclusive. The nanostructured film with silver particles was not effective in reducing bacterial adhesion of A. actinomycetemcomitans.

A qualidade final do preparo do canal destaca-se, dentre outras condições, pela ausência de magma dentinário e pelo aumento da permeabilidade dentinária, de modo a permitir pela primeira, a falta de substrato para desenvolvimento de microbiota e melhor adaptação do material obturador e, pelo segundo a possibilidade de alcançar na maior profundidade do túbulo dentinário as sujidades ali eventualmente presentes e fazer com que a medicação intracanal atue plenamente no sistema endodôntico. Metodologias experimentais de avaliação dessas qualidades aferem isoladamente cada uma delas dificultando a percepção de que a interação de ambas poderia permitir compreender o seu real papel no êxito da terapia endodôntica. O objetivo deste estudo consistiu-se em criar um procedimento capaz de, no mesmo espécime dental, avaliar a presença de magma e o quanto de permeabilidade dentinária radicular se alcança após o preparo químico-cirúrgico e a irrigação-aspiração final com diferentes irrigantes. Quarenta dentes unirradiculares humanos foram preparados com instrumentos rotatórios e Endo-PTC + NaOCl a 1% e divididos em quatro grupos (n=10) no momento da irrigação-aspiração final de acordo com o irrigante a ser empregado: G I (controle) - NaOCl a 1%; G II - EDTA a 17%; G III - EDTA-T a 17% e G IV - MTAD®. Os canais foram preenchidos com azul de metileno a 0,5% e mantidos em frascos por 48 h. Decorrido este tempo, as coroas foram removidas e as raízes foram clivadas no sentido transversal obtendose fragmentos do terço cervical, médio e apical. Os espécimes foram fotografados e analisados no programa ImageLab quanto à penetração do corante. Após esta análise, os fragmentos foram novamente clivados no sentido longitudinal e preparados para MEV. As eletromicrografias foram analisadas por três diferentes avaliadores e qualificadas por escores. As substâncias irrigadoras utilizadas, quando comparadas entre si, tiveram efeitos semelhantes sobre a permeabilidade dentinária, considerando as raízes por inteiras e pelos seus terços. Na avaliação individual das substâncias irrigadoras, as diferenças de permeabilidade entre os terços radiculares não foram estatisticamente significantes, exceto para o EDTA-T cujo terço apical teve menor penetração do corante. Quando a substância irrigadora com ação quelante/desmineralizante foi empregada para irrigação-aspiração final do canal radicular, o magma dentinário foi eficientemente removido enquanto a irrigação somente com NaOCl não foi suficiente para remover o magma. Os três terços do canal radicular apresentaram o mesmo grau de limpeza das paredes da dentina radicular, exceto para o EDTA-T, cujo terço apical apresentou maior quantidade de magma quando comparado aos terços cervical e médio. A vinculação dos resultados estatísticos da permeabilidade dentinária com a remoção do magma dentinário não mostrou a mesma relação uniforme para as substâncias irrigadoras avaliadas, quer na sua totalidade quer nos seus terços, deduzindo-se que maior ou menor permeabilidade necessariamente não corresponde a menor ou maior presença de magma dentinário. As análises da permeabilidade dentinária e da remoção do magma dentinário, com aplicação inicial do corante seguido de processamento para MEV, mostraram-se viáveis nos mesmos espécimes radiculares. / After root canal preparation and removal of smear layer, penetration of intracanal dressing deep in dentinal tubules to reduce microbial growth is enhanced. Removal of smear layer also permits a more effective cleaning of organic tissue and bacteria from within the dentinal tubules and allows a better adaptation of obturation material along root canal walls. Other studies have evaluated smear layer removal and dentinal permeability in isolation on different specimens, making it difficult to interpret the interaction between smear layer and dentin permeability and their real roles in root canal treatment. The aim of this study was to create a procedure to evaluate the presence of smear layer and what its influence is on root dentin permeability after chemomechanical root canal preparation and final irrigation-aspiration with different chemicals using the same specimen. Forty single root human teeth were instrumented with rotary instruments and Endo-PTC + 1% NaOCl and ramdomly divided into four groups (n=10) at the final rinse step, according to the irrigant used: G I (control) - 1% NaOCl; G II - 17% EDTA; G III - 17% EDTA-T and G IV - MTAD®. The root canals were filled with 0.5% methylene blue and maintained in bottles for 48 h. After this time, the crowns were cut off and the roots were transversally split resulting in three fragments: coronal, middle and apical. The specimens were analyzed using ImageLab software to evaluate dye penetration. After this analysis, the fragments were then axially split and prepared for SEM. The photomicrographs were analyzed by three different evaluators and qualified by scores. When the whole roots were analyzed and the irrigants used were compared among themselves, the same effect on dentin permeability was observed. Individual evaluation of the irrigants showed, the differences in the permeability levels for all 3 root canal thirds were not statistically significant, except for the apical third of the EDTA-T irrigation group which exhibited less dye penetration. When a decalcifying irrigant was used for final rinse, the smear layer was efficiently removed. In contrast a final rinse with NaOCl was not enough to remove this layer. In all irrigation experimental groups the three different thirds of the root canals showed the same amount of smear layer removal, except for the EDTA-T group, which exhibited higher amounts of smear layer removal in the apical third compared to coronal and middle thirds. The results of both studies (dentin permeability and smear layer removal) did not show an even relationship for the irrigants evaluated, neither on their smear layer in the entire canal nor was it observed in each root canal thirds evaluated. This inferres that higher or lower dentinal permeability does not necessarily correspond to a higher or lower amount of smear layer presence. The Pearson correlation test supports these statements. The analysis of dentin permeability with initial introduction of a dye followed by the smear layer removal analysis under SEM, was shown to be a feasible procedure using the same root specimen.