Avaliação da interface de cinco sistemas de implantes e seus respectivos abutments com auxílio do método de microscopia eletrônica de varredura

Pós-graduação em Odontologia - FOA

Influência do tipo de fundição e uso de retificação na interface pilar/cilindro protético na adaptação marginal e tensão peri-implantar sobre conexão protética tipo Micro-Unit

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Avaliação da interface dentina/agentes protetores em restaurações com resina composta, através de microscopia eletrônica de varredura

Pós-graduação em Ciências Odontológicas - FOAR

Avaliação do desajuste vertical da interface implante/pilares UCLA com cinta metálica de cinco marcas distintas: análise intra e entre-sistemas

A adaptação passiva entre prótese e implante é fundamental para a longevidade de procedimentos reabilitadores através de implantes odontológicos. Diante disso, este trabalho teve como objetivo avaliar a adaptação na interface UCLA com cinta metálica e implante utilizando-se componentes de um mesmo sistema de implantes e combinações de componentes de diferentes sistemas, através de microscopia eletrônica de varredura. Componentes de 5 empresas foram utilizados: Biomet 3i, Conexão, Neodent, SIN e Titanium fix. Foram realizadas leituras nas interfaces direita e esquerda das várias combinações entre UCLA e implantes, com aumento de 300x. As médias de (des)ajuste vertical foram submetidas a análise estatística pelo teste Student-Newman Keuls, com significância de 5% (p<0,05). Os resultados da análise intra-sistema mostraram desajuste estatisticamente significante para o abutment UCLA SIN com cinta de ouro (desajuste médio 3,88_m) comparando-se com os demais sistemas. Para a análise entre-sistemas, sugere-se que nem todas as combinações podem ser consideradas compatíveis relativamente ao desajuste vertical.

Sistemas adesivos convencional e autocondicionante: análise micromecânica tridimensional da interface dentina-adesivo

Pós-graduação em Odontologia - FOA

Avaliação das propriedades nanomecânicas e do comportamento micromecânico da interface dentina/adesivo antes e após a degradação hidrolítica: análises através de nanoindentação e método dos elementos finitos tridimensional

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Efeitos dos ascorbato de sódio e alfatocoferol na resistência à fratura, resistência de união e na interface adesiva na dentina de dentes tratados endodonticamente submetidos a clareamento dental com peróxido de hidrogênio

Pós-graduação em Ciências Odontológicas - FOAR

Marginal adaptation of class II cavities restored with bulk-fill composites

Objectives: To determine the marginal adaptation of bulk-fill composites in class II MO cavities.Methods: Standardized class II MO cavities with bevelled enamel margins were prepared in 40 extracted human molars. The teeth were randomly assigned to one of the five experimental groups (n = 8). The teeth were restored with two horizontal increments of composite (4 mm and 2 mm thickness). The experimental groups were (1st/2nd increment): Gr. A - Venus Bulk-Fill/Venus Diamond; Gr. B - Tetric EvoCeram BulkFill/Tetric EvoCeram; Gr. C - Surefil SDR/Ceram-X; Gr. D - SonicFill; Gr. E - Ceram-X/Ceram-X (control). After finishing procedures, impressions were made using a polyvinyl siloxane and epoxy resin replicas were obtained. Thermo-mechanical stressing was carried out 24 h after the restorative procedure. All specimens were submitted to 240,000 occlusal loading and simultaneous 600 thermal cycles in water at 5 degrees C and 50 degrees C. After loading, a new set of epoxy resin replicas was obtained. Scanning electron microscopy was carried out at 200x magnification. Results for the marginal adaptation were expressed as percentages of continuity relative to the exposed interface and analyzed by ANOVA and Duncan post hoc test (p < 0.05).Results: In enamel, no significant differences were detected before and after thermo-mechanical loading between groups. In dentine, the worst results were observed in Gr. A.Conclusion: By applying simple layering techniques, bulk-fill materials do not allow better marginal adaptation than a standard composite. Clinical significance: A new class of resin-base composite (bulk-fill) was recently launched on the market. The bulk-fill composites exhibited adequate marginal adaptation and similar to the results of the standard composite. (C) 2014 Elsevier Ltd. All rights reserved.

SEM Evaluation of the Interface Between Filling and Root- End Filling Materials

The aim of this ex vivo study was to evaluate, by scanning electron microscopy (SEM), the presence of gaps at the interface between filling material and three root-end filling materials. Thirty human upper molars disto-buccal roots were instrumented and filled with gutta-percha and eugenol-based sealer. The apicoectomy was performed 2mm from the apex and retrograde cavities were prepared with ultrasonic points (3mm in deep). The samples were divided into three experimental groups (n=10): Group Iwhite mineral trioxide aggregate (MTA); Group IISuper EBA; and Group IIIPortland cement. The root-end filling materials were inserted into the retocavities using a MTA carrier. After 48h, the roots were transversally sectioned in order to obtain the apical 5mm. Next, each specimen was prepared longitudinally with crescent granulation of abrasives water-wet sandpapers in order to expose the filling and root-end filling materials. Then, the specimens were subjected to slow dehydration with silica gel, mounted onto specific stubs and coated with paladium coverage for SEM analysis of the interface between filling and root-end filling materials. The percentage of gaps at the interfacial area was calculated by using Image Tool 3.0 software. Super EBA presented the higher percentage of gaps (1.5 +/- 0.67%), whereas MTA presented the lowest values (0.33 +/- 0.20%; p=0.0004). Despite the statistical differences observed between Super EBA and MTA, all the root-end filling materials presented great adaptation to the filling material, presenting small amount of gaps. SCANNING 36:252-257, 2014. (c) 2013 Wiley Periodicals, Inc.

Effect of Er:YAG laser and diamond drill on hybrid layer morphology obtained with self-etch adhesive: analysis by SEM and confocal laser scanning microscopy (CLSM)

This study aimed to evaluate the effect of Er:YAG (L) and diamond drills (DD) on: 1) the microshear bond strength (MPa); 2) the adhesive interface of two-step (TS) – Adper Scotchbond Multipurpose and one-step (OS) adhesives – Adper EasyOne, both from 3M ESPE. Material and methods: According to the preparation condition and adhesives, the samples were divided into four groups: DD_TS (control); DD_OS; L_TS and L_OS. 60 bovine incisors were randomly divided into experimental and groups: 40 for microshear bond strength (n = 10) and 20 for the adhesive interface morphology [6 to measure the thickness of the hybrid layer (HL) and length of tags (t) by CLSM (n = 3); 12 to the adhesive interface morphology by SEM (n = 3) and 2 to illustrate the effect of the instruments on dentine by SEM (n = 1)]. To conduct the microshear bond strength test, four cylinders (0.7 mm in diameter and 1 mm in height with area of adhesion of 0.38 mm) were constructed with resin composite (Filtek Z350 XT – 3M ESPE) on each dentin surface treated by either L or DD and after adhesives application. Microshear bond strength was performed in universal testing machine (EMIC 2000) with load cell of 500 kgf and a crosshead speed of 0.5 mm / min. Adhesive interface was characterized by thickness of hybrid layer (HL) and length of tags (t) in nm, with the aid of UTHSCSA ImageTool software. Results: Microshear bond strength values were: L_TS 34.10 ± 19.07, DD_TS 24.26 ± 9.35, L_OS 33.18 ± 12.46, DD_OS 21.24 ± 13.96. Two-way ANOVA resulted in statistically significant differences only for instruments (p = 0.047). Mann-Whitney identified the instruments which determined significant differences for HL thickness and tag length (t). Concerning to the adhesive types, these differences were only observed for (t). Conclusion: It can be concluded that 1) laser Er:YAG results in higher microshear bond strength values regardless of the adhesive system (TS and OS); 2) the tags did not significant affect the microshear bond strength; 3) the adhesive interface was affected by both the instruments for cavity preparation and the type of adhesive system used.

Avaliação do selamento de ápices radiculares retrobturados ou recobertos com diferentes materiais mediante infiltração marginal por corante e análise da interface em microscopia eletrônica de varredura

The purpose of this study was to evaluate the apical sealing ability and the marginal adaptation of five dental materials used in retrofillings or applied to the bevelled root surface. One hundred and forty extracted single rooted human teeth were used, divided into seven groups of twenty each. ln the first, second, third and fourth groups, the teeth were apicoectomized, submitted to cavity preparations and retrofilled with one of the following materiais: zinc free silver amalgam, a dentin bonding system plus composite resin, a glass ionomer cement ora compomer. In the fifth, sixth and seventh groups, the teeth were apicoectomized and capped on the bevelled root surface with one of the following materiais: a dentin bonding system plus composite resin, a glass ionomer cement or a compomer. Two specimens of each experimental group were evaluated for the marginal adaptation using scanning electron microscopy. The remaining 126 specimens were immersed in 2% methylene blue dye, stored for one week at 37ºC and the infiltration was evaluated with a stereomicroscope. The results showed that the glass ionomer cement presented the lowest values of marginal infiltration when used as retrofilling material, with a significant statistical difference when compared with the others tested materials. When used as apical capping, the glass ionomer cement and the compomer were equivalent and significantly better than the dentin bonding system plus composite resin. Using scanning electron microscopy, all the materials showed some slight adjustment problem. ln the retrofilling, the smallest marginal gaps were observed with the compomer and the dentin bonding system plus composite resin, while the largest were observed with the glass ionomer cement and zinc free silver amalgam. ln the apical capping, the smallest marginal gaps were observed with the compomer and the dentin bonding system plus composite resin and ...

A hybrid technology for parallel recording of single ion channels

Hybrid technologies, thanks to the convergence of integrated microelectronic devices and new class of microfluidic structures could open new perspectives to the way how nanoscale events are discovered, monitored and controlled. The key point of this thesis is to evaluate the impact of such an approach into applications of ion-channel High Throughput Screening (HTS)platforms. This approach offers promising opportunities for the development of new classes of sensitive, reliable and cheap sensors. There are numerous advantages of embedding microelectronic readout structures strictly coupled to sensing elements. On the one hand the signal-to-noise-ratio is increased as a result of scaling. On the other, the readout miniaturization allows organization of sensors into arrays, increasing the capability of the platform in terms of number of acquired data, as required in the HTS approach, to improve sensing accuracy and reliabiity. However, accurate interface design is required to establish efficient communication between ionic-based and electronic-based signals. The work made in this thesis will show a first example of a complete parallel readout system with single ion channel resolution, using a compact and scalable hybrid architecture suitable to be interfaced to large array of sensors, ensuring simultaneous signal recording and smart control of the signal-to-noise ratio and bandwidth trade off. More specifically, an array of microfluidic polymer structures, hosting artificial lipid bilayers blocks where single ion channel pores are embededed, is coupled with an array of ultra-low noise current amplifiers for signal amplification and data processing. As demonstrating working example, the platform was used to acquire ultra small currents derived by single non-covalent molecular binding between alpha-hemolysin pores and beta-cyclodextrin molecules in artificial lipid membranes.

Inorganic-organic hybrid polymers: Solution-processible coating materials for defined surface functionalization

A new class of inorganic-organic hybrid polymers could successfully been prepared by the combination of different polymerization techniques. The access to a broad range of organic polymers incorporated into the hybrid polymer was realized using two independent approaches.rnIn the first approach a functional poly(silsesquioxane) (PSSQ) network was pre-formed, which was capable to initiate a controlled radical polymerization to graft organic vinyl-type monomers from the PSSQ precursor. As controlled radical polymerization techniques atom transfer radical polymerization (ATRP), as well as reversible addition fragmentation chain transfer (RAFT) polymerization could be used after defined tuning of the PSSQ precursor either toward a PSSQ macro-initiator or to a PSSQ macro-chain-transfer-agent. The polymerization pathway, consisting of polycondensation of trialkoxy-silanes followed by grafting-from polymerization of different monomers, allowed synthesis of various functional hybrid polymers. A controlled synthesis of the PSSQ precursors could successfully be performed using a microreactor setup; the molecular weight could be adjusted easily while the polydispersity index could be decreased well below 2.rnThe second approach aimed to incorporate differently derived organic polymers. As examples, polycarbonate and poly(ethylene glycol) were end-group-modified using trialkoxysilanes. After end-group-functionalization these organic polymers could be incorporated into a PSSQ network.rnThese different hybrid polymers showed extraordinary coating abilities. All polymers could be processed from solution by spin-coating or dip-coating. The high amount of reactive silanol moieties in the PSSQ part could be cross-linked after application by annealing at 130° for 1h. Not only cross-linking of the whole film was achieved, which resulted in mechanical interlocking with the substrate, also chemical bonds to metal or metal oxide surfaces were formed. All coating materials showed high stability and adhesion onto various underlying materials, reaching from metals (like steel or gold) and metal oxides (like glass) to plastics (like polycarbonate or polytetrafluoroethylene).rnAs the material and the synthetic pathway were very tolerant toward different functionalities, various functional monomers could be incorporated in the final coating material. The incorporation of N-isopropylacrylamide yielded in temperature-responsive surface coatings, whereas the incorporation of redox-active monomers allowed the preparation of semi-conductive coatings, capable to produce smooth hole-injection layers on transparent conductive electrodes used in optoelectronic devices.rnThe range of possible applications could be increased tremendously by incorporation of reactive monomers, capable to undergo fast and quantitative conversions by polymer-analogous reactions. For example, grafting active esters from a PSSQ precursor yielded a reactive surface coating after application onto numerous substrates. Just by dipping the coated substrate into a solution of a functionalized amine, the desired function could be immobilized at the interface as well as throughout the whole film. The obtained reactive surface coatings could be used as basis for different functional coatings for various applications. The conversion with specifically tuned amines yielded in surfaces with adjustable wetting behaviors, switchable wetting behaviors or as recognition element for surface-oriented bio-analytical devices. The combination of hybrid materials with orthogonal reactivities allowed for the first time the preparation of multi-reactive surfaces which could be functionalized sequentially with defined fractions of different groups at the interface. rnThe introduced concept to synthesis functional hybrid polymers unifies the main requirements on an ideal coating material. Strong adhesion on a wide range of underlying materials was achieved by secondary condensation of the PSSQ part, whereas the organic part allowed incorporation of various functionalities. Thus, a flexible platform to create functional and reactive surface coatings was achieved, which could be applied to different substrates. rn

Specific enzymatic cleavage and payload release from peptide-based hybrid nanocapsules

Within this thesis, new approaches for the concepts of peptide-polymer conjugates and peptide-based hybrid nanomaterials are investigated. In the first part, the synthesis of a triblock polymer-peptide-polymer is carried out following a typical peptide coupling reaction, both in solution and on solid-phase. The peptide sequence is chosen, so that it is cleaved by an enzyme preparation of trypsin. End-functionalized polystyrene is used as a model hydrophobic polymer and coupled to the peptide sequence. The results show successful coupling reactions in both methods, while the solid phase method produced a more defined product. Suspensions, consisting of peptide-polymer conjugates particles, are prepared in water by ultrasonication. In contact with the enzyme, the peptide constituting the conjugated particles is cleaved. This demonstrates the enzymatic cleavage in heterophase of enzymatic sequence bond to hydrophobic polymers, and is of great interest for the encapsulation and delivery of hydrophobic molecules.rnA second approach is the preparation of peptide-based hybrid nanocapsules. This is achieved by interfacial polyaddition in inverse miniemulsion with the peptide sequence functionalized with additional amino acids. A method suitable to the use of a peptide sequence for interfacial polyaddition was developed. It is shown that, the polarity of the dispersed phase influences the structures prepared, from particle-like to polymeric shell with a liquid core.rnThe peptide sequence is equipped with a FRET pair (more exactly, an internally-quenched fluorescent system) which allows the real-time monitoring of the enzymatic cleavage of the recognition site. This system shows the successful cleavage of the peptide-based nanocapsules when trypsin preparation is added to the suspensions. A water-soluble fluorescent polymer is efficiently entrapped and its possible use as marker for the capsules is highlighted. Furthermore, a small water-soluble fluorescent dye (SR-101) is successfully encapsulated and the encapsulation efficiency as a function of the functionality of the peptide and the amount of comonomer equivalent (toluene diisocyanate) is studied. The dye is encapsulated at such a high concentration, that self-quenching occurs. Thus, the release of the encapsulated dye triggered by the enzymatic cleavage of the peptide results in a fluorescence recovery of the dye. The fluorescence recovery of the FRET pair in the peptide and of the encapsulated dye correlate well.rnFinally, nanocapsules based on a hepsin-cleavable peptide sequence are prepared. Hepsin is an enzyme, which is highly upregulated in prostate cancer cells. The cleavage of the nanocapsules is investigated with healthy and “cancerous” (hepsin-expressing) cell cultures. The degradation, followed via fluorescence recovery of the FRET system, is faster for the suspensions introduced in the hepsin expressing cell cultures.rnIn summary, this work tackles the domain of responsive nanomaterials for drug delivery from a new perspective. It presents the adaptation of the miniemulsion process for hybrid peptide-based materials, and their successful use in preparing specific enzyme-responsive nanoparticles, with hydrophilic payload release properties.rn

Aggregation of hybrid molecules and film formation of colloidal monolayers

A unique characteristic of soft matter is its ability to self-assemble into larger structures. Characterizing these structures is crucial for their applications. In the first part of this work, I investigated DNA-organic hybrid material by means of Fluorescence Correlation Spectroscopy (FCS) and Fluorescence Cross-Correlation Spectroscopy (FCCS). DNA-organic hybrid materials, a novel class of hybrid materials composed of synthetic macromolecules and oligodeoxynucleotide segmenta, are mostly amphiphilic and can self-assemble into supramolecular structures in aqueous solution. A hybrid material of a fluorophore, perylenediimide (PDI), and a DNA segment (DNA-PDI) has been developed in Prof. A. Hermann’s group (University of Groningen). This novel material has the ability to form aggregates through pi-pi stacking between planar PDIs and can be traced in solution due to the fluorescence of PDI. I have determined the diffusion coefficient of DNA-PDI conjugates in aqueous solution by means of FCS. In addition, I investigated whether such DNA-PDIs form aggregates with certain structure, for instance dimers. rnOnce the DNA hybrid material self-assemble into supermolecular structures for instance into micelles, the single molecules do not necessarily stay in one specific micelle. Actually, a single molecule may enter and leave micelles constantly. The average residence time of a single molecule in a certain micelle depends on the nature of the molecule. I have chosen DNA-b-polypropylene oxide (PPO) as model molecules and investigated the residence time of DNA-b-PPO molecules in their according micelles by means of FCCS.rnBesides the DNA hybrid materials, polymeric colloids can also form ordered structures once they are brought to an air/water interface. Here, hexagonally densely packed monolayers can be generated. These monolayers can be deposited onto different surfaces as coating layers. In the second part of this work, I investigated the mechanical properties of such colloidal monolayers using micromechanical cantilevers. When a coating layer is deposited on a cantilever, it can modify the elasticity of the cantilever. This variation can be reflected either by a deflection or by a resonance frequency shift of the cantilever. In turn, detecting these changes provides information about the mechanical properties of the coating layer. rnIn the second part of this work, polymeric colloidal monolayers were coated on a cantilever and homogenous polymer films of a few hundred nanometers in thickness were generated from these colloidal monolayers by thermal annealing or organic vapor annealing. Both the film formation process and the mechanical properties of these resulting homogenous films were investigated by means of cantilever. rnElastic property changes of the coating film, for example upon absorption of organic vapors, induce a deflection of the cantilever. This effect enables a cantilever to detect target molecules, when the cantilever is coated with an active layer with specific affinity to target molecules. In the last part of this thesis, I investigated the applicability of suitably functionalized micromechanical cantilevers as sensors. In particular, glucose sensitive polymer brushes were grafted on a cantilever and the deflection of this cantilever was measured during exposure to glucose solution. rn