RESUMO Esmalte e dentina são substratos dentários simultaneamente presentes na maioria das cavidades preparadas para restaurações adesivas, mas não há estudos sobre a morfologia regional das interfaces de união em uma mesma cavidade. Adesivos autocondicionantes incorporam a smear layer na camada híbrida e, conseqüentemente, as bactérias que porventura estejam presentes nela. Recentemente surgiu um adesivo autocondicionante com propriedades antibacterianas, conferidas pela adição de MDPB ao primer, mas ainda há poucas pesquisas sobre a morfologia da interface de união produzida por este material. Este estudo teve por objetivo analisar a morfologia de interfaces de união em diferentes regiões de cavidades MOD, através de microscopia eletrônica de varredura - MEV, em casos com adesivos autocondicionantes com ou sem MDPB. Como controle, foram usados dois adesivos de frasco único, cuja morfologia está amplamente descrita na literatura. Foram preparadas dezesseis cavidades Classe II em terceiros molares humanos hígidos, que foram restauradas com Z250 e um dos seguintes sistemas adesivos, aplicados segundo instruções dos fabricantes: ABF, Clearfil SE Bond, Single Bond e Prime & Bond NT. Após vinte e quatro horas de armazenamento em água destilada a 37ºC, os dentes restaurados foram seccionados em três planos de corte e preparados para análise em MEV, segundo o protocolo descrito por Montes et al. (2001). Também foram preparadas réplicas dos espécimes em resina epóxica. A morfologia das interfaces de união apresentou diferenças dependendo da região observada e também do tipo de sistema adesivo. A presença de MDPB não alterou a morfologia da interface de união dos adesivos autocondicionantes. A morfologia das interfaces de união em esmalte revelou perfeita adaptação ao substrato para todos os produtos estudados. / ABSTRACT Enamel and dentin are dental substrates simultaneously present in most cavity preparations for bonded restorations. Yet, no study can be found regarding the regional morphology of bonding interfaces present in a same cavity. Self-etching adhesive systems incorporate the smear layer into the formed hybrid layer, and consequently bacteria that might be present. Recently a self-etching system with antibacterial properties provided by the addition of MDPB was introduced in the market, but there is still little research on the interfacial morphology obtained with this material. This study aimed at analyzing the interfacial morphology in different areas of MOD cavities prepared using adhesive systems either with or without MDPB, by means of Scanning Electron Microscopy – SEM. Two single bottle adhesive systems whose morphology is widely described in the literature were used as control groups. Sixteen class II cavities were cut in sound human molars and restores using Z250 resin composite and one of the following adhesive systems, applied strictly according to the manufacturers’ instructions: ABF, Clearfil SE Bond, Single Bond and Prime & Bond NT. After 24-hour storage in distilled water at 37ºC, the teeth were sectioned in three directions and prepared for SEM analysis according to the protocol described by Montes et al. (2001). Replicas were also obtained from each specimen using epoxy resin. The interfacial morphology showed differences depending on the observed area, and also on the adhesive system. The presence of MDPB did not alter the interfacial morphology of the bonded interfaces obtained with self-etching adhesive systems. Bonded interfaces in enamel revealed perfect adaptation for all studied materials.

No description available.

RESUMO Esmalte e dentina são substratos dentários simultaneamente presentes na maioria das cavidades preparadas para restaurações adesivas, mas não há estudos sobre a morfologia regional das interfaces de união em uma mesma cavidade. Adesivos autocondicionantes incorporam a smear layer na camada híbrida e, conseqüentemente, as bactérias que porventura estejam presentes nela. Recentemente surgiu um adesivo autocondicionante com propriedades antibacterianas, conferidas pela adição de MDPB ao primer, mas ainda há poucas pesquisas sobre a morfologia da interface de união produzida por este material. Este estudo teve por objetivo analisar a morfologia de interfaces de união em diferentes regiões de cavidades MOD, através de microscopia eletrônica de varredura - MEV, em casos com adesivos autocondicionantes com ou sem MDPB. Como controle, foram usados dois adesivos de frasco único, cuja morfologia está amplamente descrita na literatura. Foram preparadas dezesseis cavidades Classe II em terceiros molares humanos hígidos, que foram restauradas com Z250 e um dos seguintes sistemas adesivos, aplicados segundo instruções dos fabricantes: ABF, Clearfil SE Bond, Single Bond e Prime & Bond NT. Após vinte e quatro horas de armazenamento em água destilada a 37ºC, os dentes restaurados foram seccionados em três planos de corte e preparados para análise em MEV, segundo o protocolo descrito por Montes et al. (2001). Também foram preparadas réplicas dos espécimes em resina epóxica. A morfologia das interfaces de união apresentou diferenças dependendo da região observada e também do tipo de sistema adesivo. A presença de MDPB não alterou a morfologia da interface de união dos adesivos autocondicionantes. A morfologia das interfaces de união em esmalte revelou perfeita adaptação ao substrato para todos os produtos estudados. / ABSTRACT Enamel and dentin are dental substrates simultaneously present in most cavity preparations for bonded restorations. Yet, no study can be found regarding the regional morphology of bonding interfaces present in a same cavity. Self-etching adhesive systems incorporate the smear layer into the formed hybrid layer, and consequently bacteria that might be present. Recently a self-etching system with antibacterial properties provided by the addition of MDPB was introduced in the market, but there is still little research on the interfacial morphology obtained with this material. This study aimed at analyzing the interfacial morphology in different areas of MOD cavities prepared using adhesive systems either with or without MDPB, by means of Scanning Electron Microscopy – SEM. Two single bottle adhesive systems whose morphology is widely described in the literature were used as control groups. Sixteen class II cavities were cut in sound human molars and restores using Z250 resin composite and one of the following adhesive systems, applied strictly according to the manufacturers’ instructions: ABF, Clearfil SE Bond, Single Bond and Prime & Bond NT. After 24-hour storage in distilled water at 37ºC, the teeth were sectioned in three directions and prepared for SEM analysis according to the protocol described by Montes et al. (2001). Replicas were also obtained from each specimen using epoxy resin. The interfacial morphology showed differences depending on the observed area, and also on the adhesive system. The presence of MDPB did not alter the interfacial morphology of the bonded interfaces obtained with self-etching adhesive systems. Bonded interfaces in enamel revealed perfect adaptation for all studied materials.

In this dissertation, four test approaches were developed to characterize the adhesion performance and durability of adhesive bonds for specific applications in areas spanning from structural adhesive joints to popular confectionaries such as chewing gum. In the first chapter, a double cantilever beam (DCB) specimen geometry is proposed for combinatorial fracture studies of structural adhesive bonds. This specimen geometry enabled the characterization of fracture energy vs. bondline thickness trends through fewer tests than those required during a conventional "one at a time" characterization approach, potentially offering a significant reduction in characterization times. The second chapter investigates the adhesive fracture resistance and crack path selection in adhesive joints containing patterns of discreet localized weak interfaces created using physical vapor deposition of copper. In a DCB specimen tested under mode-I conditions, fracture energy within the patterned regions scaled according to a simple rule of mixture, while reverse R-curve and R-curve type trends were observed in the regions surrounding weak interface patterns. Under mixed mode conditions such that bonding surface with patterns is subjected to axial tension, fracture energy did not show R-curve type trends while it was observed that a crack could be made to avoid exceptionally weak interfaces when loaded such that bonding surface with defects is subjected to axial compression. In the third chapter, an adaptation of the probe tack test is proposed to characterize the adhesion behavior of gum cuds. This test method allowed the introduction of substrates with well-defined surface energies and topologies to study their effects on gum cud adhesion. This approach and reported insights could potentially be useful in developing chewing gum formulations that facilitate easy removal of improperly discarded gum cuds from adhering surfaces. In the fourth chapter we highlight a procedure to obtain insights into the long-term performance of silicone sealants designed for load-bearing applications such as solar panel support sealants. Using small strain constitutive tests and time-temperature-superposition principle, thermal shift factors were obtained and successfully used to characterize the creep rupture master curves for specific joint configurations, leading to insights into delayed failures corresponding to three years through experiments carried out in one month. / Ph. D.

This body of research investigated the bonding efficiency of self-etching primer adhesives to enamel and dentine with various surface characteristics. A series of preliminary experiments was carried out to determine the effect of operator experience, dentine tubule orientation, bond strength test method and resin composite material used on bond strengths. The results of the preliminary tests concluded that it is essential to develop skills in material handling and the test methods used; 2-step self-etching primer adhesives exhibit higher but more variable microshear bond strengths (µSBS) than ‘all-in-one’ adhesives on dentine at different depths and tubule orientations; fracture toughness and bond strength test results suggest that the fracture toughness of a resin composite may not be of significant influence on microtensile and µSBS tests outcomes for nano-filled hybrid materials. / An investigation of the bonding ability of self-etching primer adhesives under various tooth preparation conditions was carried out. Enamel and dentine specimens were prepared from human teeth and finished with various rotary cutting instruments and the erbium, chromium:yttrium, scandium, gallium, garnet laser. Specimens were bonded with two 2-step self-etching primer adhesives and two ‘all-in-one’ adhesives with a resin composite. The results showed that one of the 2-step adhesives exhibited higher but more variable µSBS than the ‘all-in-one’ adhesives and a silorane-based self-etching primer adhesive system to enamel and dentine. / The relationship between enamel microhardness and µSBS was evaluated. Enamel specimens were prepared and finished with one half of the surface tested for hardness using the Vickers test. The other half of the enamel surface was bonded using either a 2-step self-etching primer adhesive or an ‘all-in-one’ adhesive and a hybrid resin composite. Mean Vickers hardness numbers and µSBS for each enamel surface were calculated. Analysis using Pearson’s parametric test for regression analysis evaluated the correlation between Vickers hardness and µSBS. The results revealed a weak negative insignificant correlation between VHN and µSBS for the 2-step adhesive and no correlation for the ‘all-in-one’ adhesive. / The effect of conditioning and casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) on bonding to bleached and unbleached enamel was investigated. Four groups of enamel specimens: untreated control; bleaching with 16% carbamide peroxide gel for 90 min daily x 14 days; treated with CPP-ACP paste (Tooth Mousse, GC Corp., Japan) for 60 min daily x 7 days and bleached and CPP-ACP-treated were used. The specimens were divided into a further two groups and bonded with a total-etch adhesive or a 2-step self-etching primer adhesive. Specimens bonded with the self-etching primer adhesive were sub-divided into four conditioning subgroups before bonding: no conditioning; 30 – 40% phosphoric; 15% EDTA; 20% polyacrylic acid. Specimens were tested in shear mode until failure and analysed by 2-way ANOVA, one-way ANOVA and Tukey’s post-hoc test. The µSBS of the total-etch adhesive was not affected by enamel treatment. Bleaching reduced the µSBS of the self-etching primer adhesive but preconditioning with phosphoric acid and polyacrylic acid improved bond strengths after CPP-ACP application. Bond failure analysis revealed a predominance of adhesive failures after bleaching, but prior conditioning reduced the proportion of adhesive failures. Scanning electron microscopy (SEM) revealed that the interfacial morphology produced by the 2-step self-etching primer adhesive was independent of enamel treatment except after bleaching. Phosphoric acid etching was not inhibited by CPP-ACP treatment. Resin tag formation was observed with prior phosphoric acid and polyacrylic acid conditioning. / The effect of conditioning and CPP-ACP application on dentine bonding was also investigated. Dentine specimens with and without the smear layer were prepared and divided into a further two groups, CPP-ACP paste applied to one group for 60 min daily x 7 days and the other group was untreated. The two groups were divided into three subgroups for conditioning: no conditioning; 30 - 40% phosphoric acid; 20% polyacrylic acid. The dentine was bonded using a 2-step self-etching primer adhesive and an ‘all-in-one’ adhesive, and tested as previously described. Statistical analysis was carried out using one-way ANOVA and Tukey’s post-hoc test at α = 0.05. The results showed that the µSBS of both adhesives were not significantly affected on smear-covered dentine but was affected on smearless dentine. Conditioning did not improve bond strengths. Bond failure analysis showed more adhesive failures for the ‘all-in-one’ adhesive, particularly on smearless dentine and with prior polyacrylic acid conditioning. SEM revealed a similar morphology of the bonded interface for the 2-step self-etching primer adhesive regardless of conditioning; and areas of bond failures for the ‘all-in-one’ adhesive. / The 2-step self-etching primer adhesives exhibited higher bond strength and more regular bond integrity than the ‘all-in-one’ adhesives, as shown on the SEM observations. However, the ‘all-in-one’ adhesives exhibited less variability in bond strengths to tooth surface characteristics.

The aim of this study was to compare the in vitro microbial leakage in 4 micro-hybrid composites in combination with 4 single-component dental adhesives (Scotchbond 1/Z100 MP = group 1; Syntac Single-Component/Tetric Flow = group 3; OptiBond Solo/XRV Herculite = group 5; Solobond M/Arabesk Top = group 7) and 4 multi-component dental adhesives (Scotchbond Multi-Purpose/Z100 MP = group 2; Syntac/Tetric Flow = group 4; OptiBond FL/XRV Herculite = group 6; Solobond Plus/Arabesk Top = group 8). Ninety-four mixed standardized Class V cavities of human caries-free extracted premolars were filled with eight different composite adhesive systems using a one-layer (groups 1–4) or a two-layer technique (groups 5–8). After thermocycling and incubation in a broth culture of Streptococcus mutans and Lactobacillus acidophilus, followed by decalcification and staining, the extent and the type of microbial leakage were measured histologically. The extent of microbial leakage in the composite restorations was very low in all groups and there were no significant differences between adhesives. Z100 MP in combination with single- and multi-component adhesives showed a significantly higher microbial leakage than Tetric Flow systems (U test: p = 0.037). XRV Herculite adhesive systems showed significantly less extensive microbial leakage than Arabesk Top adhesive systems (U test: p < 0.001). The single-component dental adhesives achieved a marginal adaptation of composites comparable to that of multi-component adhesives in vitro. / Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.

Electrically conductive adhesives (ECAs) are one of the lead-free interconnect materials with the advantages of environmental friendliness, mild processing conditions, fewer processing steps, low stress on the substrates, and fine pitch interconnect capability. However, some challenging issues still exist for the currently available ECAs, including lower electrical conductivity, conductivity fatigue in reliability tests, limited current-carrying capability, poor impact strength, etc. The interfacial properties is one of the major considerations when resolving these challenges and developing high performance conductive adhesives. Surface functionalization and interface modification are the major approaches used in this thesis. Fundamental understanding and analysis of the interaction between various types of interface modifiers and ECA materials and substrates are the key for the development of high performance ECA for lead-free interconnects. The results of this thesis provide the guideline for the enhancement of interfacial properties of metal-metal and metal-polymer interactions. Systematic investigation of various types of ECAs contributes to a better understanding of materials requirements for different applications, such as surface mount technology (SMT), flip chip applications, flat panel display modules with high resolution, etc. Improvement of the electrical, thermal and reliability of different ECAs make them a potentially ideal candidate for high power and fine pitch microelectronics packaging option.

Submitted by JÚLIO HEBER SILVA (julioheber@yahoo.com.br) on 2018-05-22T17:33:36Z No. of bitstreams: 2 Tese - Andreia Assis Carvalho - 2018.pdf: 4561805 bytes, checksum: 5562226572f75d161d963c396d0c974f (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2018-05-23T11:38:00Z (GMT) No. of bitstreams: 2 Tese - Andreia Assis Carvalho - 2018.pdf: 4561805 bytes, checksum: 5562226572f75d161d963c396d0c974f (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Made available in DSpace on 2018-05-23T11:38:00Z (GMT). No. of bitstreams: 2 Tese - Andreia Assis Carvalho - 2018.pdf: 4561805 bytes, checksum: 5562226572f75d161d963c396d0c974f (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Previous issue date: 2018-04-20 / Fundação de Amparo à Pesquisa do Estado de Goiás - FAPEG / The objective of this study was to evaluate the clinical behavior of direct composite resin restorations (Class I and II), varying the universal dental adhesive application protocol, using the FDI and USPHS evaluation criteria. It was a randomized, double-blind, mouth5 divided, and sample-based randomized controlled trial. The selected participants should have a Class I and/or II restorative need for at least three dental elements or multiples of three resulting from the presence of carious lesions and/or unsatisfactory restorations. Three protocols for the application of the Single Bond Universal adhesive (3M ESPE) were tested (n=150): CAT (control) = etch-and-rinse + adhesive (n=50); CASE = selective etching in enamel + adhesive (n=50) and Ac = self-etch (n=50). The three groups were similarly restored using Filtek Z350 XT composite resin (3M ESPE) by means of the oblique incremental technique. Clinical evaluations were performed by two evaluators at the baseline (T1) and after 15.8 (±2.7 months) (T2), using the FDI and USPHS criteria. Friedman (between groups at different times), Wilcoxon (between times for each group) and McNemar (between FDI and USPHS criteria) were performed, α=0.05. The Kappa test showed excellent inter-examiner agreement (κ>0.80). For the "superficial staining" property, a statistically significant difference was observed in T2 between the CAT and CASE groups (p=0.01) with higher values for CAT and, when T1 and T2 were compared for each group, there were differences in the CAT group (p=0.001) and in the Ac group (p=0.007) for T2. For the other comparisons between groups and times there were no statistically significant differences, even when the FDI and USPHS criteria were compared (p≥0.05). It can be concluded that the different protocols of universal adhesive application (CAT, CASE and Ac) did not influence the clinical behavior of the restorations evaluated in 15.8 months of evaluation. The FDI and USPHS criteria provided comparable results. / Esse trabalho objetivou avaliar o comportamento clínico de restaurações diretas de resina composta (Classe I e II), variando o protocolo de aplicação do adesivo dentário universal, por meio dos critérios de avaliação FDI e USPHS. Trata-se de um ensaio clínico contrlado randomizado, duplo-cego, boca-dividida e de amostra por conveniência. Os participantes selecionados deveriam ter necessidade restauradora de Classe I e/ou II no mínimo em três elementos dentários ou múltiplos de três, resultantes da presença de lesões cariosas e/ou restaurações insatisfatórias. Três protocolos de aplicação do adesivo Single Bond Universal (3M ESPE) foram testados (n=150): CAT (controle) = Condicionamento ácido total + adesivo (n=50); CASE = Condicionamento ácido seletivo em esmalte + adesivo (n=50) e Ac = autocondicionante (n=50). Os três grupos foram restaurados de forma similar utilizando resina composta Filtek Z350 XT (3M ESPE) por meio da técnica incremental oblíqua. As avaliações clínicas foram realizadas por dois avaliadores no baseline (T1) e após 15,8 (±2,7 meses) (T2), por meio dos critérios FDI e USPHS. Foram realizados os testes Friedman (entre os grupos nos diferentes tempos), Wilcoxon (entre os tempos para cada grupo) e McNemar (entre os critérios FDI e USPHS), α=0,05. O teste Kappa apresentou excelente concordância interexaminadores (κ>0,80). Para a propriedade “manchamento superficial”, observou-se diferença estatisticamente significante no T2 entre os grupos CAT e CASE (p=0,01) com maiores valores para CAT e, quando comparados T1 e T2 para cada grupo, houve diferença no grupo CAT (p=0,001) e no grupo Ac (p=0,007) para T2. Para as demais comparações entre os grupos e tempos não houve diferenças estatisticamente significantes, inclusive quando os critérios FDI e USPHS foram comparados (p≥0,05). Pode-se concluir que os diferentes protocolos de aplicação do adesivo universal (CAT, CASE e Ac) não influenciaram o comportamento clínico das restaurações avaliadas em 15,8 meses de avaliação. Os critérios FDI e USPHS proporcionaram resultados comparáveis entre si.

La démocratisation des technologies du collage dans le domaine aérospatial amène les industriels à exiger des adhésifs toujours plus performants. L’objectif de cette thèse est d’optimiser les propriétés thermomécaniques d’un adhésif polyépoxyde bi-composant qui devra présenter des propriétés structurales entre -150°C et +150°C, tout en respectant des exigences de mise en oeuvre.L’analyse de la littérature et des expériences préliminaires a permis de sélectionner le système polyépoxyde modèle binaire le plus pertinent en termes de réactivité à l’ambiante et de propriétés sur assemblage collé. Pour optimiser la résistance en température élevée de ce système, deux voies ont été explorées : l’incorporation d’époxydes multi-fonctionnalisés pour augmenter la densité de réticulation, et l’utilisation d’amines cycliques qui accroit la rigidité des segments macromoléculaires. Pour améliorer les propriétés de résistance à la propagation de fissure à basse température, les additifs de renforcement montrent un intérêt certain pour la formulation d’adhésifs structuraux polymérisés à température ambiante. Sur la base de ces résultats, plusieurs formulations complexes ont pu être élaborées. Des phénomènes de synergie et d’inhibition entre les différents éléments des formulations ont été constatés, sans pouvoir être totalement compris ce qui met en lumière la difficulté de prévoir le comportement d’adhésifs complexes, à l’image des formulations commerciales.Ces travaux de thèse ont permis de développer un adhésif structural répondant aux exigences strictes du secteur aérospatial, et de dégager une stratégie de formulation qui pourra être appliquée à d’autres secteurs d’activités. / The democratisation of bonding technologies in aerospace field leads industrials to demand more and more efficient adhesives. The aim of this thesis is to optimise thermomechanical properties of two-component epoxy adhesives which need to preserve structural properties on a large scale of temperature (from -150°C to +150°C) and observing application process requirements.The analysis of scientific literature and preliminary experiments enable to select the most relevant binary epoxy system in terms of reactivity and bonding mechanical properties. To optimise high temperature resistance of this epoxy system, two approaches have been explored: addition of multi-functionalised epoxy resin to extend the crosslink density, and use of cycloaliphatic amines which increase the rigidity of macromolecular segments. To improve crack propagation resistance in low temperature, tougheners reveal an interest to formulate room temperature structural adhesives. On the basis of these results, complex formulations have been developed. Synergy and inhibition phenomenon between the formulation blends have been observed without being able to fully understand them which highlight the difficulty to predict the behaviour of complex adhesives such as commercial formulations.This thesis works allowed to develop a two-component epoxy adhesive formulation which meets aerospace requirements, and to bring about a formulation strategy which could be adapted to others sectors activities.

The aim of this study was to compare the in vitro microbial leakage in 4 micro-hybrid composites in combination with 4 single-component dental adhesives (Scotchbond 1/Z100 MP = group 1; Syntac Single-Component/Tetric Flow = group 3; OptiBond Solo/XRV Herculite = group 5; Solobond M/Arabesk Top = group 7) and 4 multi-component dental adhesives (Scotchbond Multi-Purpose/Z100 MP = group 2; Syntac/Tetric Flow = group 4; OptiBond FL/XRV Herculite = group 6; Solobond Plus/Arabesk Top = group 8). Ninety-four mixed standardized Class V cavities of human caries-free extracted premolars were filled with eight different composite adhesive systems using a one-layer (groups 1–4) or a two-layer technique (groups 5–8). After thermocycling and incubation in a broth culture of Streptococcus mutans and Lactobacillus acidophilus, followed by decalcification and staining, the extent and the type of microbial leakage were measured histologically. The extent of microbial leakage in the composite restorations was very low in all groups and there were no significant differences between adhesives. Z100 MP in combination with single- and multi-component adhesives showed a significantly higher microbial leakage than Tetric Flow systems (U test: p = 0.037). XRV Herculite adhesive systems showed significantly less extensive microbial leakage than Arabesk Top adhesive systems (U test: p < 0.001). The single-component dental adhesives achieved a marginal adaptation of composites comparable to that of multi-component adhesives in vitro. / Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.