Thesis (MEng)--Stellenbosch University, 2014. / ENGLISH ABSTRACT: Flexible pavement designers have a choice of two wearing course: either asphalt concrete or surfacing seals. The latter have been widely used by several countries as their preferred wearing course over other methods, especially countries with a limited number of average inhabitants per square kilometre. Moreover, the surfacing seals were identified as an efficient cost effective road preventive maintenance technique. Surfacing seals in New Zealand, South Africa and Australia cover about 65%, 80% and 90% of their surfaced road networks respectively. The preference of surfacing seals is due to their competitive initial cost and ease of construction. In South Africa, the life expectancy of surfacing seals varies between 8 and 12 years with an average of 10 years. This has not been the case in a number of surfacing seals constructed in winter, especially when the night recorded temperature is below 10oC. The dominant failure mechanism is ravelling (chip loss) soon after construction due to traffic loading. This chip loss is linked to the poor adhesion bond development rate in the bitumen-aggregate system during winter adverse conditions. In order to address the issue of premature chip loss the need for the development of a robust adhesion test method was identified. For that purpose, recently, researchers in the bitumen industry developed the Bitumen Bond Strength test method. This method was used in this study. This study intends to contribute to the understanding of binder-aggregate adhesion bond development for winter surfacing seals using the BBS test. Binder type, precoat type and conditioning, aggregate type and curing time are amongst the factors influencing winter seals adhesion bond performance. An experimental matrix involving three types of binder, two types of aggregate, four different precoating fluids, two precoat conditionings and two binder-curing times were then developed and investigated. Winter weather parameters affecting adhesion properties were also taken into consideration during the course of the investigation. Throughout the test, the procedure described in AASHTO TP 91-11 was followed. However, in order to enhance the control of the binder application temperature, a new method for hot applied binder sample preparation was developed as part of this study. The findings show that there is a significant difference between adhesion properties of the hot applied binders (70/100 and S-E1) and the emulsion (SC-E1). In most of the cases, the hot applied binders performed better than the emulsion. The failure mode observed was found to be linked to the condition of the precoating. The influence of the precoat type and conditioning, and effect of binder curing time were significantly highlighted. The use of a dry precoat benefited the adhesion bond strength up to around 50% relatively to the corresponding non-precoated combination. However, a decrement in the bond strength due to precoating of up to 28.7% was also observed. A statistical analysis using ANOVA did not illustrate any statistical significant effect of the aggregate type. The interaction effects analysis using ANOVA revealed the aggregate type interacting with precoat type to be the most influential interaction at level two. The precoat conditioning implication to the adhesion development rate, which influences the time for opening to traffic after construction, was illustrated. Insightful aspects on the compatibility between the binder type and precoat type and conditioning during the aggregate precoating practices and on the time for opening to traffic are highlighted. Finally, the repeatability analysis proved the BBS test to be a repeatable testing method with caution. Recommendations for further studies that could support the conclusions drawn in this study were provided. / AFRIKAANSE OPSOMMING: Buigbare plaveiselontwerpers het 'n keuse van twee deklae: óf Asfalt of oppervlak seëls. Laasgenoemde word algemeen gebruik deur verskeie lande as hul voorkeur deklaag, veral die lande met beperkte aantal gemiddelde inwoners per vierkante kilometer. Verder, is die seëls geïdentifiseer as 'n doeltreffende koste-effektiewe deklaag tegniek. Oppervlakseëls in Nieu-Seeland, Suid-Afrika en Australië dek ongeveer 65%, 80% en 90% van hul padnetwerke onderskeidelik. Die seëls se voorkeur is te danke aan hul mededingende aanvanklike koste en eenvoudige vorm van die konstruksie. In Suid-Afrika wissel die seël se lewensverwagting tussen 8 en 12 jaar met 'n gemiddeld van 10 jaar. Dit is egter nie die geval van 'n aantal seëls wat in die winter gebou word nie, veral wanneer die aangetekende nagtemperatuur onder 10o C daal nie. Die dominante swigtingsmeganisme is stroping (klipverlies) kort na konstruksie. Hierdie klipverlies is gekoppel aan die power kleef-ontwikkeling van bitumen gedurende die winter. Ten einde die probleem van voortydige klipverlies aan te spreek het die behoefte vir die ontwikkeling van 'n robuuste toetsmetode ontstaan. Om hierdie rede het navorsers onlangs in die bitumenbedryf die “BBS toetsmetode” ontwikkel en is dié toetsmetode in hierdie studie gebruik. Hierdie studie beoog om by te dra tot die begrip van bindmiddel-klip kleefontwikkeling vir die winter seëls dmv die BBS toets. Die faktore, insluitend maar nie beperk tot bindmiddeltipe, voorafdekking (“PRECOAT”) -tipe en kondisionering, aggregaattipe en kuurtyd beïnvloed winter seëls se kleefeienskappe. 'n Eksperimentele matriks met drie tipes bindmiddels, twee tipes aggregate, vier verskillende voorafdekking-vloeistowwe, twee voorafdekking kondisionering en twee bindmiddel kuurtye is toe ontwikkel en ondersoek. Winter weer parameters wat kleefeienskappe beïnvloed is ook in ag geneem tydens die verloop van die ondersoek. Regdeur die studie is die prosedure AASHTO TP 91-11 gevolg, maar ten einde die beheer van die bindmiddel spuittemperatuur te verbeter, is ‘n nuwe metode vir warmspuit-bindmonsters voorbereiding ontwikkel as deel van hierdie studie. Die bevindinge toon dat daar 'n beduidende verskil tussen die kleefeienskappe van die warm aangewende bindmiddels (70/100 en S-E1) en die emulsie (SC-E1) is. In die meeste van die gevalle het die warmspuit-bindmiddels beter as emulsie gevaar. Daar is gevind dat die swigtingsmeganisme verbind word met die toestand van die voorafdekking. Die invloed van voorafdekkingtipe, kondisionering, en die effek van bindmiddelkuurtyd is duidelik uitgelig. Die gebruik van droë voorafdekking het die kleefkrag tot sowat 50% verhoog relatief tot die ooreenstemmende onbedekte klipkombinasie. Daar is egter ook ‘n verlaging van die kleefkrag weens voorafdekking gevind van tot so hoog soos 28,7 persent. Die statistiese ontleding met behulp van ANOVA het geen statisties beduidende effek van die verksillende aggregaattipe te vore gebring nie. Die interaksie-effek analise, met behulp van ANOVA, het wel die interaksie met voorafdekkingtipe met aggregaat die mees invloedryke bevestig. Die voorafdekking kondisioneering het ver rykende kleefkrag implikasies bloot gelê, wat die tyd vir die opening van die verkeer na konstruksie beïnvloed. Insigwekkende aspekte oor die versoenbaarheid tussen die bindmiddeltipe, voorafdekkingtipe, kondisionering, voorafdekkingpraktyk en tyd tot opening vir verkeer word uitgelig. Ten slotte, die herhaalbaarheidsanalise het die BBS toets as 'n herhaalbare toetsmetode met omsigtigheid bewys. Daar is aanbevelings tot verdere studies, wat uit die gevolgtrekking gekom het, gemaak.

Les systèmes d’ancrages adhésifs sont utilisés dans plusieurs applications en génie civil, notamment en réhabilitation et réparation des ouvrages d’infrastructure tels que des dalles de ponts, chaussées, tunnels, barrages, murs, poteaux, ainsi que dans certains travaux d’exploration géologique et minière. Un système d’ancrage adhésif comprend trois composants : l’élément d’ancrage : une barre d’armature ou une tige filetée ; le matériau adhésif : polymérique, cimentaire ou hybride ; et le substrat : en béton ou en maçonnerie. Les charges imposées sur les barres d’ancrage sont transmises au substrat par adhérence chimique (réactions) et liaison mécanique (interlock) entre les composants mentionnés. Le modèle de design d’adhérence uniforme établit que la performance structurale d’un système d’ancrage adhésif est déterminée par la contrainte de l’adhérence (τ), développée sur toute la surface de contact, entre les composants à l’intérieur du trou d’ancrage. Ce projet, en partenariat avec l’entreprise AMBEX, étudie et évalue la performance des systèmes d’ancrage avec adhésifs en matériau cimentaire, par rapport au comportement sous chargement continu. Pour ce faire, on a ancré des barres d’armature dans un substrat en béton conventionnel. Les deux adhésifs étudiés sont les cartouches d’ancrage AAC et ARC. On a tenu compte des paramètres géométriques et d’installation en assurant la rupture de l’adhérence lors des essais d’arrachement. On a évalué deux conditions en service: température ambiante (21ºC) et élevée (43ºC). On a effectué des essais statiques de traction et des essais sous chargement soutenu. Les résultats sont présentés dans des graphiques « chargedéplacement-temps », afin d’établir des prédictions futures de comportement. Le projet montre les avantages des ancrages adhésifs en matériau cimentaire, tels que le taux de fluage très faible sous chargement soutenu, et quelques limitations aussi, comme la variabilité des résultats à l’arrachement pour les ancrages avec la cartouche AAC. / Abstract : Adhesive anchoring systems are used in many civil engineering applications, including rehabilitation and repair of infrastructure such as bridge decks, roadways, tunnels, dams, walls, columns, and in some geological explorations and mining. An adhesive anchoring system consists of three components: the anchor: a reinforcing bar or a threaded rod; the adhesive material: polymeric, cementitious or hybrid; and a substrate of concrete or masonry. The loads applied on the anchor rods are transmitted by a chemical adhesion to the substrate (reactions) and mechanical interlock between the components mentioned. The design pattern of uniform adhesion establishes that the structural performance of an adhesive anchoring system is determined by the bond strength (τ) developed across the contact surface, between the components within the anchor hole. This project, in partnership with AMBEX, investigates and assesses the performance of an anchoring system, with an adhesive of cementitious material, related to the creep behaviour. To achieve this, steel rebars were anchored in a conventional concrete substrate. Two adhesives were evaluated: AAC and ARC cartridges. Geometrical and installation parameters were taken into account, to ensure bond failure during pullout tests. Two service conditions were studied: room temperature (21ºC) and high temperature (43ºC). Static tensile tests and creep tests were performed. The results are presented in graphs “load-displacement-time”, in order to make predictions of future behavior. The project shows the advantages of adhesive anchors made of cementitious material, as a feeble creep rate at sustained load, and also some limitations, as the variability of tension test results for anchors tested with AAC cartridge.

As lesões cervicais não cariosas (LCNCs) são definidas pela perda de estrutura dental na junção cemento/esmalte que envolve três mecanismos de estresse mecânico (tensão), atrito (fricção) e erosão (degradação química).. Existem tratamentos preventivos e dessensibilizantes para o principal sintoma das LCNCs, a hipersensibilidade dentinária cervical (HDC), porém, em casos que há perda de estrutura dental maior que 1mm é necessário realizar uma intervenção restauradora. Dessa forma, o objetivo deste estudo foi avaliar a resistência de união da dentina erodida e abrasionada modificada com diferentes pré-tratamentos e posteriormente restauradas com resina composta, através do teste de microtração. Para tanto, foram selecionados 40 molares humanos íntegros, que tiveram as porções oclusais seccionadas até exposição da dentina. Os espécimes passaram por desafio erosivo e abrasivo em uma ciclagem de 5 dias. Após os desafios, os espécimes receberam os tratamentos de superfície (n=10): G1: controle sem tratamento; G2: tratamento de superfície com ponta diamantada; G3: jateamento com óxido de alumínio, G4: ciclagem com enxaguatório fluoretado Elmex Erosion. Feito isso os espécimes foram restaurados, seccionados em palitos e submetidos ao teste de microtração em uma máquina universal de ensaios a 0,5mm/min. Para a analise estatística, foi utilizado o teste paramétrico de análise de variância (ANOVA) um fator e o teste auxiliar de Tukey. Foi observado que não houve diferença entre os tratamentos com ponta diamantada, óxido de alumínio e enxaguatório fluoretado. O único grupo a se diferenciar dos demais foi o grupo controle que apresentou valores de resistência de união inferiores. Dentro das limitações de um trabalho in vitro, conclui-se que os tratamentos de superfície estudados são procedimentos indicados para melhorar a adesão dental frente à necessidade de restaurar uma LCNC. / Non-carious cervical lesions (NCCLs) are defined by loss of dental structure at the cement/enamel junction involving three mechanisms of mechanical stress (tension), friction and erosion (chemical degradation). There are preventive and desensitizing treatments for the the main symptom of NCCLs, cervical dentin hypersensitivity (CDH), but in cases where there is loss of tooth structure greater than 1mm, a restorative intervention is necessary. Thus, the objective of this study was to evaluate the bond strength of the eroded and abraded dentin modified with different pre-treatments and later restored with composite resin, through the microtensile test. For this, 40 sound human molars were selected, which had the occlusal portions sectioned until exposure of the dentin. The specimens underwent erosive and abrasive challenge in a 5-day cycling. After the challenges, the specimens received the surface treatments (n = 10): G1: control without treatment; G2: surface treatment with diamond tip; G3: sandblasting with aluminum oxide, G4: cycling with fluoridated rinse Elmex Erosion. After this, the specimens were restored, sectioned on sticks and subjected to the microtensile test in a universal test machine at 0.5mm/min. For statistical analysis, the parametric analysis of variance (ANOVA) one factor and the Tukey auxiliary test were used. It was observed that there was no difference between treatments with diamond tip, aluminum oxide and fluoride. The only group to differentiate from the others was the control group that presented inferior bond strength values. Within the limitations of an in vitro work, it is concluded that the surface treatments studied are procedures indicated to improve dental adhesion in view of the need to restore NCCL.

Buscou-se minimizar ou prevenir a degradação das fibrilas colágenas, tanto no controle da progressão do desgaste erosivo em dentina, quanto na preservação das interfaces adesivas aí estabelecidas, por meio do uso de agentes antiproteolíticos (clorexidina/CHX e epigalocatequina-3-galato/EGCG) ou, ao mesmo tempo, promotores de ligações cruzadas entre elas (proantocianidina/PAC). O papel de algumas dessas estratégias no estabelecimento, e conservação, de interfaces adesivas em dentina erodida, substrato adverso à interação com materiais adesivos, tem sido, porém, pouquíssimas vezes reportado. Este estudo in vitro propôs-se a avaliar, pois, o efeito de tais agentes, usados como estratégias para prevenção/controle do desgaste, na resistência de união (RU) do conjunto sistema adesivo condicione e lave simplificado-resina composta à dentina erodida, comparada à normal. A dentina superficial oclusal de terceiros molares foi apenas submetida à ação de uma lixa de SiC (granulação 600; 1 min; N: substrato normal) ou sequencialmente a desafio erosivo inicial (Coca-Cola®; 5 min). Recebeu, então, ou não (C: controle/sem aplicação), a aplicação de um dos géis com os seguintes princípios ativos - P: placebo/sem princípio ativo; CHX: digluconato de clorexidina a 0,12%; EGCG: epigalocatequina-3-galato a 400 ?m; PAC: proantocianidina a 10%. Aquela de início desmineralizada ainda foi submetida a ciclagem de pH (Coca-Cola®; imersões de 5 min, 3x/dia, 5 dias; E: substrato erodido). Após condicionamento (H3PO4 a 37%; 15 s; lavagem 30 s; secagem com papel absorvente), o adesivo AdperTM Single Bond 2® foi aplicado em todos os espécimes e a porção coronária, reconstruída com a resina FiltekTM Z350®. Transcorridas 24 h (água destilada/37?C), os espécimes foram seccionados em palitos e testados (?TBS; 0,5 mm/min). As superfícies fraturadas de cada palito foram avaliadas utilizando-se um microscópio digital (50x de aumento). Os valores de RU obtidos foram organizados considerando- se cada dente como unidade experimental e os testes de Análise de Variância a 2 critérios e de Tukey aplicados (?=0,05). Um dente extra para cada grupo foi tratado exatamente como os outros, mas o corante fluorescente rodamina B foi previamente adicionado (0,16 mg/mL) ao sistema adesivo para permitir a avaliação qualitativa da interface adesiva por meio de Microscopia Confocal de Varredura a Laser. Analisando-se os dados obtidos pôde-se observar que, diferentemente da variável aplicação de géis para prevenção/controle do desgaste erosivo (p=0,076), a variável condição do substrato dentinário exerceu influência significante sobre os resultados (p<0,001). Ademais, não houve interação entre elas (p=0,979). Os valores imediatos de RU ao substrato erodido foram, pois, sempre inferiores que aqueles ao substrato normal, independentemente da aplicação, ou não, de qualquer um dos géis para prevenção/controle do desgaste erosivo. Quanto ao padrão de fratura dos palitos testados, as falhas adesivas e mistas foram predominantes em relação às coesivas, independentemente se em dentina ou em resina. Menores porcentagens de falhas coesivas ainda puderam ser verificadas para o substrato erodido, com relação ao normal. No que se refere à análise qualitativa, observou-se, para o erodido, comparado ao normal, independetemente do tratamento para controle do desgaste, camada escura subjacente à de adesivo propriamente, representação da menor concentração de material marcado por rodamina B, bem como tags resinosos com maior comprimento e em maior quantidade. Assim sendo, conclui-se, por ora, que as estratégias estudadas não foram capazes de favorecer, tampouco de prejudicar, o estabelecimento de interface adesiva em dentina erodida. / In order to minimize the degradation of collagen fibrils, both to control the progression of the dentin erosive wear and to preserve adhesive interfaces established there, antiproteolytic (chlorhexidine/CHX and epigallocatechin-3-gallate/EGCG) or, at the same time, collagen cross-linking agents (grape seed proanthocyanidin extract/PAC) started to be successfully used. Some of these strategies in the establishment and preservation of adhesive interfaces on eroded dentin, a substrate adverse to the interaction with adhesive materials, has been seldom reported yet. This in vitro study aimed to evaluate, thus, the effect of such agents, used as strategies for wear preventing/controlling, on bond strength (BS) of a simplified etch-and-rinse adhesive system adhesive plus a resin composite to eroded, and normal (parameter for comparisons) dentin. Superficial occlusal dentin of third molars was only ground with a SiC paper (600-grit; 1 min; N: normal substrate), or subsequently submitted to an initial erosive challenge (Coca-Cola®; 5 min). It, then, received or not (C: control/without application), application of one of the gels with the following active principles - P: placebo/without active principle; CHX: 0.012% chlorhexidine digluconate; EGCG: epigallocatechin-3-gallate at 400 ?m; PAC: 10% proanthocyanidin. Initial demineralized dentin was still submitted to a pH cycling (Coca-Cola®, 5 min immersions, 3x/day, 5 days, E: eroded substrate). After acid-etched (37% H3PO4; 15 sec; 30 sec washing; drying with absorbent paper), the adhesive Adper(TM) Single Bond 2® was applied in all specimens and resin composite buildups were constructed with Filtek(TM)Z350®. After 24 h (distilled water/37?C), specimens were sectioned in beams and tested (?TBS; 0.5 mm/min). Obtained BS values were organized considering each tooth as an experimental unit and two-way ANOVA and Tukey tests were applied (?=0.05). An extra tooth for each group was treated just like the others, but the adhesive system was marked by the addition of rhodamine B (0.16 mg/mL) to allow qualitative evaluation of the adhesive interface by means of Confocal Laser Scanning Microscopy. As opposed to the variable application of gels for wear preventing/controlling (p=0.076), the condition of the dentin substrate had a significant influence on the results (p<0.001). In addition, there was no interaction between them (p=0.979). Immediate BS values to the eroded substrate were always lower than that to the normal substrate, regardless of the application or not of any of the gels for wear preventing/controlling. As for the fracture pattern of the tested beams, adhesive and mixed failures were predominant in relation to the cohesive failures, regardless of whether in dentin or in resin. Lower percentages of cohesive failures could still be verified for the eroded substrate, relative to the normal one. Concerning the qualitative analysis, it was observed, for the eroded substrate, compared to the normal, independently of the treatment for wear preventing/controlling, a dark layer underlying that of the adhesive itself, which represents a lower concentration of rhodamine B-labeled material, as well as resinous tags with greater length and in greater quantity. Therefore, studied strategies were not able either to improve, neither to impair, the establishment of adhesive interface on eroded dentin.

O estabelecimento de interfaces adesivas no substrato dentinário artificialmente erodido, conceitualmente pobre em minerais, revestido por matriz orgânica exposta, é pouco promissor. Por ora, tornam-no similar àquele verificado para a dentina normal/hígida apenas a asperização ou, quando do uso de adesivos universais, a desproteinização com hipoclorito de sódio. Manter a camada de fibrilas colágenas, por meio do uso de inibidores de proteinases, talvez mesmo que compactada por abrasão, pode, porém, ser conveniente, já que desempenha importante papel nos processos de des e remineralização, inclusive contendo a progressão do desgaste erosivo e erosivo-abrasivo, e no estabelecimento de uma camada híbrida propriamente dita. Avaliou-se, pois, de imediato, a resistência de união do conjunto sistema adesivo condicione e lave simplificado-resina composta à dentina, considerando-se como fatores experimentais a condição desse substrato, em três níveis (N: normal; E: erodido; EA: erodido-abrasionado), e a aplicação de um gel para prevenção/controle do desgaste erosivo em três níveis (C: controle/sem aplicação; P: placebo/sem princípio ativo; CHX: digluconato de clorexidina a 0,12%). Para determinação do substrato normal, a dentina superficial oclusal de terceiros molares foi apenas submetida à ação de uma lixa de SiC (#600; 1 min; N); para a do erodido e do erodidoabrasionado, sequencialmente, de pronto, a desafio erosivo inicial (Coca-Cola®; 5 min). Aplicou-se sobre ela, então, ou não (controle/sem aplicação), um dos géis: placebo/sem princípio ativo; ou à base de CHX a 0,12%. Aquela de início desmineralizada ainda foi submetida à ciclagem de pH (Coca-Cola®; imersões de 5 min, 3x/dia, 5 dias), determinando-se, fatidicamente, o substrato erodido (E), ou a ciclagem de pH associada a escovação (escova elétrica/dentifrício com flúor diluído em água, 2,5 N, 30 s, 2x/dia, após 1º e último desafios ácidos), determinando-se o substrato erodido-abrasionado (EA). Após condicionamento (H3PO4 a 37%; 15 s; lavagem 30 s; secagem com papel absorvente), o adesivo AdperTM Single Bond 2® foi aplicado em todos os espécimes e a porção coronária, reconstruída com a resina FiltekTM Z350®. Transcorridas 24 h (água destilada / 37?C), os espécimes foram seccionados em palitos e testados (?TBS; 0,5 mm/min). Os valores de RU obtidos foram organizados considerando-se cada dente como unidade experimental e os testes de Análise de Variância a 2 critérios e de Tukey, aplicados (?=0,05). Um dente extra para cada grupo foi tratado exatamente como os outros, mas o corante fluorescente rodamina B foi previamente adicionado (0,16 mg/mL) ao sistema adesivo para permitir a avaliação qualitativa da interface adesiva por meio de Microscopia Confocal de Varredura a Laser. Diferentemente da variável aplicação de géis para prevenção/controle do desgaste erosivo (p=0,359), a variável condição do substrato dentinário exerceu influência significante sobre os resultados (p<0,001). Ademais, não houve interação entre elas (p=0,856). Os valores imediatos de RU ao substrato erodido e ao erodido-abrasionado, equivalentes entre si, foram sempre inferiores àqueles ao substrato normal, independentemente da aplicação, ou não, do gel de CHX, ou placebo, para prevenção/controle do desgaste erosivo. No tocante ao padrão de fratura dos palitos testados, as falhas adesivas e mistas foram predominantes em relação às coesivas, independentemente se em dentina ou em resina. Quanto à análise qualitativa, nota-se que tags resinosos se manifestam em maior número e comprimento nos substratos submetidos a desafio erosivo inicial, ou seja, o erodido e o erodido-abrasionado, independentemente da aplicação de qualquer estratégia para controle da progressão do desgaste. Dentre eles, para o substrato erodido, há uma identificável camada escura subjacente à de adesivo propriamente dito, entre os tags resinosos, representação da menor concentração de material marcado por rodamina B. Para o substrato erodido-abrasionado, verifica-se camada híbrida devidamente expressa por anuviado vermelho subjacente à camada de adesivo, mais e menos espessa, respectivamente, que a estabelecida no substrato normal e erodido. Destarte, conclui-se que o gel de CHX não foi capaz de determinar, por meio da preservação/controle do desgaste erosivo, ou erosivo-abrasivo, substrato tão favorável à adesão com os materiais resinosos quanto o normal, mesmo que não o tenha desajudado ainda mais. / The establishment of adhesive interfaces on artificially eroded dentin substrate, conceptually poor in minerals, coated with an exposed organic matrix, is little promising. For the time being, only diamond bur surface roughening and deproteinization with sodium hypochlorite, when universal adhesives are used, make it similar to the obtained for normal/sound dentin. Maintaining the layer of collagen fibrils, using protease inhibitors, perhaps even when compressed by abrasion, may, however, be convenient, since it plays an important role in the demineralization and remineralization processes, including the erosive and erosive-abrasive wear progression, and in establishing a hybrid layer itself. The aim of this study was to evaluate, immediately, bond strength (BS) of an etch-and-rinse adhesive system plus a composite to dentin, considering the condition of its substrate in three levels (N: normal; E: eroded; EA: eroded-abraded), and the application of a gel for the prevention/control of the erosive wear in three levels (C: control / without application, P: placebo / without an active principle, and CHX: 0.12% chlorhexidine digluconate). To determine the normal substrate, occlusal dentin from third molars was subjected solely to the action of a SiC sandpaper (# 600; 1 min; N); to determine the eroded and eroded-abraded, it was sequentially, and readily, subjected to an initial erosive challenge (Coca-Cola®, 5 min). One of the gels were applied, or not (control / without application), on it: placebo / without active principle; or containing 0.12% CHX. The initial demineralized one was still submitted to a pH cycling (Coca-Cola®, immersions of 5 min, 3x /day, 5 days), determining the eroded substrate (E), or to the pH cycling associated to brushing (electric toothbrush/fluoride toothpaste diluted in water, 2.5 N, 30 s, 2x/day, after 1st and last acid challenges), determining the eroded-abraded substrate (EA). After acid-etching (37% H3PO4, 15 sec, 30 sec washing, drying with absorbent paper), Adper(TM) Single Bond 2® adhesive was applied to all specimens and resin composite buildups constructed with Filtek(TM)Z350®. After 24 h (distilled water / 37?C), specimens were sectioned in beams and tested (?TBS, 0.5 mm/min). BS values obtained were organized considering each tooth as an experimental unit and a twoway ANOVA and Tukey test, applied (?=0.05). An extra tooth for each group was treated exactly like the others, but rhodamine B fluorescent dye was previously added (0.16 mg / mL) to the adhesive system to allow qualitative evaluation of the adhesive interface by means of Confocal Laser Scanning Microscopy. Differently from the variable application of gels for prevention/control of erosive wear (p=0.359), the condition of the dentin substrate had a significant influence on the results (p<0.001). In addition, there was no interaction between them (p=0.856). Immediate BS values to eroded and eroded-abraded substrates, equivalent to each other, were always lower than that to the sound substrate, regardless of the application, or not, of the CHX or the placebo gel for prevention/control of erosive wear. Concerning the fracture pattern of the tested beams, adhesive and mixed failures were predominant in relation to the cohesive, regardless of whether in dentin or in resin composite. As for the qualitative analysis, it is noticed that resinous tags are manifested in greater number and length in the substrates submitted to erosive initial challenge, that is, eroded and erodedabraded substrates, regardless of the application of any strategy to control progression of wear. Among them, for the eroded substrate, there is an identifiable dark layer underlying that of the adhesive itself, among the resin tags, representing the lowest concentration of material marked by rhodamine B. For the eroded-abraded substrate, hybrid layer is duly expressed by a red blur underlying the layer of adhesive, more and less thick than that established in the normal and eroded substrates, respectively. Therefore, it is concluded that the CHX gel was not able to determine, while preserving/controlling the erosive or erosive-abrasive wear, a substrate as favorable to bonding with resinous materials as a sound one, even if it has not impaired it even more.

Le principe de la projection dynamique par gaz froid ou « cold spray » repose sur la projection de particules de poudres convoyées par un gaz à des vitesses supersoniques vers un substrat. La déformation des particules à l’impact avec ce dernier permet la construction d’un dépôt. Ce procédé permet de conserver la microstructure des particules de poudre et de produire des dépôts peu poreux. Cette dernière caractéristique est essentielle dans le cadre d’applications anticorrosion. L’ambition de la thèse est de comprendre le rôle de la microstructure sur les mécanismes de corrosion marine d’un dépôt à base d’aluminium élaboré par cold spray. Pour atteindre cet objectif sont projetées des poudres à base d’aluminium (aluminium pur, alliages d’aluminium et mélanges avec ajout d’alumine) sur un substrat en acier. Les microstructures des dépôts sont étudiées jusqu’à l’échelle nanométrique (MET). L’adhérence des dépôts est mesurée par l’essai de plot collé. A partir des microstructures sont proposés plusieurs mécanismes de formation de la porosité dans un dépôt cold spray à différentes échelles. Une étude numérique par éléments finis complète cette analyse microstructurale. Grâce aux mesures de la vitesse (DPV-2000) et de la température (caméra thermique) d’impact des particules, les paramètres de nouveaux modèles matériau sont optimisés pour simuler le comportement de l’aluminium et de l’alumine à l’impact. De plus, plusieurs essais de corrosion marine (immersion et brouillard salin) sont conduits. L’étude des microstructures corrodées permettent d’établir différents mécanismes de corrosion du dépôt cold spray. Un lien entre la porosité du dépôt et son comportement en corrosion est notamment montré. Enfin, une première approche du transfert de technologie du procédé à l’échelle industrielle est décrite. / Cold spray process is based on spraying particles carried by a gas at a supersonic speed onto a substrate. Particle deformation during impact with the substrate creates a coating. This spraying process can retain particle microstructure and produce very dense coating. This property is crucial for anticorrosion applications. The aim of this work is to understand the effect of cold spray aluminum coating microstructure on marine corrosion mechanisms. To achieve this goal, several aluminum powders (including pure aluminum, aluminum alloys and mixtures with alumina) are sprayed onto a steel substrate. Coating microstructure is studied down to a nanoscale (TEM). The coating-substrate bond strength is determined using pull-off testing. From a thorough microstructure study, various mechanisms are proposed to explain multiscale porosity formation in coatings. A numerical study using finite elements modeling complements this microstructure analysis. From particle speed (DPV-2000) and temperature (thermal camera) measurements during impact, new material models are optimized to model aluminum and alumina behavior at particle impact. Moreover, corrosion tests are conducted (including immersion and salt spray tests). The study of corroded coating microstructures is used to identify corrosion mechanisms which occur in the coating. A relationship between coating porosity and its corrosion behavior is particularly brought into light. Finally, a first approach to a technological transfer of this process to an industrial application is proposed.

Este estudo longitudinal investigou a influência de tratamentos de superfície com o laser de Er:YAG com 50?s de largura de pulso sobre a adesão de dois sistemas adesivos autocondicionantes (SA) em dentina hígida (DH) e dentina afetada por cárie (DAC) através dos teste de resistência de união (RU) de microcisalhamento (?SBS), teste de ultramicrodureza da camada de adesivo (NdA) e da camada híbrida (NdCH), além de análise da interface adesiva com microscopia eletrônica de varredura (MEV). A análise qualitativa dos tratamentos de superfície realizados foi executada através de MEV e microscopia eletrônica de transmissão (MET). A dentina oclusal planificada de 215 molares humanos foi protegida com verniz ácido resistente, exceto em janela de 4x5mm para produção de DAC artificial após 7 dias de desafio cariogênico com biofilme de S. mutans, permitindo dados pareados por substrato. Os espécimes foram divididos nos grupos experimentais de acordo com: tratamento de superfície [controle-sem tratamento-(G1); Laser 80-80mJ, 2 Hz, 12.58J/cm2-(G2); Laser 50-50mJ, 10 Hz, 9.4J/cm2-(G3)]; sistema adesivo [Clearfil SE Bond(CF) e Single Bond Universal(SB)]; substrato [DH(h) ou DAC(a)] e tempo de armazenamento em saliva artificial [24 horas (24) ou 1 ano (1)], compondo 24 grupos experimentais: CFG1h24; CFG1h1; CFG1a24; CFG1a1; CFG2h24; CFG2h1; CFG2a24; CFG2a1; CFG3h24; CFG3h1; CFG3a24; CFG3a1; SBG1h24; SBG1h1; SBG1a24; SBG1a1; SBG2h24; SBG2h1; SBG2a24; SBG2a1; SBG3h24; SBG3h1; SBG3a24; SBG3a1. Nos grupos tratados com laser a largura temporal de pulso foi ajustada em 50?s. A resina composta Z350XT foi utilizada para a confecção dos corpos de prova. Os sistemas adesivos foram aplicados de acordo com as instruções do fabricante. As análises de MEV e MET de superfície avaliaram somente o efeito dos tratamentos em ambos os substratos testados. Os valores de RU e de nanodureza foram analisados através do teste de ANOVA (três fatores) e do teste de comparações múltiplas de Tukey (?=0,05). Para o teste de ?SBS, para ambos os SA, e todos tratamentos de superfície, a DAC apresentou valores de RU menores comparados à DH; a influência do armazenamento em saliva artificial foi substrato dependente: corpos de prova obtidos com DAC apresentaram queda nos valores de RU após 1 ano de armazenamento, enquanto nenhuma diferença entre os grupos experimentais foi observada em dentina hígida. NdA revelou que apenas os corpos de prova construídos com CF apresentaram redução dos valores após 1 ano. A NdCH obtida com CF e SB, resultou em menores valores em DAC comparada à DH, após 1 ano de armazenamento ambos os substratos apresentaram redução da NdCH, para todos tratamentos de superfície. A MEV revelou que todas as interfaces adesivas, especialmente aquelas obtidas em DAC, sofreram degradação intensa após 1 ano. Os tratamentos com Laser 80 e Laser 50 promovem alteração superficial característica de ablação em DAC e DH, conforme observado em MEV de superfície, e alterações de fibrilas colágenas observadas em MET. Independentemente dos SA, a adesão e nanodureza em DAC é menor que em DH. Todas as interfaces adesivas obtidas foram sensíveis ao armazenamento em saliva artificial por 1 ano. A adesão não foi influenciada pelo tratamento com o laser Er:YAG com 50?s de largura de pulso. / This longitudinal study investigated the influence of super short pulse Er:YAG laser treatment on microshear bond strength (?SBS), adhesive and hybrid layer nanohardness test and qualitative interface scanning electron microscopy (SEM) of two self-etch adhesive systems to sound (SD) and caries-affected like dentin (CAD). Additionally, qualitative investigation of surface treatments by SEM and transmission electron microscopy (TEM) were performed. CAD lesions (4x5mm) were produced by 7 days S. mutans biofilm cariogenic challenge in 215 human ground flat human dentin specimens, enabling paired data by substrate. Specimen were divided in groups according to surface treatment [control-no treatment-(G1); Laser 80-80mJ, 2Hz, 12.58J/cm2-(G2); Laser 50-50mJ, 10Hz, 9.4J/cm2-(G3)]; self-etching adhesive system [Clearfil SE Bond(CF) and Single Bond Universal(SB)]; substrate [SD(h) or CAD(a)] and artificial saliva storage [24 hours(24) or 1 year(1)]: CFG1h24; CFG1h1; CFG1a24; CFG1a1; CFG2h24; CFG2h1; CFG2a24; CFG2a1; CFG3h24; CFG3h1; CFG3a24; CFG3a1; SBG1h24; SBG1h1; SBG1a24; SBG1a1; SBG2h24; SBG2h1; SBG2a24; SBG2a1; SBG3h24; SBG3h1; SBG3a24; SBG3a1. Pulse duration was set in 50?s for laser groups. ?SBS, nanohardness and interface SEM specimen preparation was constructed with Z350XT composite resin. Adhesive systems were applied according to manufacturer\'s instructions. Surface SEM and TEM specimen only evaluated treatment effects on distinct substrates. The ?SBS and nanohardness means were analysed using three-way ANOVA and Tukey´s multiples comparisons test (?=0.05). For ?SBS test, for both adhesive systems, and all surface treatments, CAD revealed lower ?SBS values compared to SD; the influence of artificial saliva storage was substrate dependent. CAD specimens resulted in lower ?SBS values after 1 year, while no difference among experimental groups was observed in SD. The adhesive layer (AL) nanohardness statistical evaluation revealed that only CF specimens decreased the AL nanohardness after 1 year of storage. The hybrid layer (HL) produced with CF and SB, resulted in lower nanohardness values for CAD than SD, which reduces after 1 year storage, for all surface treatments. Interface SEM analysis revealed that all adhesive interfaces, especially those in CAD, have experienced degradation after 1 year of storage. Laser 80 and Laser 50 promotes surface ablation characteristics in CAD and SD, as noted in surface SEM and collagen fibrils alterations observed in TEM. Despite of adhesive systems, bonding and nanohardness to CAD is lower than to SD. All tested adhesive interfaces were sensitive to saliva storage. Surface treatment with 50?s Er:YAG laser did not influence on bonding.

A dentina em diferentes profundidades apresenta diferentes densidades tubulares e permeabilidades dentinárias, afetando diretamente a adesão dos sistemas adesivos. Objetivos: avaliar a resistência ao cisalhamento de quatro sistemas adesivos e a densidade tubular em diferentes profundidades de dentina. Material e Método: Quatro grupos de dentina de terceiros molares humanos (superior vestibular, superior palatina, inferior vestibular, inferior lingual) foram avaliados quanto à resistência ao cisalhamento (Método ISO 11405) e em microscopia eletrônica de varredura para as profundidades superficial, 0.5, 1.0, 1.5 e 2.0 mm. Os adesivos Adper Single Bond, Xeno III, Clearfil SE Bond e Adper Prompt L-Pop foram selecionados. As análises foram realizadas nos coposde- prova de forma vinculada e os dados submetidos à ANOVA. Resultados: Os resultados dos testes de resistência ao cisalhamento mostraram que os molares superiores apresentaram significância estatística para os fatores profundidade e adesivo, e para as interações profundidade X adesivo, face X profundidade e face X adesivo. Os molares inferiores revelaram significância para os três fatores de variação e para as interações profundidade X adesivo e face X adesivo. O adesivo Xeno III apresentou valores médios superiores tanto nos molares superiores como inferiores. A análise em microscopia eletrônica de varredura revelou aumento da densidade tubular à medida do aumento da profundidade da dentina. Conclusões: Em molares humanos, os fatores profundidade de dentina e sistema adesivo influenciaram a resistência ao cisalhamento. À medida do aumento da profundidade da dentina, a densidade tubular aumenta e a resistência ao cisalhamento diminui, porém esta relação pode ser modificada pelo sistema adesivo / Dentin at various depths presents different tubular density and permeability, thus directly affecting the adhesion of bonding systems. Aim: to evaluate the relationship between tubular density and shear strength of four bonding systems at different dentin depths. Material and methods: upper and lower human molars were analyzed regarding dentin tubular density at different depths by scanning electron microscopy, as well as shear strength (ISO TR 11405 method) for the dependent variables depth (surface dentin, 0.5, 1.0, 1.5 and 2.0 mm), bonding system (total etch and self-etching) and tooth aspect (buccal or palatal/lingual). The bonding systems Single Bond Adper, Xeno III, Clearfil SE Bond e Adper Prompt L-Pop were selected. The analysis were performed in a sampledependent way and results were submitted to the ANOVA test. Results: scanning electron microscopy revealed an increase in tubular density accompanying the depth. Shear strength tests showed that upper molars present significant differences for the factors depth and bonding system, as well as for the interactions depth x bonding system, aspect x depth and aspect x bonding system. Lower molars revealed significance for the three dependent variables and for the interactions depth x bonding system and aspect x bonding system. The Xeno III bonding system presented average values higher than the other products, both in upper and lower molars, in deep dentin (1.0, 1.5 and 2.0), in a regular way. Conclusions: In general, as the dentinal depth increases, so does the tubular density. In human molars, the dependent variables dentin depth and bonding system influenced the shear strength. The self-etching bonding system Xeno III revealed potential maintenance of shear strength when used in dentin at different depths. As dentin depth increases, so does the tubular density, thus lowering shear strength; however, this relationship is dependent on the bonding system used.

A dentina em diferentes profundidades apresenta diferentes densidades tubulares e permeabilidades dentinárias, afetando diretamente a adesão dos sistemas adesivos. Objetivos: avaliar a resistência ao cisalhamento de quatro sistemas adesivos e a densidade tubular em diferentes profundidades de dentina. Material e Método: Quatro grupos de dentina de terceiros molares humanos (superior vestibular, superior palatina, inferior vestibular, inferior lingual) foram avaliados quanto à resistência ao cisalhamento (Método ISO 11405) e em microscopia eletrônica de varredura para as profundidades superficial, 0.5, 1.0, 1.5 e 2.0 mm. Os adesivos Adper Single Bond, Xeno III, Clearfil SE Bond e Adper Prompt L-Pop foram selecionados. As análises foram realizadas nos coposde- prova de forma vinculada e os dados submetidos à ANOVA. Resultados: Os resultados dos testes de resistência ao cisalhamento mostraram que os molares superiores apresentaram significância estatística para os fatores profundidade e adesivo, e para as interações profundidade X adesivo, face X profundidade e face X adesivo. Os molares inferiores revelaram significância para os três fatores de variação e para as interações profundidade X adesivo e face X adesivo. O adesivo Xeno III apresentou valores médios superiores tanto nos molares superiores como inferiores. A análise em microscopia eletrônica de varredura revelou aumento da densidade tubular à medida do aumento da profundidade da dentina. Conclusões: Em molares humanos, os fatores profundidade de dentina e sistema adesivo influenciaram a resistência ao cisalhamento. À medida do aumento da profundidade da dentina, a densidade tubular aumenta e a resistência ao cisalhamento diminui, porém esta relação pode ser modificada pelo sistema adesivo / Dentin at various depths presents different tubular density and permeability, thus directly affecting the adhesion of bonding systems. Aim: to evaluate the relationship between tubular density and shear strength of four bonding systems at different dentin depths. Material and methods: upper and lower human molars were analyzed regarding dentin tubular density at different depths by scanning electron microscopy, as well as shear strength (ISO TR 11405 method) for the dependent variables depth (surface dentin, 0.5, 1.0, 1.5 and 2.0 mm), bonding system (total etch and self-etching) and tooth aspect (buccal or palatal/lingual). The bonding systems Single Bond Adper, Xeno III, Clearfil SE Bond e Adper Prompt L-Pop were selected. The analysis were performed in a sampledependent way and results were submitted to the ANOVA test. Results: scanning electron microscopy revealed an increase in tubular density accompanying the depth. Shear strength tests showed that upper molars present significant differences for the factors depth and bonding system, as well as for the interactions depth x bonding system, aspect x depth and aspect x bonding system. Lower molars revealed significance for the three dependent variables and for the interactions depth x bonding system and aspect x bonding system. The Xeno III bonding system presented average values higher than the other products, both in upper and lower molars, in deep dentin (1.0, 1.5 and 2.0), in a regular way. Conclusions: In general, as the dentinal depth increases, so does the tubular density. In human molars, the dependent variables dentin depth and bonding system influenced the shear strength. The self-etching bonding system Xeno III revealed potential maintenance of shear strength when used in dentin at different depths. As dentin depth increases, so does the tubular density, thus lowering shear strength; however, this relationship is dependent on the bonding system used.

Avanços na tecnologia introduziram o laser como um grande aliado na remoção seletiva do tecido cariado. Entretanto, o efeito dos lasers e seus diferentes parâmetros nos tecidos duros dentais e fibrilas colágenas não foi completamente estudado. O objetivo deste estudo foi avaliar os efeitos da irradiação com os lasers de Er:YAG e Er,Cr:YSGG na morfologia e na resistência de união da dentina irradiada à resina composta. Sessenta e quatro hemi-discos de dentina obtidos de terceiros molares humanos foram aleatoriamente divididos em 9 grupos (n=7): G1 Controle (não irradiado); G2 Laser de Er:YAG 250 mJ, 4 Hz; G3 Laser de Er:YAG 200 mJ, 4 Hz; G4 Laser de Er:YAG 180 mJ, 10 Hz; G5 Laser de Er:YAG 160 mJ, 10 Hz; G6 - Laser de Er,Cr:YSGG 2W, 20 Hz; G7 - Laser de Er,Cr:YSGG 2,5W, 20 Hz; G8 - Laser de Er,Cr:YSGG 3W, 20 Hz; G9 - Laser de Er,Cr:YSGG 4W, 20 Hz. Destes, vinte e sete amostras (n=3) foram processadas e destinadas à avaliação em Microscopia Eletrônica de Varredura (MEV) para análise morfológica de superfície e em corte transversal da dentina irradiada. Nove fragmentos (n=1) foram submetidos à Microscopia Eletrônica de Transmissão (MET) e vinte e sete (n=3) foram restaurados para análise da interface adesiva. Para o teste de resistência de união, 45 superfícies dentinárias planificadas foram restauradas e, após 24 horas de armazenamento em água, foram submetidas ao teste de microtração. O teste de ANOVA (=5%) foi realizado e verificou-se que o G1 apresentou os maiores valores de resistência de união quando comparado aos demais grupos experimentais. Não houve diferença estatisticamente significativa entre os grupos irradiados, e a análise morfológica revelou para estes grupos uma superfície irregular, com aparência escamosa, sem smear layer e com os túbulos dentinários abertos. Nos cortes transversais foi possível observar que esses efeitos se estendem à subsuperfície dentinária e resultam na formação de um padrão modificado dos tags durante o processo de hibridização. Os resultados deste estudo in vitro sugerem que a irradiação com os lasers de Er:YAG e Er,Cr:YSGG promovem um padrão morfológico específico da superfície dentinária, os quais podem interferir negativamente nos valores de resistência de união à resina composta. / Improvements on technology have introduced the laser as a great ally in the selected removal of dental caries. However, the different laser parameters and their effects on dental hard tissues and collagen fibrils have not yet been completely studied. The aim of the present study was to evaluate the effect of Er:YAG and Er,Cr:YSGG laser irradiation on dentin morphology and on microtensile bond strength of resin composite to the irradiated dentin. Sixty-four dentin hemi-disks obtained from sound human third molars were randomly divided into 9 groups (n=7): G1 Control, G2 Er:YAG Laser 250 mJ, 4 Hz; G3 Er:YAG Laser 200 mJ, 4 Hz; G4 Er:YAG Laser 180 mJ, 10 Hz; G5 Er:YAG Laser 160 mJ, 10 Hz; G6 - Er,Cr:YSGG Laser 2W, 20 Hz; G7 - Er,Cr:YSGG Laser 2,5W, 20 Hz; G8 - Er,Cr:YSGG Laser 3W, 20 Hz; G9 - Er,Cr:YSGG Laser 4W, 20 Hz. Twenty seven specimens (n=3) were processed for Scanning Electron Microscopy (SEM) for surface and cross-sectional morphological analysis. Nine specimens (n=1) were processed for Transmission Electron Microscopy (TEM) and twenty seven (n=3) were restored to evaluate the adhesive interface. For the microtensile bond strength (^TBS) test, 45 flat occlusal dentin surfaces were restored and after storage in water for 24h, were submitted to ^TBS test. ANOVA (=5%) showed that G1 (control group) presented the highest ^TBS values when compared with the irradiated groups, which did not differ from each other. SEM analysis showed an irregular scaly surface, free of smear layer and with open dentinal tubules. The cross-sectional dentin micrographs showed that the effects of laser extended to the dentin subsurface resulting in a pattern of tags modified in the hibridization process. The findings of this in vitro study showed that both Er:YAG and Er,Cr:YSGG laser irradiation resulted in a specific morphological pattern of dentin that negatively affects the bond strength to resin composite to such dentin.