Influência da Concentração e do Tempo de Condicionamento com Ácido Hidrofluorídrico na Rugosidade e Morfologia Superficial de uma Zircônia Glazeada / Influence of Hydrofluoric Acid Concentration and Etching Time on the Surface Roughness and Morphology of a Glazed Zirconia

Objetivo: Avaliar o efeito da concentração e do tempo de condicionamento com ácido fluorídrico na rugosidade e morfologia superficial de uma zircônia glazeada. Materiais e Métodos: Blocos de cerâmica à base de zircônia (5×5×3 mm) (Vita YZ-2000-Cubes, Vita- Zahnfabrik, Alemanha) foram confeccionados e divididos em 6 grupos, de acordo com os fatores "concentração do ácido fluorídrico (HF)" (5% e 10%) e "tempo de condicionamento" (20 s, 60 s e 90 s) (n=2): HF10/20 = HF 10% + 20 s; HF10/60 = HF 10% + 60 s; HF10/90 = HF 10% + 90 s; HF5/20 = HF 5% + 20 s; HF5/60 = HF 5% + 60 s; HF5/ 90 = HF 5% + 90 s. O glaze (Vita Akzent, Vita-Zahnfabrik, Alemanha) foi aplicado com o auxílio de um pincel e sinterizado de acordo com as recomendações do fabricante. Após os diferentes protocolos de condicionamento, foram aferidas cinco medições de rugosidade (Ra) para cada espécime em Perfilômetro Digital (Wyko®, Modelo NT- 1100, Veeco, EUA). Os dados (µm) obtidos foram analisados estatisticamente com análise de variância (ANOVA 2-fatores) e Teste de Tukey (95%). Resultados: O fator "concentração do ácido fluorídrico" (p=0,149) não foi significante estatísticamente. No entanto, o fator "tempo de condicionamento" (p=0,009) foi significante. A interação entre os fatores também apresentou significância estatística (p=0,00). As médias de rugosidade (±desvio-padrão) obtidas foram (µm): GHF10/20=1,94(±0,72)A, GHF5/90=1,92(±0,19)A, GHF5/ 20=1,38(±0.48)AB, GHF5/60=1,18(±0,63)B, GHF10/60=1,17(±0,30)B, GHF10/90=0,82(±0,27)B (Tukey). Conclusão: Conclui-se que o ácido fluorídrico (10%) em maior concentração, associado a um menor tempo de condicionamento (20 s), promoveu maior rugosidade superficial da zircônia glazeada. (AU)

Objective: The aim of this study was to evaluate the effect of different etching protocols on the surface roughness of a glazed zirconia. Material and Methods: Zirconia ceramic-blocks (5 × 5 × 3 mm) (Vita YZ-2000-Cubes, Vita-Zahnfabrik, Germany) were prepared and divided into 6 groups according to the variables "concentration of hydrofluoric acid (HF)" (5 % and 10 %) and " etching time " (20 s, 60 s and 90 s) (n = 2), as follows: HF10/20 = HF 10% + 20 s; HF10/60 = HF 10% + 60 s; HF10/90 = HF 10% + 90 s; HF5/20 = HF 5% + 20 s; HF5/60 = HF 5% + 60 s; HF5/90 = HF 5% + 90 s. The glaze (Vita Akzent, Vita- Zahnfabrik, Germany) was applied with a brush and sintered according to the manufacturer's recommendations. After different etching protocols, five roughness (Ra) measurements were taken for each specimen in a digital profilometer (Wyko ®, Model NT-1100, Veeco, USA). The data were statistically analyzed using analysis of variance (ANOVA 2­way) and Tukey's test (95%). Results: The variable "concentration of hydrofluoric acid" (p=0.149) was not statistically significant, while the variable "etching time" (p=0.009) was significant. The interaction between variables was statistically significant (p = 0.00). The roughness averages (± standard deviation) obtained were (µm): GHF10/20=1.94(±0.72)A, GHF5/90=1.92(±0.19)A, GHF5/ 20=1.38(±0.48)AB, GHF5/60=1.18(±0.63)B, GHF10/60=1.17(±0.30)B, GHF10/90=0.82(±0.27)B (Tukey). Conclusion: It can be concluded that hydrofluoric acid (10%) at a higher concentration associated with a lower etching time (20 s) promoted higher superficial roughness on glazed zirconia. (AU)

A aplicação de um glaze na superfície de cimentação melhora a adesão da zircônia ao cimento resinoso? / Does the application of a glaze layer in the intaglio surface improve the adhesion between zirconia and resin cement?

Este trabalho teve como objetivo avaliar o efeito de diferentes tratamentos de superfície na resistência adesiva entre a interface zircônia/cimento resinoso. Blocos de zircônia (12 x 11,6 x 1,2 mm) foram divididos em cinco grupos (n=10) e classificados conforme o tratamento de superfície. Nas amostras em que a superfície não foi jateada, os filmes de glaze foram avaliados em função do condicionamento ou não das amostras com ácido fluorídrico (HF). No jateamento das superfícies das cerâmicas foram utilizadas microesferas de alumina, com e sem revestimento de sílica, e avaliada a influência dos tratamentos na resistência adesiva entre a superfície da cerâmica e o cimento resinoso. No teste de resistência de união, as amostras com glaze condicionado e com jateamento (alumina + sílica) apresentaram resultados superiores em relação às amostras não jateadas. As falhas foram classificadas em adesiva, mista e coesiva com a ajuda de um estereomicroscópio. A caracterização das superfícies foi avaliada por microscopia eletrônica de varredura e espectroscopia de energia dispersiva. A espessura dos filmes glaze, obtida pela micrografi a da secção transversal das amostras, apresentou espessuras semelhantes independentemente do tratamento. Os tratamentos de superfície da zircônia com glaze condicionado (com e sem secagem) e jateamento (alumina + sílica) obtiveram os melhores resultados de resistência de união.

This work aimed to evaluate the effect of different surface treatments on bond strength at the zirconia/resin cement interface. Zirconia blocks (12 x 11.6 x 1.2 mm) were divided into five groups (n=10) and classified according to the surface treatment. In the samples wherein the surface glaze has not been sandblasted the films were assessed for conditioning or not the samples with hydrofluoric acid (HF). Alumina microespheres with and without silica coating were used to blast the surfaces, and also to study the effect of treatments on bond strength between the ceramic surface and the resin cement. In the bond strength test samples with conditioning glaze and sandblasting (alumina + silica) showed higher scores than the non-blasted samples. The flaws were classified as adhesive, cohesive and mixed with the aid of a stereomicroscope. Surface characterization was evaluated by scanning electron microscopy and energy dispersive spectroscopy. The thickness of the glaze film obtained by the micrograph of the cross section of the samples showed similar thicknesses regardless of treatment applied. The zirconia surface treatments with conditioning glaze (with and without drying) and sandblasting (alumina + silica) generated the best bond strength results.

Influence of drying time of adhesive systems on the bond strength between resin cement and feldspathic ceramic / nfluência do tempo de secagem de sistemas adesivos na resistência de união entre cimento resinoso e cerâmica feldspática

Objetivo: Este estudo se propôs avaliar o efeito de diferentes tempos de secagem de dois adesivos tipo ‘total-etch & rinse’ e ciclagem térmica na resistência adesiva entre cerâmica feldspatica e cimento resinoso. Material e Métodos: Trinta e dois blocos (12×10×4 mm) de cerâmica feldspática e respectivos blocos (32) de resina composta foram obtidos. A superfície de cimentação de cada bloco cerâmico foicondicionada por ácido fluorídrico (HF), silanizada (S), e recebeu a aplicação de um dos dois sistemas adesivos testados (SB - Single Bond 2, 3M-ESPE; ou PB – Prime & Bond NT, Dentsply). Então a superfície com o adesivo foi seca em diferentes tempos (5, 10 e 15s) antes da cimentação. Após, um cimento resinoso foi aplicado sobre a superfície de cimentação e o bloco correspondente de resina foi cimentado. Os palitos para microtração foram obtidos, sendo que metade deles foram imediatamente testados, enquanto os demais foram submetidos à ciclagem térmica e armazenagem (150 dias). Para os grupos sem envelhecimento, o tempo de secagem mais longo (15s) aumentou a resistência para o adesivo SB, enquanto que reduziu a resistência para o adesivoPB. Resultados: Para os grupos envelhecidos, as resistências adesivas dos diferentes tempos de secagem não foram diferentes estatisticamente, independente do adesivo. A falha predominante foi coesiva do cimento resinoso, seguido pela falha na interface cerâmica cimento. Conclusão: Conclui se que tempos mais longos de secagem podem melhorar a resistência adesiva à cerâmica testada, usando o adesivo SB. Por outro lado, tempos mais curtos podem otimizar a adesão para o adesivo PB. O envelhecimento afetou a adesão somente nos grupos do adesivo SB

Objective: This study evaluated the effect of drying times of two total-etch & rinse adhesives on the resin bond strength to a feldsphatic ceramic, before and after aging. Material and Methods:Feldsphatic-ceramic CAD-CAM bars were cut into blocks (12×10×4 mm) with a cutting machine (N = 32). Impressions were made of each ceramic block with silicone putty material and the negativespace was filled with a composite resin. The bonding ceramic surface was etched with hydrofluoric acid, silanized, and the adhesive system (SB- Single Bond 2, 3M-ESPE; or PB- Prime & Bond NT, Dentsply) was applied. The samples were dried at different times (5, 10 and 15 s) before the cementation. The resin and ceramic blocks were cemented bya dual cure resin cement. All samples were stored in distilled water at 37 °C for 24 h. For the μ-TBS test, the samples were sliced into microbars. Half of the bars of each block was tested after 24 h and, the other bars were submitted to thermocycling (12,000×) and water storage (150 d). For the 24 h groups, the longer drying time increased (p < 0.05) the bond strength of SB (water/alcohol adhesive), while reduced (p < 0.05) for the PB group (acetone based adhesive). Results: For the aged groups, the bond strength for the different drying times had no significant difference, for the both adhesives. Conclusion: Longer drying times increased the bond strength values of SB. Smaller drying times increased the bond strength values of PB. The aging protocol influenced the bond strength of SB groups.

Influence of CAD-CAM diamond bur deterioration on surface roughness and maximum failure load of Y-TZP-based restorations.

PURPOSE: To investigate the influence of CAD-CAM diamond bur deterioration on surface roughness (Ra) and maximum failure load (Lf) of Y-TZP-based ceramic (YZ) substructures (SB) veneered with a feldspathic porcelain. METHODS: Two sets of burs (B1 and B2) were used to fabricate 30 YZ SB each in a CAD/CAM system (Cerec InLab). The SB were identified (1-30) according to the milling sequence (MS). SEM images of the burs were recorded before milling, and after milling 15 and 30 SB. The SB Ra was measured. All SB were veneered, cemented onto a fiber reinforced epoxy resin die, and loaded to failure. Specimens from B1 group were cyclic fatigued (106 cycles) before loading to failure. Fractographic analysis was performed. Data were statistically analyzed using Student's t-test, Weibull analysis, Pearson's correlation and ANOVA (α= 0.05). RESULTS: The mean Ra value of B1 specimens was statistically greater than B2. Weibull modulus of B1 and B2 were statistically similar. The correlation between MS and Lf was not statistically significant for the groups. MS and Ra had significant correlation for both groups (B1: r= -0.514, P= 0.015; B2: r= -0.462, P= 0.03). Although the visual aspect (SEM) of the burs was similar after 30 millings, the mean Ra values were significantly different after 27 millings for B1 and 24 millings for B2.

Pressable feldspathic inlays in premolars: effect of cementation strategy and mechanical cycling on the adhesive bond between dentin and restoration.

PURPOSE: To evaluate the effect of the cementation strategy and mechanical cycling (MC) on the microtensile bond strength (MTBS) of feldspathic inlays cemented to premolars. MATERIALS AND METHODS: Forty-eight human premolars were prepared and porcelain inlays were produced. Specimens were allocated into 3 groups, based on the cementation strategy: 1) conventional adhesive cementation (RelyX ARC, 3M ESPE): application of etch-and-rinse single bottle adhesive to dentin / ceramic surface treated with hydrofluoric acid (HF) and silane (S) / cementation with resin cement; 2) simplified cementation using a self-adhesive resin cement (RelyX U100, 3M ESPE); 3) modified simplified cementation using a self-adhesive resin cement (RelyX U100, 3M ESPE) with HF+S treatment. Half of the specimens from each group were submitted to MC (2x106 pulses, frequency = 4 Hz, load = 100 N). Each specimen was serially sliced for MTBS and the failures were classified. The stress distribution analysis using FEA was verified. RESULTS: All of the bar-samples from G2 were lost during cutting of the specimens. Mechanical-cycling had no significant effect on bond strength, whereas cementation strategy significant affected MTBS results. The most common type of failure was cohesive of cement. FEA showed that stresses were concentrated mainly at the loading region going up to the root fixation. CONCLUSION: Porcelain inlays cemented with conventional resin cement or self-adhesive resin cement should be associated with ceramic surface treatment. FEA showed the most critical zone for failure is located in the cement region close to the marginal crest.

Caracterização de uma cerâmica 3Y-TZP e avaliação do efeito de tratamentos de superfície na adesão da cerâmica ao glaze ou cimento resinoso / Characterization of a 3-YTZP ceramic and evaluation of the surface treatment on the adhesion of ceramic and glaze or resin cement

O objetivo do presente estudo foi avaliar os parâmetros de adesão entre glaze e full-contour zirconia (FCZ) e FCZ glazeada e cimento resinoso. Zircônia e glaze tiveram as suas propriedades caracterizadas. Amostras de FCZ foram divididas em 5 grupos: (GL) aplicação de glaze; (AL+GL) jateamento com óxido de alumínio + glaze; (CJ+GL) partículas de óxido de alumínio modificada por sílica(Cojet®) + glaze; (SP+GL) tratamento químico com solução piranha + glaze; (CJ) Cojet. Microscopia eletrônica de varredura (MEV) e de força atômica (MFA) foram realizadas para avaliar a topografia das amostras. Scratch test foi realizado para avaliar o tipo de união entre zircônia e glaze após os diferentes tratamentos [(GL), (AL), (CJ) e (SP). Durante a cimentação, os grupos glazeados [(GL), (AL+GL), (CJ+GL) e (SP+GL)] foram tratados com ácido fluorídrico (HF) e silano; e o grupo não glazeado (CJ) apenas com silano. O cimento resinoso foi unido à zircônia utilizando um dispositivo específico para o teste de cisalhamento (SBS). Para a realização do teste SBS, metade dos espécimes de cada tratamento foi ensaiada 24 h após a cimentação e a outra metade foi envelhecida (armazenagem e termociclagem). Para a avaliação da retenção, foram confeccionados coroas FCZ e preparos para coroa total em substrato deresina epóxica (G10) (simulando um dente). Os grupos que receberam tratamento na superfície interna da coroa [(GL), (CJ+GL), (SP+GL) e (CJ)] foram cimentados com cimento resinoso sem MDP (Multilink Automix, 3M). O grupo que não recebeu tratamento na superfície interna (PF) foi cimentado utilizando um cimento resinoso contendo MDP (Panavia F, Kuraray). Os dados de adesão foram analisados estatisticamente (ANOVA e Tukey test). A full-contour zirconia apresentou alta densidade, microestrutura homogênea e propriedades mecânicas comparáveis à zircônia tradicional. O glaze correspondente apresentou picos coincidentes com à fase leucita (DRX) com morfologia irregular em formato e tamanho. ...

The aim of the present study was to evaluate the adhesive parameters between glaze and full-contour zirconia (FCZ) and overglazed FCZ and resin cement. Zirconia and glaze were tested to determined theirs properties. FCZ samples were divided into 5 groups: (GL) glaze application; (AL+GL)sandblasting with aluminum oxide + glaze; (CJ+GL) tribochemical silica coating (Cojet®) + glaze; (SP+GL) chemical surface treatment with piranha solution+glaze; (CJ) Cojet. Electron scanning microscopy (SEM) and atomic force microscopy (MFA) were performed to evaluate the FCZ topography.Scratch test was executed to evaluate the bonding between FCZ and glazeafter the different surface pretreatment. For the bonding procedures the glazed groups [(GL), (AL+GL), (CJ+GL) and (SP+GL)] were etched with hydrofluoric acid (HF) and treated with a silane coupling agent and the group without glaze (CJ) was treated only with a silane. The resin cement was bonded to the zirconia surface using a dedicated device for the shear test(SBS). For the SBS test, half of the samples were tested after 24 h and theother half after storage and thermocycling. To evaluate the tensile retention of FCZ crowns cemented on epoxy resin (G10) specimens simulating fullcontour crowns were made. Pretreated groups [(GL), (CJ+GL), (SP+GL) and (CJ)] were bonded with a resin cement without MDP (Multilink Automix, 3M). The group without surface pretreatment (PF) was bonded with a MDP-based resin cement (Panavia F, Kuraray). The adhesive data were statistically analysed (ANOVA e Tukey test). FCZ showed high density, homogeneous microstructure and mechanical properties similar to the traditional zirconia. FCZ glaze was characterized as a leucite with irregular shape and size morphology. The scratch test pattern was similar for all the evaluated groups and classified as a cohesive failure of the glaze. The shear data suggested that the chemicall treatment, before the glaze application, did not improve the bonding ...

Influence of convergence angle of tooth preparation on the fracture resistance of Y-TZP-based all-ceramic restorations.

OBJECTIVE: To investigate the influence of the convergence angle of tooth preparation on the fracture load of Y-TZP-based ceramic (YZ - Vita YZ) substructure (SB) veneered with a feldspathic porcelain (VM9 - Vita VM9). METHODS: Finite element stress analysis (FEA) was performed to examine the stress distribution of the system. Eighty YZ SB were fabricated using a CAD-CAM system and divided into four groups (n=20), according to the total occlusal convergence (TOC) angle: G6 - 6° TOC; G12 - 12° TOC; G20 - 20° TOC; and G20MOD - 20° TOC with modified SB. All SB were veneered with VM9, cemented in a fiber reinforced epoxy resin die, and loaded to failure. Half of the specimens from each group (n=10) were cyclic fatigued (10(6) cycles) before testing. Failure analysis was performed to determine the fracture origin. Data were statistically analyzed using Anova and Tukey's tests (α=0.05). RESULTS: The greatest mean load to fracture value was found for the G20MOD, which was predicted by the FEA. Cyclic fatigue did not significantly affect the load of fracture. Catastrophic failure originating from the internal occlusal surface of the SB was the predominant failure mode, except for G20MOD. SIGNIFICANCE: The YZ-VM9 restorations resisted greater compression load than the usual physiological occlusal load, regardless of the TOC angle of preparations. Yet, the G20MOD design produced the best performance among the experimental conditions evaluated.

Restaurações inlays em cerâmicas feldspáticas injetadas em pré molares: efeito da estratégia de cimentação e da ciclagem mecânica na resistência adesiva entre dentina e restauração / Feldspathic Ceramic inlays restorations in premolars injected: effects of the bonding strategy and mechanical cycling on the bond strength between dentin and restoration

O estudo avaliou o efeito da estratégia de cimentação e da ciclagem mecânica na resistência de união entre dentina e restauração. O tipo de falha dos espécimes foi classificado e a distribuição de tensões foi analisada pela simulação utilizando o método de análise por elementos finitos (MEF). Quarenta e oito (N= 48) pré-molares superiores foram preparados (cavidade tipo MOD) e 48 restaurações inlays de cerâmica feldspática foram obtidas. Os espécimes foram alocadas em 3 grupos, considerando a estratégia de cimentação (N= 16): 1- convencional (Grupos 1 e 2): sistema adesivo condicionamento total de passo único (tratamento da dentina), tratamento da superfície cerâmica com ácido fluorídrico (HF) e silano (S), e cimentação com cimento resinoso; 2- estratégia simplificada (grupos 3 e 4) utilizando o cimento resinoso autoadesivo RelyX U100 (3M) sem tratamento das superfícies da dentina e da cerâmica; 3- estratégia simplificada modificada (grupos 5 e 6) utilizando o cimento resinoso RelyX U100 associado ao tratamento de superfície com HF+S. Os dentes dos grupos 2, 4 e 6 não foram ciclados, enquanto que aqueles dos grupos 1, 3 e 5 foram submetidos a ciclagem mecânica (CM): 2.000.000 pulsos, carga de 100N sobre as cúspides (a restauração não recebeu carga), a 37 oC. Cada espécime foi seccionado de forma seriada para produzir corpos de prova em forma de barras dente-restauração-dente para serem submetidas ao teste de microtração. A região da fratura de cada espécime foi analisada e classificada. A distribuição de tensões em um modelo virtual simulando as condições do estudo in vitro, pelo método de elementos finitos, foi verificada. A Análise de Variância mostrou que: o efeito interação dos fatores não foi estatisticamente significante (a alteração da resistência de união em razão da ciclagem mecânica (CM) para a Estratégia 1 não difere estatisticamente da alteração constatada para a Estratégia 3)...

The study evaluated the effect of the bonding strategy and mechanical cycling on the bond strength between dentin and inlay restoration. The specimens failure mode and stress distribution (Finite element analysis FEA) was analyzed. Forty-eight (n = 48) pre-molars were prepared (MOD cavity) and 48 feldspathic ceramic inlays restorations were obtained. Specimens (tooth-restoration) were allocated into three groups considering the bonding strategy (n = 16): 1 - Conventional (groups 1 and 2): one-step total etch adhesive system (dentin treatment), hydrofluoric acid (HF) and silane (S) ceramic surface treatment, cementation with resin cement, 2 - Simplified (groups 3 and 4): RelyX U100 (3M) adhesive resin cement without dentin and ceramic surface treatment; 3 - Simplified modified (groups 5 and 6): RelyX U100 associated with HF + surface treatment. Specimens from groups 1, 3 and were subjected to mechanical cycling (CM) - 2,000,000 pulses, 100N on the cusp, 37ºC. Each specimen was sectioned to produce tooth-restoration-tooth bars specimens (cross-sectional area: 1mm2) that were submitted to microtensile bond strength test. The fractured area of each specimen was analyzed. Stress distribution was analyzed by a virtual model simulating the in vitro study by FEA. Variance analysis showed that: factors effect interaction was not statistically significant (there was no statistically differences between strength bond values with CM from groups 1 and 3). Strategy effect was statistically significant (strategy 3 mean strength bond [5.59 MPa] was significantly higher than the strategy 1strength bond [3.44 MPa]). Predominant failure mode was cement-cohesive-type. Von Mises analysis showed stress concentration at cement near the marginal ridge. It can be concluded that feldspathic porcelain cementation with dual or self-adhesive resin cement should be associated with 9% hydrofluoric acid and silane agent application. The simplified cementation...