Different bonding agents effect on adhesive bond strength: lithium disilicate glass ceramic / Efeito de diferentes agentes de união na cimentação adesiva em superfície cerâmica de dissilicato de lítio

Introduction: The silanization of the ceramic surface prior to applying the adhesive and/or resinous materials plays an important role in bond strength. Nowadays, a new family of adhesive systems has been introduced into the market, aiming to simplify the technique of adhesive procedures during cementation. Objective: To investigate the effectiveness of different bonding agents containing silane and primer on Lithium Disilicate Glass Ceramic (LD) surface by shear bond strength tests. Material and method: 130 LD ceramic blocks were included in acrylic resin, polished and washed in ultrasound for 10 minutes. The specimens were divided into 2 groups according to surface treatment: Polished Surface (PS); Hydrofluoric Acid 9.5% - 20s (HF). Each group was divided into 5 subgroups (n = 13) according to bonding agent type: metallic primer containing MDP (ZPrimePlus, Bisco Inc); two traditional silanes (MonobondPlus, IvoclarVivadent / Porcelain Prime, Bisco Inc.); mixture of silane and resin (Kerr Silane, Kerr); mixture of silane and universal adhesive (Single-bond Universal, 3M Espe). The specimens were mounted in a standard device for shear testing (UltradentBonding Assembly), cemented with dual resin cement (RelyX UltimateTM, 3M Espe.) and photo-polymerized for 20s. The samples were tested after 24 hours and 3 months of storage in distilled water at ±36 °C. The data were analyzed by 3-Way Anova and Tukey's test (α = 5%). Result: Shear bond strength (SBS) was significantly influenced by surface treatment, bonding agent used and storage (p <0.001). Conclusion: Adequate adhesive bond strength to Lithium Disilicate Glass Ceramic can be obtained with traditional silanes, combined with HF acid pretreatment surface.

Introdução: A silanização da superfície cerâmica antes da aplicação do adesivo e/ou materiais resinosos desempenha um papel importante na resistência adesiva. Atualmente, uma nova família de sistemas adesivos foi introduzida no mercado, visando simplificar a técnica dos procedimentos adesivos durante a cimentação. Objetivo: Investigar a eficácia de diferentes soluções contendo silano e primer na superfície de cerâmicas de Dissilicato de Lítio (DLT) por meio de testes de resistência adesiva por cisalhamento. Material e método: 130 blocos cerâmicos DLT foram incluídos em resina acrílica, polidos e lavados em ultra-som por 10 minutos. Os espécimes foram divididos em 2 grupos de acordo com tratamento de superfície: Superfície Polida (PS); Ácido Hidro-Fluorídrico 9,5% - 20s (HF). Cada grupo foi dividido em 5 sub-grupos (n = 13) de acordo com o tipo de primer/silano: primer metálico contendo MDP (ZprimePlus, Bisco Inc); dois silanos tradicionais (MonobondPlus, IvoclarVivadent / Porcelain Prime, Bisco Inc.); mistura de silano e resina (Kerr Silane, Kerr); mistura de silano e adesivo universal (Single-bond Universal, 3M Espe). Os espécimes foram montados em um dispositivo padrão (UltradentBonding Assembly) para teste de cisalhamento Bisco Shear Bond Tester), cimentados com cimento resinoso dual (RelyX UltimateTM, 3M Espe.) e foto-polimerizados por 20s. O teste foi realizado após o período de: 24 horas e 3 meses de armazenamento em água destilada à ±36 °C. Os dados foram analisados por 3-Way Anova e Teste de Tukey (α=5%). Resultado: A resistência adesiva ao cisalhamento (SBS) foi significativamente influenciada pelo tipo de tratamento da superfície, pelo tipo de agente de união utilizado e pelo armazenamento (p<0,001). Conclusão: Adequada resistência adesiva pode ser obtida com silanos tradicionais, combinados com o pré-tratamento de superfície com ácido HF.

Alternativas de tratamientos de superficie para adhesión de cerámica de disilicado de litio / Alternatives of surface treatments for adhesion of lithium disilicate ceramics

Introduction: the clinical success of a restoration is strongly associated with the quality and durability of the ceramic-cement resin interface. In order to obtain an adequate union between these materials of different nature surface treatments are used and achieve mechanical retention or chemical interaction. Objectives: to check if any method promotes a true chemical bond between lithium disilicate ceramics and resin cement. As well as determineif there is any treatment that reports bonding values comparable to hydrofluoric acid and silane (gold standard). Methods: a systematic literature review was developed based on the PRISMA strategy, where the databases were searched: Science Direct, Pubmed (MEDLINE), EMBASE, Springer Journal, SciELO with MeSH and free terms from 2005 to November 2016 for articles in English and Spanish on surface treatments for lithium disilicate. Results: from 58 publications selected a sample of 21 articles. Two articles reported high risk of bias. Conclusions: hydrofluoric acid and silane continue to be the method with the highest and most reliable adhesion values in the literature. Universal adhesives are an alternative to promote chemical adhesion additional to the silane. Diamond burs, Nd: YAG and Er: YAG laser are not recommended as surface treatments(AU)

Introducción: el éxito clínico de una restauración se asocia fuertemente a la calidad y duración de la interface cerámica-cemento resinoso. Para que exista una adecuada unión entre estos materiales de distinta naturaleza se emplean tratamientos de superficie para lograr una buena retención mecánica o interacción química. Objetivos: revisar si algún método promueve una verdadera adhesión química entre la cerámica de disilicato de litio y el cemento resinoso, así como determinar si existe algún tratamiento que reporte valores de unión comparables al ácido fluorhídrico y silano (patrón de oro). Métodos: se desarrolló una revisión sistemática de literatura basada en la estrategia PRISMA, donde se buscó en las bases de datos: Science Direct, Pubmed (MEDLINE), EMBASE, Springer Journal, SciELO con términos MeSH y libres desde el 2005 a noviembre de 2016 para artículos en inglés y español sobre tratamientos de superficie para disilicato de litio. Resultados: de 58 publicaciones, se seleccionó una muestra de 21 artículos. Dos artículos reportaron riesgo de sesgo alto. Conclusiones: el ácido fluorhídrico y silano continúan siendo el método con los valores de adhesión más altos y confiables de la literatura. Los adhesivos universales son una alternativa para promover adhesión química adicional al silano. Fresas diamantadas, laser Nd: YAG y Er:YAG no se recomienda como tratamientos de superficie(AU)

The effects of sinter temperature on the crystalline phase and microstructural evolution of lithium disilicate glass-ceramic / 实用口腔医学杂志

Objective:To investigate the influence of sinter temperature alteration on the crystalline phase and microstructure of lithium disilicate glass-ceramic.Methods:Samples of lithium disilicate glass-ceramic were heated using the standard two stage heating-schedule at different final temperatures.All samples were observed by X-ray diffractometer (XRD),field emission scanning electron microscope(FESEM) and energy-dispersive X-ray spectroscopy(FE-SEM-EDS) for the evaluation of crystalline phase and microstructural evolution.Results:Crystalline phase and microstructure of ceramic samples showed significant changes during processing at different temperatures,especially at 800 ℃.Samples sintered at 840 ℃ displayed higher crystallinity(P<0.05) and denser microstructure.Conclusion:Temperature control is important in ceramic sintering.800 ℃ and 840 ℃ are the critical temperature points in the crystalline phase and microstructural evolution of lithium disilicate glass-ceramic.

The Effect of Hydrofluoric Acid Concentration and Heat on the Bonding to Lithium Disilicate Glass Ceramic

Abstract The aim of this study was to evaluate the effects of hydrofluoric acid (HF) concentration and previous heat treatment (PHT) on the surface morphology and micro-shear bond strength (mSBS) of a lithium disilicate glass ceramic (EMX) to resin cement. One hundred four EMX specimens were randomly assigned to two groups (n=52) according to the HF concentration: 5% and 10%. A new random distribution was made according to the PHTs (n=13): control (no PHT); previously heated HF (70 °C); previously heated EMX surface (85 °C); the combination of heated HF + heated EMX surface. The etching time was set at 20 s. All EMX blocks were silanated and received a thin layer of an unfilled resin. Five resin cement cylinders were made on each EMX surface using Tygon tubes as matrices, and then stored for 24 h at 37 °C. One random etched EMX sample from each group was analyzed using field-emission scanning electron microscopy (FE-SEM). The data were subjected to two-way ANOVA and multiple comparisons were performed using the Tukey post hoc test (a=0.05). For the control groups, 5% HF showed statistically lower mSBS values when compared to 10% HF (p<0.05). PHT increased the mSBS values for 5% HF, yielding statistically similar results to non-PHT 10% HF (p<0.05). FE-SEM images showed increased glassy matrix removal when PHT was applied to HF 5%, but not to the same degree as for 10% HF. PHT has the potential to improve the bond strength of 5% HF concentration on lithium disilicate glass ceramic.

Resumo O objetivo deste estudo foi avaliar os efeitos das concentrações de ácido fluorídrico (AF) e do prévio tratamento térmico (PTT) na morfologia da superfície e resistência de união ao microcisalhamento (mRUM) de uma cerâmica vítrea de dissilicato de lítio (EMX) ao cimento resinoso. Cento e quatro espécimes de EMX foram aleatoriamente distribuídos em dois grupos (n=52) de acordo com a concentração do AF: 5% e 10%. Os espécimes foram novamente distribuídos de forma aleatória de acordo com o PTT (n=13): controle (sem PTT); AF previamente aquecido (70 °C); superfície do EMX previamente aquecida (85 °C); combinação entre AF e EMX aquecidos. O tempo de condicionamento foi fixado em 20 s. Todos os espécimes de EMX foram silanizados e receberam a aplicação de uma fina camada de um adesivo sem carga. Cinco cilindros de cimento resinoso foram confeccionados usando tubos Tygon como matrizes e então armazenados por 24 h a 37 °C. Uma amostra condicionada de cada grupo foi aleatoriamente selecionada e analisada em um microscópio eletrônico de varredura em emissão de campo (MEVEC). Os dados foram submetidos ao teste ANOVA de dois fatores e múltiplas comparações foram feitas pelo teste de Tukey (a=0.05). Para os grupos controle, AF 5% mostrou valor de mRUM estatisticamente menor do que AF 10% (p<0.05). PTT aumentou os valores de mRUM para o AF 5%, proporcionando resultados estatisticamente similares ao grupo AF 10% controle (p<0.05). MEVEC mostrou um aumento na remoção da matriz vítrea quando o PTT foi aplicado ao grupo AF 5%, no entanto esse efeito não foi visto no grupo AF 10%. O PTT tem o potencial de melhorar a resistência de união do AF 5% na cerâmica vítrea reforçada por disilicato de lítio.

Micromorfología superficial de 2 cerámicas grabables tratadas con diferentes ácidos / Superficial micromorphology of 2 etchable ceramics treated with different acids

Para lograr una unión fuerte entre las restauraciones de cerámica sin metal y las resinas de cementación se indican acondicionamientos de superficie previos a la cementación. Nuestro objetivo es describir y comparar al MEB las superficies de cerámicas feldespáticas y reforzadas con disilicato de litio antes y después de ser tratadas con 2 procedimientos ácidos. Se utilizaron 8 bloques de cerámica feldespática (A) y 8 de cerámica reforzada con disilicato de litio (B). Se subdividieron en 2 grupos de 4 bloques (A1 y A2) y (B1 y B2). Los grupos A1 y B1 fueron tratados con ácido fluorhídrico 9% (HF) y los grupos A2 y B2 con ácido fluorhídrico, seguido de ácido fosfórico al 35%. Posteriormente, se observaron al MEB (1.000 ×) y se procesaron las imágenes con el programa Matlab R2012a, que mide el contraste. Los estadísticos utilizados fueron el test ANOVA y el test «t¼ no pareado Resultados El ácido fluorhídrico 9% crea irregularidades en ambos tipos de cerámicas. Al aplicar HF, seguido de ácido fosfórico sobre la cerámica feldespática no se aprecian diferencias en el contraste, con respecto a utilizar solo HF. Al usar ambos ácidos, en la cerámica reforzada con disilicato de litio se aprecian menos irregularidades respecto a las tratadas con un solo ácido. Conclusiones El ácido fluorhídrico 9% crea microrretenciones en ambas cerámicas. El HF al 9%, seguido del ácido fosfórico 35% parece modificar los valores de contraste de la cerámica colada, en cambio en las feldespáticas no hay diferencias significativas con ambos tratamientos.

Surface conditioning prior to cementing is indicated to achieve a strong bond between metal-free ceramic restorations and resin cements. The aim of this study is to describe and compare the scanning electron microscopy (SEM) images of the surfaces of Feldspathic ceramic and Lithium disilicate glass ceramic before and after being treated with two acid procedures. For this, 8 blocks of Feldspathic ceramic (A) and 8 of Ceramic lithium disilicate (B) were used. They were subdivided into two groups of 4 blocks (A1 and A2) and (B1 and B2). Groups A1 and B1 were treated with 9% Hydrofluoric Acid (HF) and the A2 and B2 groups, with 9% Hydrofluoric Acid followed by 35% Phosphoric Acid. Subsequently, they were observed using SEM (1,000 ×) and the images processed with the program Matlab R2012a, which measures the contrast. The statistics used were ANOVA test and the unpaired t test. Results 9% Hydrofluoric Acid creates irregularities in both types of ceramics. When applying HF followed by Phosphoric Acid on Feldspathic ceramics, no differences in contrast were found, compared to using only HF. With ceramic lithium disilicate using both acids, there are fewer irregularities with respect to those treated with a single acid. Conclusion 9% Hydrofluoric Acid creates micro-retentions in both ceramics. 9% HF followed by 35% Phosphoric Acid appears to significantly modify the Lithium disilicate glass ceramic contrast values. On the other hand, the Feldspathic ceramic showed no significant differences with both treatments.

Evaluation of marginal fit of 2 CAD-CAM anatomic contour zirconia crown systems and lithium disilicate glass-ceramic crown

PURPOSE: This study was to evaluate the marginal fit of two CAD-CAM anatomic contour zirconia crown systems compared to lithium disilicate glass-ceramic crowns. MATERIALS AND METHODS: Shoulder and deep chamfer margin were formed on each acrylic resin tooth model of a maxillary first premolar. Two CAD-CAM systems (Prettau(R)Zirconia and ZENOSTAR(R)ZR translucent) and lithium disilicate glass ceramic (IPS e.max(R)press) crowns were made (n=16). Each crown was bonded to stone dies with resin cement (Rely X Unicem). Marginal gap and absolute marginal discrepancy of crowns were measured using a light microscope equipped with a digital camera (Leica DFC295) magnified by a factor of 100. Two-way analysis of variance (ANOVA) and post-hoc Tukey's HSD test were conducted to analyze the significance of crown marginal fit regarding the finish line configuration and the fabrication system. RESULTS: The mean marginal gap of lithium disilicate glass ceramic crowns (IPS e.max(R)press) was significantly lower than that of the CAD-CAM anatomic contour zirconia crown system (Prettau(R)Zirconia) (P<.05). Both fabrication systems and finish line configurations significantly influenced the absolute marginal discrepancy (P<.05). CONCLUSION: The lithium disilicate glass ceramic crown (IPS e.max(R)press) had significantly smaller marginal gap than the CAD-CAM anatomic contour zirconia crown system (Prettau(R)Zirconia). In terms of absolute marginal discrepancy, the CAD-CAM anatomic contour zirconia crown system (ZENOSTAR(R)ZR translucent) had under-extended margin, whereas the CAD-CAM anatomic contour zirconia crown system (Prettau(R)Zirconia) and lithium disilicate glass ceramic crowns (IPS e.max(R)press) had overextended margins.

Flexural strength and microstructure of two lithium disilicate glass ceramics for CAD/CAM restoration in the dental clinic

OBJECTIVES: There has been a growing interest in glass ceramic systems with good esthetics, high fracture resistance and bonding durability, and simplified fabrication techniques using CAD/CAM. The aim of this study is to compare flexural strength before and after heat treatment of two lithium disilicate CAD/CAM blocks, IPS e.max CAD (Ivoclar Vivadent) and Rosetta SM (Hass), and to observe their crystalline structures. MATERIALS AND METHODS: Biaxial flexural strength was tested according to ISO 6872 with 20 disc form specimens sliced from each block before and after heat treatment. Also, the crystalline structures were observed using field-emission scanning microscopy (FE-SEM, Hitachi) and x-ray diffraction (XRD, Rigaku) analysis. The mean values of the biaxial flexural strength were analyzed by the Mann-Whitney U test at a significance level of p = 0.05. RESULTS: There were no statistically significant differences in flexural strength between IPS e.max CAD and Rosetta SM either before heat treatment or after heat treatment. For both ceramics, the initial flexural strength greatly increased after heat treatment, with significant differences (p < 0.05). The FE-SEM images presented similar patterns of crystalline structure in the two ceramics. In the XRD analysis, they also had similar patterns, presenting high peak positions corresponding to the standard lithium metasilicate and lithium disilicate at each stage of heat treatment. CONCLUSIONS: IPS e.max CAD and Rosetta SM showed no significant differences in flexural strength. They had a similar crystalline pattern and molecular composition.

Effect of hydrofluoric acid etching duration on the roughness and flexural strength of a lithium disilicate-based glass ceramic

The aim of this study was to examine the effect of different acid etching times on the surface roughness and flexural strength of a lithium disilicate-based glass ceramic. Ceramic bar-shaped specimens (16 mm x 2 mm x 2 mm) were produced from ceramic blocks. All specimens were polished and sonically cleaned in distilled water. Specimens were randomly divided into 5 groups (n=15). Group A (control) no treatment. Groups B-E were etched with 4.9 percent hydrofluoric acid (HF) for 4 different etching periods: 20 s, 60 s, 90 s and 180 s, respectively. Etched surfaces were observed under scanning electron microscopy. Surface profilometry was used to examine the roughness of the etched ceramic surfaces, and the specimens were loaded to failure using a 3-point bending test to determine the flexural strength. Data were analyzed using one-way ANOVA and Tukey's test (?=0.05). All etching periods produced significantly rougher surfaces than the control group (p<0.05). Roughness values increased with the increase of the etching time. The mean flexural strength values were (MPa): A=417 ± 55; B=367 ± 68; C=363 ± 84; D=329 ± 70; and E=314 ± 62. HF etching significantly reduced the mean flexural strength as the etching time increased (p=0.003). In conclusion, the findings of this study showed that the increase of HF etching time affected the surface roughness and the flexural strength of a lithium disilicate-based glass ceramic, confirming the study hypothesis.

O objetivo deste estudo foi avaliar o efeito de diferentes tempos de condicionamento ácido na rugosidade de superfície e resistência flexural de uma cerâmica à base de disilicato de lítio. Espécimes cerâmicos em forma de barra (16 mm x 2 mm x 2 mm) foram produzidos a partir de blocos cerâmicos. Todos os espécimes foram polidos e limpos em banho de ultrasom em água destilada. Os espécimes foram aleatoriamente divididos em 5 grupos (n=15). Grupo A (controle) sem tratamento. Grupos B-E condicionamento com ácido fluorídrico 4,9 por cento (HF) por 4 diferentes períodos de condicionamento: 20 s, 60 s, 90 s e 180 s, respectivamente. As superfícies condicionadas foram observadas sob microscopia eletrônica de varredura. Perfilometria de superfície foi utilizada para examinar a rugosidade das superfícies condicionadas, e os espécimes foram carregados até a falha pelo teste de flexão três pontos. Os valores foram analisados usando ANOVA um fator e teste de Tukey (?=0,05). Todos os períodos de condicionamento produziram superfícies significantemente mais rugosas do que o grupo controle (p<0,05). Os valores de rugosidade aumentaram com o tempo de condicionamento. Os valores médios de resistência à flexão foram (MPa): A=417 ± 55; B=367 ± 68; C=363 ± 84; D=329 ± 70; e E=314 ± 62. O condicionamento com HF reduziu significativamente os valores médios de resistência à flexão conforme o tempo de condicionamento aumentou (p=0,003). Os achados deste estudo mostraram que o aumento do tempo de condicionamento ácido influenciou a rugosidade de superfície e resistência flexural de uma cerâmica à base de disilicato de lítio confirmando a hipótese do mesmo.

FLEXURE STRENGTH AND MICROSTRUCTURE OF IPS EMPRESS 2 GLASS-CERAMIC ON HEAT PRESSING AND HEAT TREATMENTS / 대한치과보철학회지

This investigation was designed to determine whether heat-pressing and/or simulated heat treatments affected the flexure strength and the microstructure of the lithium disilicate glassceramic in the IPS Empress 2 system. Four groups of the specimens were prepared as follows group 1 - as-received material ; group 2 - heat-pressed material ; group 3 - heat pressed and simulated initial heat-treated material ; group 4 - heat-pressed and the simulated heat-treated material with full firings for a final restoration. The three-point bending test and the scanning electron microscope (SEM) analysis was conducted for the purpose of this study. The flexure strength of group. 2 was significantly higher than that of group 1. However, there were no significant differences in strength among group 2, 3, and 4, and between group 1 and 4. The SEM micrographs of the lithium disilicate glass-ceramic showed the closely packed, multi-directionally interlocking microstructure of numerous lithium disilicate crystals protruding from the glass matrix. The crystals of the heat-pressed materials (group 2, 3, and.4) were a little denser and about two times bigger than those of the as-received material (group 1). This change of microstructure is more obviously exhibited particularly between group 1 and 2. However, there was no a marked difference among group 2, 3, and 4 after the heat pressing procedure. Although there were significant increase of the strength and some changes of the microstructure after the heat-pressing operation, the conr bination of the heat-pressing and the simulated subsequent heat treatments did not produce the increase of strength of IPS Empress 2 glass-ceramic.