Recycling CAD/CAM lithium disilicate ceramic: effect of surface treatment and aging on the bond strength to resin cement.

PURPOSE: To investigate the effect of recycling of lithium disilicate (LD), surface treatment and thermocycling (TC) on the bond strength (SBS) to resin cement. MATERIALS AND METHODS: Blocks of LD were made according to the recycling cycle, with 24 blocks for each strategy: Control-conventional sintering; 1R (1 recycling cycle) and 3R (3 recycling cycles). For the recycling groups, blocks were waxed (10x10x3mm), mounted in a silicone ring, poured with investment material, and then residues of sintered LD blocks were pressed by the lost wax technique. The residual LD was reused as described until reach 3R. Afterwards, the blocks were embedded in acrylic resin, sanded and divided (n=15) according to the factors "surface treatment" (HF20s+Silane and HF120s+Silane and Monobond Etch&Prime- MEP) and TC (with/10.000 cycles and without). After surface treatment, cylinders (Ø:2mm) of resin cement were made and submitted to SBS test (100KgF,1mm/min). Data (MPa) were analyzed by 3-way ANOVA, Tukey's test (5%) and Weibull analysis. Failure analysis was performed with stereomicroscope. RESULTS: ANOVA revealed that all factors were significant (P=.000*). The group 3RMEP(105.09±19.49) presented the highest SBS among the experimental groups. 1RHF20sTc(7.50±1.97) group had the lowest SBS, similar to the CHF20sTc(15.69±3.77), 1RHF20s(15.12±3.03), 1RHF120sTc(14.60±3.43) and 3RHF20sTc(15.65±0.97). The Weibull modulus and characteristic strength varied among the experimental groups (P=0.0). Failure analysis revealed adhesive and mixed types. CONCLUSION: The recycling of DL ceramics increases the SBS to resin cement when the ceramic is treated with HF120s+S or MEP.

Preheated Composite as an Alternative for Bonding Feldspathic and Hybrid Ceramics: A Microshear Bond Strength Study.

PURPOSE: To evaluate the bond strength between alternative or conventional luting agents and indirect restorative materials. MATERIALS AND METHODS: Blocks of a polymer-infiltrated ceramic network (PICN, Vita Enamic) and a feldspathic ceramic (FEL, Vita Mark II) were sliced and divided according to the luting agent: resin cement (PICN-RC, FEL-RC), flowable composite (PICN-FC, FEL-FC), or preheated composite (PICN-PH, FEL-PH). The ceramic surfaces were polished, etched with 5% hydrofluoric acid for 60 s, and then a silane layer was applied. Cylinders of the luting agents were built up on the ceramic surfaces. In half the samples, the microshear bond strength (µSBS) was tested after 24 h (baseline). The other half was tested after 5000 thermocycles (5°C-55°C) (aging). The failure modes were determined using a stereomicroscope, and the ceramic surfaces were analyzed using a scanning electron microscope. Data were statistically analyzed with two-way ANOVA. RESULTS: Thermocycling reduced the bond strength values of all experimental groups. Regarding FEL, the preheated composite obtained the highest results. Resin cement showed results similar to the flowable composite at baseline and after aging. The highest results of PICN were obtained from the preheated composite followed by resin cement and flowable composite. Significant differences among the three luting agents were observed before and after aging. The most frequent failures among the experimental groups were adhesive and cohesive in the ceramic. CONCLUSION: Bond strength results indicate that the preheated composite can be an alternative for adhesive cementation when applied on the tested feldspathic ceramic or PICN.

Efeito do envelhecimento hidrotérmico na resistência ao desgaste, topografia superficial, microdureza e tenacidade à fratura de diferentes zircônias / Effect of hydrothermal aging on wear resistance, surface topography, microhardness and fracture toughness of different zirconias

Este estudo propôs avaliar o efeito do envelhecimento hidrotérmico no padrão de desgaste, topografia superficial, microdureza, tenacidade à fratura e composição cristalina das zircônias 3Y-TZP, 5Y-PSZ e multicamadas. Para isso, foram utilizadas as zircônias 3Y-TZP - Zpex e 5Y-TZP - Zpex Smile (Tosoh Corporation) para confecção de discos (Ø= 12 mm e 1,2 mm de espessura) e a ZirCAD Prime (Ivoclar Vivadent) para confecção de blocos (14 x 14 x 1,5 mm). Os espécimes foram divididos em 6 grupos (n=18) entre os fatores "tipo de zircônia" (3Y-TZP, 5Y-TZP e multicamadas) e "envelhecimento hidrotérmico" (com e sem). Exceto para os grupos controle, as amostras passaram por envelhecimento em reator hidrotérmico (134◦C, 20 horas, 2,2 bar). As amostras (n=10) foram submetidas ao desgaste por deslizamento horizontal de 2 mm, com esferas de zircônia 3Y-TZP como antagonistas (150N, 4Hz, 600.000 ciclos). O volume do desgaste e os parâmetros de rugosidade foram quantificados em perfilômetro de contato. A altura do desgaste dos antagonistas foi determinada em estereomicroscópio óptico. Foram realizadas a análise de difração de raios-X, espectroscopia Raman e microscopia eletrônica de varredura para cada grupo experimental, bem como microdureza Vickers e tenacidade à fratura. Os dados de volume de desgaste, altura dos antagonistas e rugosidade foram analisados estatisticamente por meio do ANOVA on Ranks e teste de Dunn. Os dados de microdureza e tenacidade à fratura foram analisados estatisticamente por meio do ANOVA 2 fatores e Tukey 5%. Os dados das análises de difração de raios-X e microscopia eletrônica de varredura foram submetidos à análise qualitativa. Com os resultados obtidos, foi possível observar que o envelhecimento hidrotérmico afetou o desgaste apenas para as zircônias 3Y-TZP e multicamadas, tendo o grupo 3Y-TZP com envelhecimento o maior volume de desgaste, semelhante estatisticamente à zircônia multicamadas com envelhecimento. Para os parâmetros de rugosidade, o fator "envelhecimento" foi significativo apenas para o parâmetro Ra. O envelhecimento hidrotérmico afetou a dureza e tenacidade à fratura para a zircônia 3Y-TZP e para as diferentes camadas da zircônia multicamadas. As análises microestruturais indicaram que a fase monoclínica é mais sujeita ao desgaste e o envelhecimento hidrotérmico causou mudança de fase para 3Y-TZP. O MEV mostrou que o envelhecimento hidrotérmico causou arrancamento de grãos e desgaste em camadas para a zircônia 3Y-TZP e superfícies mais irregulares e rugosas para a zircônia 5Y-PSZ e multicamadas. Desse modo, podemos concluir que o envelhecimento hidrotérmico aumenta o desgaste para as zircônias 3Y-TZP e multicamadas e produz transformação de fase, sendo a camada monoclínica mais sujeita ao desgaste. Além disso, o envelhecimento hidrotérmico não alterou a incidência do desgaste para a zircônia 5Y-PSZ, mas produziu alterações superficiais vistas por micrografias (AU)

This study aimed to evaluate the effect of hydrothermal aging on the wear pattern, surface topography, microhardness, fracture toughness and crystalline composition of 3Y-TZP, 5YPSZ and multilayer zirconia. 3Y-TZP - Zpex and 5Y-TZP - Zpex Smile (Tosoh Corporation, Japão) were used to fabricate discs (Ø= 12 mm x 1,2 mm) and ZirCAD Prime (Ivoclar Vivadent, Liechtenstein) to fabricate blocks (14 mm x 14 mm x 1,5 mm). The specimens were divided into 6 groups (n=18) according to the following factors "type of zirconia" (3Y-TZP, 5Y-TZP e multilayers) and "hydrothermal aging" (with and without). Except for the control groups, the samples aged in hydrothermal reactor (134◦C, 20 horas, 2,2 bar). The samples were subjected to wear through cyclic load (150N, 4Hz, 600.000 cycles) with horizontal sliding of 2 mm (n=10) under distilled water, using 3Y-TZP zirconia spheres (Ø= 6mm) as antagonist. The wear volume and roughness parameters were quantified using a contact profilometer. The height of the wear of the antagonists was determined by stereomicroscope. X-rays diffraction analysis, Raman spectroscopy, and scanning electron microscopy were performed for each experimental group, along with fracture toughness and Vickers microhardness measurements. The data of the wear volume and roughness were analyzed statistically by ANOVA on Ranks and Dunn test. The microhardness and fracture toughness data were statistically analyzed by two-way ANOVA and Tukey test (α=0.05). The data of X-rays diffraction analysis and electronic microscope were subjected to the descriptive analysis. The results showed that hydrothermal aging affected the wear of only 3Y-TZP and multilayers zirconia. The 3Y-TZP group with aging had the highest wear volume; however, it was statistically similar to the wear observed in the multilayer zirconia with aging. Regarding the wear of the antagonist, there was no statistical difference between the groups. For the roughness parameters, the "aging" factor was significant only for the Ra parameter. The hydrothermal aging affected the hardness and fracture toughness for 3Y-TZP zirconia and the different layers of zirconia multilayers. The microstructure analyses indicated that the monoclinic phase is more susceptible to wear, and hydrothermal aging caused phase transformation on 3Y-TZP. The scanning electron microscope showed that hydrothermal aging caused grain detachment in 3Y-TZP, resulting in layered wear. For the 5Y-PSZ and multilayers zirconia, the aging caused more irregular and rougher surface. Thus, we can conclude that the hydrothermal aging increases wear in 3-TZP and multilayers zirconia, leading to a phase transformation and formation of a monoclinic layer that is more susceptible to wear. Furthermore, the hydrothermal aging did not alter the incidence of wear for 5Y-PSZ zirconia, but it caused surface alterations seen by micrograph. (AU)

Biaxial flexure strength and physicochemical characterization of a CAD/CAM lithium disilicate ceramic: effect of etching time, silane, and adhesive applications.

OBJECTIVE: To evaluate the effect of different acid etching time and bonding agent (silane and/or adhesive system) on biaxial flexural strength and physico-chemical properties of a lithium disilicate ceramic. MATERIAL AND METHODS: One hundred twenty ceramic discs were made and divided into 8 groups (n = 15) according to factors "etching time" (20 and 120 s) with hydrofluoric acid (HF) and "bonding agent" (C, no bonding agent; S, silane, A, adhesive; and SA, silane + adhesive). After surface treatment, a resin cement layer was applied to the surface and all specimens were subjected to biaxial flexural strength (BFS) test with treated surfaces loaded in tension (1 mm/min). The Weibull analyses and complementary analyses were also performed. Statistical analysis was done with 2-way ANOVA and the Tukey test (α = 0.05). RESULTS: ANOVA revealed that the factors "etching time" (p = 0.0003) and "bonding agent" (p = 0.007) were statistically significant. In the overall analysis, the HF120S group (272.02 ± 35.30A MPa) presented significantly higher BFS than that of HF120C (218.45 ± 17.15CD MPa) and HF20S (228.40 ± 37.83BCDMPa). On the other hand, the HF20A group (208.92 ± 31.16D MPa) had significantly lower BFS than HF120S (272.02 ± 35.30A), HF120A (254.42 ± 26.87ABC) and HF120SA (259.30 ± 36.55AB) groups (Tukey). The Weibull modulus (m) of all groups was significantly different from each other (p = 0.000). CONCLUSIONS: Regardless of etching time, the application of silane alone is sufficient to increase the flexural strength of glass ceramic, eliminating the need for the application of adhesive systems. Moreover, if only silane or adhesive is applied, 120-s HF application should increase the flexural resistance of the lithium disilicate ceramic. CLINICAL SIGNIFICANCE: Applications of adhesive systems after silanization can be suppressed from the surface treatment protocol of glass ceramics, since it does not improve their mechanical strength.

CAD-FEA modeling and fracture resistance of bilayer zirconia crowns manufactured by the rapid layer technology.

In the RLT (Rapid Layer Technology), veneering ceramic and framework are fabricated by computer-aided design/computer-aided manufacturing (CAD/CAM) and then cemented to obtain the restoration. This study aimed to evaluate the effect of the thickness of veneering ceramic manufactured by the RLT technique on the fracture resistance (FR) of bilayer crowns with zirconia frameworks. Twenty zirconia frameworks and twenty feldspathic posterior crowns with two different veneering ceramic occlusal thicknesses (1mm=TF1; 2mm=TF2) were manufactured using CAD/CAM system. The specimens were luted to an epoxy resin abutment with resin cement and mechanically cycled (200N and 4.5×105 Pa, 37°C, 2×106 cycles, 3Hz). The FR test was performed (10kN, 0.5mm/min), and the specimens were analyzed in a stereomicroscope. For the stress analysis (finite element analysis, FEA), a 10kN load was equal to the in vitro test, and the principal stress was evaluated. The FR data were analyzed by Student's t-test and Weibull's analysis. The thickness influenced the FR of bilayer crowns. The FR was higher in the TF2 than in the TF1 group. The TF2 group presented the highest characteristic strength compared to the group TF1. The predominant type of failure was delamination. The FEA showed higher stress concentrations below the loading application point at the veneering cement interface in the 1-mm-thick model. The bilayer crowns manufactured using the approach of 2mm of veneering ceramic promoted higher FR compared to the group with 1mm veneering ceramic. Also, the FEA showed that the veneer ceramic thickness has an effect on stress distribution in zirconia-based bilayer crowns.

CAD-FEA modeling and fracture resistance of bilayer zirconia crowns manufactured by the rapid layer technology

Abstract In the RLT (Rapid Layer Technology), veneering ceramic and framework are fabricated by computer-aided design/computer-aided manufacturing (CAD/CAM) and then cemented to obtain the restoration. This study aimed to evaluate the effect of the thickness of veneering ceramic manufactured by the RLT technique on the fracture resistance (FR) of bilayer crowns with zirconia frameworks. Twenty zirconia frameworks and twenty feldspathic posterior crowns with two different veneering ceramic occlusal thicknesses (1mm=TF1; 2mm=TF2) were manufactured using CAD/CAM system. The specimens were luted to an epoxy resin abutment with resin cement and mechanically cycled (200N and 4.5×105 Pa, 37°C, 2×106 cycles, 3Hz). The FR test was performed (10kN, 0.5mm/min), and the specimens were analyzed in a stereomicroscope. For the stress analysis (finite element analysis, FEA), a 10kN load was equal to the in vitro test, and the principal stress was evaluated. The FR data were analyzed by Student's t-test and Weibull's analysis. The thickness influenced the FR of bilayer crowns. The FR was higher in the TF2 than in the TF1 group. The TF2 group presented the highest characteristic strength compared to the group TF1. The predominant type of failure was delamination. The FEA showed higher stress concentrations below the loading application point at the veneering cement interface in the 1-mm-thick model. The bilayer crowns manufactured using the approach of 2mm of veneering ceramic promoted higher FR compared to the group with 1mm veneering ceramic. Also, the FEA showed that the veneer ceramic thickness has an effect on stress distribution in zirconia-based bilayer crowns.

Resumo Na RLT (Rapid Layer Technology), a cerâmica de cobertura e infraestrutura são fabricados pelo Computer-Aided Design / Computer-Aided Manufacturing (CAD / CAM) e cimentados para obter a restauração. Este estudo teve como objetivo avaliar o efeito da espessura da cerâmica de cobertura fabricada pela técnica RLT na resistência à fratura (RF) de coroas bilaminadas com infraestrutura de zircônia. Vinte infraestruturas de zircônia e vinte coroas posteriores feldspáticas com duas espessuras oclusais da cerâmica de cobertura (1mm = TF1; 2mm = TF2) foram fabricadas usando o sistema CAD / CAM. Os espécimes foram cimentados em preparos de resina epóxi com cimento resinoso dual e ciclados mecanicamente (200N e 4,5×105 Pa, 37° C, 2×106 ciclos, 3Hz). O teste de RF foi realizado (10kN, 0,5mm / min) e, posteriormente, os espécimes foram analisados em estereomicroscópio. Para a análise de tensão (análise de elementos finitos, FEA), uma carga de 10kN foi aplicada igual ao teste in vitro, e a tensão principal foi avaliada. Os dados de RF foram analisados pelo teste t de Student e análise de Weibull. A espessura mostrou forte influência na RF das coroas bilaminadas. A RF foi maior em TF2 do que no grupo TF1. O grupo TF2 apresentou a maior resistência característica em relação ao grupo TF1. O tipo de falha predominante foi a delaminação. O FEA mostrou maiores concentrações de tensões abaixo do ponto de aplicação da carga, na interface cimento e cerâmica de cobertura no modelo de coroa de 1 mm de espessura. As coroas de bilaminadas confeccionadas com 2 mm de cerâmica de cobertura promoveram maior RF em comparação ao grupo com cerâmica de cobertura de 1 mm. Além disso, a FEA mostrou que a espessura da cerâmica de cobertura tem um efeito na distribuição de tensões em coroas bilaminadas à base de zircônia.

Effect of different surface treatments and multimode adhesive application on the Weibull characteristics, wettability, surface topography and adhesion to CAD/CAM lithium disilicate ceramic.

METHODOLOGY: This paper aims to evaluate the effect of different surface treatments on surface topography, wettability, and shear bond strength of resin cement to glass ceramic. For SBS test, 32 blocks (7x7x2 mm) of lithium disilicate were obtained and randomly divided into eight groups (four blocks per group) according to each surface treatment (HF 20 s, 60 s, 120 s + silanization/S or Scotch Bond Universal/ SBU) and the Monobond Etch & Prime - MEP application followed or not by SBU. On each treated surface ceramic block, up to four dual-curing resin cement cylinders were prepared and light-cured for 40s (N=120/n=15). The specimens were thermocycled (10,000 cycles, 5-55°C, 30 s) and the SBS test (50KgF, 0.5 mm/min) was performed. Furthermore, failure analysis, wettability, AFM, and SEM were carried out. SBS data (MPa) were analyzed using Student's t-test, two-way ANOVA, Tukey's test (5%) and Weibull's analysis. RESULTS: For HF experimental groups, two-way ANOVA presented the factors "etching time" and "bonding agent" as significant (p<0.05). After silane application, the HF groups presented similar bond strength. SBU application compromised the SBS, except for 120s etching time (HF120sS: 23.39ᵃ±6.48 MPa; HF120sSBU: 18.76ᵃ±8.81MPa). For MEP groups, SBU application did not significantly affect the results (p=0.41). The MEP group presented the highest Weibull modulus (4.08A) and they were statistically different exclusively from the HF20sSBU (0.58B). CONCLUSION: The HF 20s, 60s, 120 s followed by silane, promoted similar resin-bond strength to ceramic and the SBU application after HF or MEP did not increase the SBS.

Hydrofluoric acid concentration, time and use of phosphoric acid on the bond strength of feldspathic ceramics.

The objective of this study was to evaluate the influence of hydrofluoric acid (HF) concentration, etching time, and application of phosphoric acid (PA) followed by neutralization with sodium bicarbonate on the bond strength between a feldspar ceramic and resin cement. Thus, 80 blocks (10 x 12 x 2 mm) of glass ceramic (VM - Vita Mark II - Vita Zahnfabrik) were made and randomly assigned to eight groups (n = 10) according to the factors: HF concentration (5 and 10%), etching time (60 and 120 s), and use of phosphoric acid (PA) (with and without). According to the experimental group, 37% PA (Condac, FGM) was applied after HF etching for 60s. Afterwards, samples were immersed in sodium bicarbonate for 1 min then in an ultrasonic bath in distilled water (5 min) for cleaning. After surface bonding treatment, cylinders (Ø = 2 mm; h = 2 mm) of dual resin cement (AllCem / FGM) were made in the center of each block. The samples were then stored in water (37ºC) for 90 days and submitted to the shear bond test (50 KgF, 1 mm/min). Failure analysis was performed by stereomicroscope and scanning electron microscopy. Data (MPa) were analyzed with 3-way ANOVA and Tukey's test. Only the factor "HF concentration" was significant (p = 0.02). Most failures were of cohesive in ceramic (40%) and mixed types (42.5%). The 10% HF resulted in higher shear bond strength value than the 5% HF. Surface cleaning with phosphoric acid followed by sodium bicarbonate and HF time (60 or 120 seconds) did not influence the resin bond strength to feldspar ceramic.

Effect of different surface treatments and multimode adhesive application on the Weibull characteristics, wettability, surface topography and adhesion to CAD/CAM lithium disilicate ceramic

Abstract This paper aims to evaluate the effect of different surface treatments on surface topography, wettability, and shear bond strength of resin cement to glass ceramic. Methodology: For SBS test, 32 blocks (7x7x2 mm) of lithium disilicate were obtained and randomly divided into eight groups (four blocks per group) according to each surface treatment (HF 20 s, 60 s, 120 s + silanization/S or Scotch Bond Universal/ SBU) and the Monobond Etch & Prime - MEP application followed or not by SBU. On each treated surface ceramic block, up to four dual-curing resin cement cylinders were prepared and light-cured for 40s (N=120/n=15). The specimens were thermocycled (10,000 cycles, 5-55°C, 30 s) and the SBS test (50KgF, 0.5 mm/min) was performed. Furthermore, failure analysis, wettability, AFM, and SEM were carried out. SBS data (MPa) were analyzed using Student's t-test, two-way ANOVA, Tukey's test (5%) and Weibull's analysis. Results: For HF experimental groups, two-way ANOVA presented the factors "etching time" and "bonding agent" as significant (p<0.05). After silane application, the HF groups presented similar bond strength. SBU application compromised the SBS, except for 120s etching time (HF120sS: 23.39ᵃ±6.48 MPa; HF120sSBU: 18.76ᵃ±8.81MPa). For MEP groups, SBU application did not significantly affect the results (p=0.41). The MEP group presented the highest Weibull modulus (4.08A) and they were statistically different exclusively from the HF20sSBU (0.58B). Conclusion: The HF 20s, 60s, 120 s followed by silane, promoted similar resin-bond strength to ceramic and the SBU application after HF or MEP did not increase the SBS.

Hydrofluoric acid concentration, time and use of phosphoric acid on the bond strength of feldspathic ceramics

Abstract The objective of this study was to evaluate the influence of hydrofluoric acid (HF) concentration, etching time, and application of phosphoric acid (PA) followed by neutralization with sodium bicarbonate on the bond strength between a feldspar ceramic and resin cement. Thus, 80 blocks (10 x 12 x 2 mm) of glass ceramic (VM - Vita Mark II - Vita Zahnfabrik) were made and randomly assigned to eight groups (n = 10) according to the factors: HF concentration (5 and 10%), etching time (60 and 120 s), and use of phosphoric acid (PA) (with and without). According to the experimental group, 37% PA (Condac, FGM) was applied after HF etching for 60s. Afterwards, samples were immersed in sodium bicarbonate for 1 min then in an ultrasonic bath in distilled water (5 min) for cleaning. After surface bonding treatment, cylinders (Ø = 2 mm; h = 2 mm) of dual resin cement (AllCem / FGM) were made in the center of each block. The samples were then stored in water (37ºC) for 90 days and submitted to the shear bond test (50 KgF, 1 mm/min). Failure analysis was performed by stereomicroscope and scanning electron microscopy. Data (MPa) were analyzed with 3-way ANOVA and Tukey's test. Only the factor "HF concentration" was significant (p = 0.02). Most failures were of cohesive in ceramic (40%) and mixed types (42.5%). The 10% HF resulted in higher shear bond strength value than the 5% HF. Surface cleaning with phosphoric acid followed by sodium bicarbonate and HF time (60 or 120 seconds) did not influence the resin bond strength to feldspar ceramic.