Simulation of CAD/CAM milling on lithium disilicate: Mechanical and topographic analyses of surface grinding different protocols.

The aim of this study was to evaluate the topography and the fatigue performance of lithium disilicate glass-ceramic after surface grinding through different laboratory protocols used to simulate the Computer-aided design/Computer-aided manufacturing (CAD/CAM) milling. Ceramic discs (IPS e.max CAD, Ø = 13.5 mm × 1.2 mm of thickness) were produced through different methodologies: milling in CAD/CAM system (CAD/CAM group); produced in-lab with a polished surface (POL group); or produced through in-lab methods and randomly distributed into five groups according to different grinding protocols to simulate the CAD/CAM milling [grinding with a CAD/CAM bur coupled to a mandrel (CAD/CAM Bur group); fine diamond bur using oscillatory movements (DBO group); fine diamond bur in x and y axes of the disc (DBXY group); #60-grit silicon carbide sandpaper (SiC group); and #60-grit wood sandpaper (WS group)]. The specimens were fatigue tested (n = 15) according to the step-stress method (initial load: 60 N; step-size: 20 N; 10,000 cycles/step; 20 Hz frequency). A roughness analysis was performed on all specimens, while fractal dimension (FD) and fractography were performed on representative samples. The Kaplan-Meier analysis showed that the POL (293.3 N) group presented better fatigue performance (higher load and number of cycles for failure) (p < 0.05) than the other groups (CAD/CAM = 222.7 N; CAD/CAM Bur = 181.3 N; DBO = 184.0 N; DBXY = 192.0 N; SiC = 182.6 N; WS = 182.6 N). For roughness, only the SiC (Ra = 1.616; Rz = 10.465) and WS (Ra = 1.673; Rz = 10.655) groups produced statistically similar Ra (µm) and Rz (µm) values to the CAD/CAM (Ra = 1.628; Rz = 9.571) group (p > 0.05). The surface created by CAD/CAM milling and POL group exhibited more complexity (FD) higher values than the experimental groups. For the ceramic surface topography images, the CAD/CAM milling visibly produced a uniform surface compared to the other groups; however, the POL group was the smoothest. The DBO, DBXY, SiC, and WS groups resulted in similar characteristics of surface topography. Therefore, although the SiC and WS groups showed similar roughness to the control group (CAD/CAM), no in-lab simulation method was fully capable to mimic the mechanical performance of the CAD/CAM-milled lithium disilicate glass-ceramic.

Effect of immediate dentin sealing and temporary cement removal on bond strength of resin cements to dentin / Efeito do selamento dentinário imediato e da remoção do cimento provisório na resistência de união de cimentos resinosos à dentina

Objective: To evaluate the influence of immediate dentin sealing (IDS) and mechanical methods for removing the temporary cement on the bond strength between dentin and resin cements. Material and Methods: Bovine incisors were ground until dentin exposure and divided according to two factors: "dentin surface treatment"' - cleaning with manual dental excavator (DE), with Robinson bristle brush and pumice paste (PP) or IDS application with Single Bond 2 (IDS/SB+PP) or Single Bond Universal (IDS/SBU+PP) plus cleaning with PP; and "resin cement" - Self-adhesive (RelyX U200) or conventional cement with self-etching adhesive (Multilink Automix). Simulating provisional restoration, acrylic resin plates were cemented onto the dentin surface (with or without IDS) with a non-eugenol temporary cement, and stored in distilled water (37 ºC; 7 days). The acrylic plates were removed, the dentin surface was cleaned (PP or DE), and starch tubes were positioned on the dentin where the resin cements were applied. After 24 h, the specimens were submitted to a microshear test (wire-loop method). Results: Two-way analysis of variance showed statistically significant influence of dentine surface treatments (p< 0.001) and resin cement (p= 0.001) in the bond strength values. The IDS/SBU+PP/U200 (7.24 MPa) and IDS/SBU+PP/MULTI (6.40 MPa) groups presented higher values when compared to cleaning with DE (DE/U200= 4.60 MPa; DE/MULTI= 1.45 MPa) and PP (PP/U200= 3.74 MPa; PP/MULTI= 3.14 MPa). Statistical difference was also found between the cements when dental excavator treatment was used (RelyX U200 ˃ Multilink Automix). The IDS/SBU+PP protocol presented a higher percentage of cohesive failures. The micrographs showed differences in dentin surface characteristics among the groups. Conclusion: Immediate dentin sealing increased the bond strength of the resin cements to dentin compared to mechanical cleaning only, regardless the resin cement. (AU)

Objetivo: Avaliar a influência do selamento dentinário imediato (IDS) e dos métodos mecânicos de remoção do cimento provisório na resistência de união entre dentina e cimentos resinosos. Materiais e Métodos: Incisivos bovinos foram desgastados até a exposição da dentina e divididos de acordo com dois fatores: "tratamento da superfície dentinária" - limpeza com cureta dentária manual (DE), com escova de cerdas Robinson e pasta de pedra-pomes (PP) ou aplicação de IDS com Single Bond 2 (IDS/SB +PP) ou Single Bond Universal (IDS/SBU+PP) mais limpeza com PP; e "cimento resinoso" - autoadesivo (RelyX U200) ou cimento convencional com adesivo autocondicionante (Multilink Automix). Simulando a restauração provisória, placas de resina acrílica foram cimentadas na superfície dentinária (com ou sem IDS) com um cimento provisório sem eugenol e armazenadas em água destilada (37 ºC; 7 dias). As placas de acrílico foram removidas, a superfície dentinária foi limpa (PP ou DE) e tubos de amido foram posicionados na dentina onde os cimentos resinosos foram aplicados. Após 24 h, os corpos-de-prova foram submetidos ao ensaio de microcisalhamento (método wire-loop). Resultados: A análise de variância de dois fatores mostrou influência estatisticamente significativa dos tratamentos de superfície dentinária (p< 0,001) e cimento resinoso (p= 0,001) nos valores de resistência de união. Os grupos IDS/SBU+PP/U200 (7,24 MPa) e IDS/SBU+PP/MULTI (6,40 MPa) apresentaram valores maiores quando comparados à limpeza com DE (DE/U200= 4,60 MPa; DE/MULTI= 1,45 MPa) e PP (PP/U200= 3,74 MPa; PP/MULTI= 3,14 MPa). Uma diferença estatística também foi encontrada entre os cimentos quando o tratamento com cureta dentária foi usado (RelyX U200 ˃ Multilink Automix). O protocolo IDS/SBU+PP apresentou maior percentual de falhas coesivas. As micrografias mostraram diferenças nas características da superfície dentinária entre os grupos. Conclusão: O selamento dentinário imediato aumentou a resistência de união dos cimentos resinosos à dentina em comparação com a limpeza mecânica apenas, independentemente do cimento resinoso.(AU)

Influence of testing environment on static fatigue behavior of a glass and a polycrystalline ceramic.

It aims on evaluate the effect of the test environment on static fatigue behavior of lithium disilicate-based (LD), and yttrium oxide-stabilized zirconia (YSZ) ceramics. Specimens of LD (IPS e.max CAD, Ivoclar Vivadent) and YSZ (IPS e.max ZirCAD MO, 3 mol% Y2O3, Ivoclar Vivadent) were randomly allocated into three groups: tested in air, inert (paraffin oil, Sigma Aldrich) or distilled water. The static fatigue test (n=15) was performed using a piston-on-three ball assembly, adapted from ISO 6872, as follows: starting load 100 N for LD and 300 N for YSZ; loading application time set to 1 hour for each loading step; step size of 50 N for LD and 100 N for YSZ, applied successively until fracture. Data from static fatigue strength (MPa) and time to fracture (hours) were recorded. Fractographic analysis was executed. Survival analysis corroborates absence of influence of environment on static fatigue outcomes (fatigue strength, time to fracture and survival rates) for YSZ. For LD, specimens tested in air presented statistically superior survival rate and static fatigue strength (p= 0.025). In regards of time to fracture, LD tested in air were superior than when tested in distilled water (p=0.019) or inert (p=0.017) environments. No statistical differences for Weibull modulus were observed. Failures started on the tensile stress surface. Thus, the test environment did not affect slow crack growth (SCG) mechanisms during static fatigue test of YSZ ceramics, but it plays a significant role for the static fatigue behavior of lithium disilicate-based glass ceramics, indicating a high susceptibility to SCG.

The influence of roughness on the resistance to impact of different CAD/CAM dental ceramics

Abstract This study aimed to investigate the effect of surface roughness (polished vs. CAD/CAM milling simulation) on impact strength of five dental ceramics for manufacturing CAD/CAM monolithic restorations. Specimens of five ceramics (FC- feldspathic glass-ceramic; PICN- polymer-infiltrated ceramic-network; ZLS- zirconia-reinforced lithium silicate glass-ceramic; LD- lithium disilicate glass-ceramic; YZ- yttria-stabilized tetragonal zirconia polycrystal ceramic) to be tested under impact (15×10×2mm3; n= 15) were divided into two groups, according to surface treatment: polishing (pol) and grinding (gri) as CAD/CAM milling simulation. Impact strength was tested using the Dynstat method. Roughness, topographic, fractographic and finite element analyses were performed. The impact strength data were analyzed by Weibull, and Pearson correlation was used to correlate roughness and impact strength data. The CAD/CAM milling simulation led to significantly (p<0.05) greater roughness (Ra and Rz) and statistically reduced the impact strength for PICN (polPICN= 4.59 to griPICN= 1.09; ±76% decrease), for LD (polLD= 17.69 to griLD= 10.09; ±43% decrease) and for YZ (polYZ= 74.99 to griYZ= 20.67; ±72% decrease) ceramics; and also promoted a more irregular topography with scratches and grooves. Fractographic and FEA analyses depicted the origin of failure at the higher stress concentration side during the impact test, where the pendulum impacted. The CAD/CAM milling simulation significantly decreased the impact strength of the evaluated ceramic materials.

Resumo Este estudo teve como objetivo investigar o efeito da rugosidade da superfície (polido vs. simulação da usinagem em CAD/CAM) na resistência ao impacto de cinco cerâmicas odontológicas indicadas na fabricação de restaurações monolíticas em CAD/CAM. Espécimes de cinco cerâmicas (FC- vitrocerâmica feldspática; PICN- rede de cerâmica infiltrada com polímero; ZLS- vitrocerâmica de silicato de lítio reforçada com zircônia; LD- vitrocerâmica de dissilicato de lítio; YZ- cerâmica policristalina de zircônia tetragonal estabilizada com ítria), a serem testados sob impacto (15 × 10 × 2mm3; n= 15), foram divididos em dois grupos, de acordo com o tratamento superficial: polimento (pol) e desgaste (gri), usado como simulação da usinagem em CAD/CAM. A resistência ao impacto foi testada usando o método Dynstat. Foram realizadas as análises de rugosidade, topografia, fractografia e análise de elementos finitos. Os dados de resistência ao impacto foram analisados pela análise de Weibull, e a correlação de Pearson foi usada para correlacionar os dados de rugosidade e resistência ao impacto. A simulação da usinagem em CAD/CAM levou a uma rugosidade (Ra e Rz) significativamente maior (p < 0,05) para todas as cerâmicas, e reduziu estatisticamente a resistência ao impacto para as cerâmicas PICN (polPICN = 4,59 para griPICN = 1,09; redução de ± 76%), LD (polLD = 17,69 para griLD = 10,09; ± 43% de redução) e YZ (polYZ = 74,99 para griYZ = 20,67; ± 72% de redução); e também promoveu uma topografia mais irregular apresentando riscos e sulcos acentuados. As análises de fractografia e de elementos finitos mostraram a origem da falha no lado de maior concentração de tensão durante o teste de impacto, onde o pêndulo impactou o espécime. A simulação da usinagem em CAD/CAM reduziu significativamente a resistência ao impacto dos materiais cerâmicos avaliados.

In-lab simulation of CAD/CAM milling of lithium disilicate glass-ceramic specimens: Effect on the fatigue behavior of the bonded ceramic.

The aim of this study was to evaluate the effect of in-lab simulation procedures performed on a lithium disilicate ceramic luted to a dentin-analogue material regarding the fatigue performance and topographic changes. Lithium disilicate ceramic (IPS e.max CAD) discs (Ø = 13.5 mm and 1.5 mm of thickness) were produced in different ways: milled in a CAD/CAM system (CAD/CAM - control group); mirror-polished (POL group); produced in-lab and ground with #60 silicon carbide paper (SiC group); with #60 wood sandpaper (WS group); with a fine diamond bur (DB group); or with a CAD/CAM bur adapted in a handpiece with a custom mandrel (MANDREL group). The ceramic discs were adhesively luted (Multilink N) onto dentin analogue discs (Ø = 12 mm and 2 mm of thickness) and fatigue testing (n = 19 discs) was performed by step-stress methodology (initial load of 200 N; step-size of 50 N; 10,000 cycles per step; 20 Hz). Surface roughness and contact angle analysis were also performed. According to Kaplan-Meier and post-hoc Mantel-Cox (log-rank), distinct fabrication methods affected the fatigue performance of bonded glass-ceramic discs (p< 0.001). The CAD/CAM group presented the lowest fatigue failure loads (1250 N) and number of cycles for failure (185,000), while the POL groups obtained the highest results (1752 N; 284,444 cycles). The in-lab groups had intermediate values (1355 - 1526 N; 206,052 - 238,684 cycles). Polished specimens presented the lowest roughness values (Ra = 0.041 µm), while the SiC (1.604 µm), WS (1.701 µm), and MANDREL (1.867 µm) groups showed statistically similar roughness values to the CAD/CAM group (1.738 µm). Despite differences before etching, the contact angle was similar among the milled and simulated groups after etching, except for the polished group. Even with some topographic similarities, the tested in-lab simulation methods were not able to mimic the milled specimens in terms of fatigue findings, leading to distinct magnitude of overestimations of the results.

Effect of different surface treatments on optical, colorimetric, and surface characteristics of a lithium disilicate glass-ceramic.

OBJECTIVE: To evaluate the effect of surface treatments on optical, colorimetric, and surface characteristics of lithium disilicate glass-ceramic. MATERIALS AND METHODS: Specimens (n = 5, IPS e.max CAD) were randomly allocated to the following treatments: mirror-polished: SiC papers; as-cut: mimicking CAD-CAM milling; ground: 90-120 µm-grit diamond bur; ground polished: ground, finished (46-30 µm-grit diamond bur), polished (diamond cups, brush and diamond paste); ground glazed: ground, glazed; ground polished glazed: association of methods. CIELAB color coordinates were obtained by a spectrophotometer. CIEDE2000 color differences (ΔE00 ) and the translucency parameter (TP00 ) were calculated. Light transmittance was assessed with a colorimeter. Surface characteristics (topography and roughness) were analyzed. Statistical differences for each condition and outcome were detected using one-way ANOVA with Tukey's post-hoc test (α = 0.05). RESULTS: TP00 data show statistical reduction after grinding (p < 0.05), which was only restored with polishing (solely or with glazing). ΔE00 shows that grinding results in perceptible variations in color (above 0.81), which were restored after all post-processing protocols (exception to only glaze application in contact with a black background). Light transmittance data corroborated such performance. Polishing and glazing reduced roughness and improved surface topography. CONCLUSION: Grinding statistically increased roughness, reduced translucency, light transmittance through the ceramic, and resulted on color differences. On contrary, polishing (followed or not by glazing) reduced roughness and enhanced ceramic translucency and light transmittance. Glaze also reduced roughness, but it still presented reduced translucency. The positioning (facing up or down) of the ceramic treated surface influenced the considered outcomes. CLINICAL SIGNIFICANCE: Grinding with diamond burs results in a deleterious impact to the optical, colorimetric and surface characteristics of lithium disilicate ceramic. Thus, polishing (followed or not by glazing) is recommended for optical and topographical enhancements when lithium disilicate monolithic restorations require occlusal adjustments.

Influence of testing environment on static fatigue behavior of a glass and a polycrystalline ceramic

Abstract It aims on evaluate the effect of the test environment on static fatigue behavior of lithium disilicate-based (LD), and yttrium oxide-stabilized zirconia (YSZ) ceramics. Specimens of LD (IPS e.max CAD, Ivoclar Vivadent) and YSZ (IPS e.max ZirCAD MO, 3 mol% Y2O3, Ivoclar Vivadent) were randomly allocated into three groups: tested in air, inert (paraffin oil, Sigma Aldrich) or distilled water. The static fatigue test (n=15) was performed using a piston-on-three ball assembly, adapted from ISO 6872, as follows: starting load 100 N for LD and 300 N for YSZ; loading application time set to 1 hour for each loading step; step size of 50 N for LD and 100 N for YSZ, applied successively until fracture. Data from static fatigue strength (MPa) and time to fracture (hours) were recorded. Fractographic analysis was executed. Survival analysis corroborates absence of influence of environment on static fatigue outcomes (fatigue strength, time to fracture and survival rates) for YSZ. For LD, specimens tested in air presented statistically superior survival rate and static fatigue strength (p= 0.025). In regards of time to fracture, LD tested in air were superior than when tested in distilled water (p=0.019) or inert (p=0.017) environments. No statistical differences for Weibull modulus were observed. Failures started on the tensile stress surface. Thus, the test environment did not affect slow crack growth (SCG) mechanisms during static fatigue test of YSZ ceramics, but it plays a significant role for the static fatigue behavior of lithium disilicate-based glass ceramics, indicating a high susceptibility to SCG.

Resumo O presente estudo objetivou investigar a influência do ambiente de teste no comportamento a fadiga estática (resistência à fratura e tempo para falha) de cerâmicas à base de dissilicato de lítio (LD) e zircônia estabilizada com ítria (YSZ). Espécimes de LD (IPS e.max CAD, Ivoclar Vivadent) e YSZ (IPS e.max ZirCAD MO, 3mol% Y2O3, Ivoclar Vivadent) foram obtidos e alocados aleatoriamente em três grupos: testado em ar, em líquido inerte (óleo de parafina) ou em água destilada. O teste de fadiga estática (n= 15) foi realizado usando o teste pistão sobre três esferas, ISO 6872, da seguinte forma: carga inicial 100 N para LD e 300 N para YSZ; tempo de aplicação de carregamento definido para 1 hora para cada etapa de carregamento; tamanho do passo de 50 N para LD e 100 N para YSZ, aplicados sucessivamente até a fratura. Dados de resistência à fadiga estática (MPa) e tempo até a fratura (horas) foram registrados. A análise fractográfica foi executada. A análise de sobrevivência corrobora a ausência de influência do ambiente de teste nos resultados de fadiga estática (resistência à fadiga, tempo de fratura e taxas de sobrevivência) para a YSZ. Para LD, os corpos de prova testados em ar apresentaram taxa de sobrevivência e resistência à fadiga estática estatisticamente superiores (p= 0,025). Em relação ao tempo de fratura, os espécimes LD testados em ar foram superiores aos testados em água destilada (p= 0,019) ou em ambiente inerte (p= 0,017). Não foram observadas diferenças estatísticas para o módulo de Weibull. Todas as falhas começaram no lado onde se concentra a tensão de tração (lado de baixo) durante o teste. Com base nisso, observa-se que o ambiente de teste não afetou os mecanismos de crescimento lento de trinca durante o teste de fadiga estática da cerâmica YSZ, mas desempenha um papel significativo na resistência à fadiga estática da cerâmica de vidro à base de dissilicato de lítio, indicando alta susceptibilidade ao crescimento lento e subcrítico de trincas.

The influence of roughness on the resistance to impact of different CAD/CAM dental ceramics.

This study aimed to investigate the effect of surface roughness (polished vs. CAD/CAM milling simulation) on impact strength of five dental ceramics for manufacturing CAD/CAM monolithic restorations. Specimens of five ceramics (FC- feldspathic glass-ceramic; PICN- polymer-infiltrated ceramic-network; ZLS- zirconia-reinforced lithium silicate glass-ceramic; LD- lithium disilicate glass-ceramic; YZ- yttria-stabilized tetragonal zirconia polycrystal ceramic) to be tested under impact (15×10×2mm3; n= 15) were divided into two groups, according to surface treatment: polishing (pol) and grinding (gri) as CAD/CAM milling simulation. Impact strength was tested using the Dynstat method. Roughness, topographic, fractographic and finite element analyses were performed. The impact strength data were analyzed by Weibull, and Pearson correlation was used to correlate roughness and impact strength data. The CAD/CAM milling simulation led to significantly (p<0.05) greater roughness (Ra and Rz) and statistically reduced the impact strength for PICN (polPICN= 4.59 to griPICN= 1.09; ±76% decrease), for LD (polLD= 17.69 to griLD= 10.09; ±43% decrease) and for YZ (polYZ= 74.99 to griYZ= 20.67; ±72% decrease) ceramics; and also promoted a more irregular topography with scratches and grooves. Fractographic and FEA analyses depicted the origin of failure at the higher stress concentration side during the impact test, where the pendulum impacted. The CAD/CAM milling simulation significantly decreased the impact strength of the evaluated ceramic materials.

Fatigue behavior and colorimetric differences of a porcelain-veneered zirconia: effect of quantity and position of specimens during firing.

PURPOSE: To evaluate the influence of quantity and positioning of veneered zirconia specimens during firing of porcelain on their fatigue performance and colorimetric differences. METHODS: Bilayer discs (Ø=15 mm) were made, following ISO 6872 guidelines, using a Y-TZP core (yttria-stabilized tetragonal zirconia polycrystal ceramic; VITA In-Ceram YZ) and a feldspathic veneering material (VITA VM9), being both layers with 0.7 mm thickness. Y-TZP discs were sintered, the veneering material was applied over it, and the bilayer specimens were fired according to two factors (n=20): 'quantity' (1 or 5 samples per firing cycle; G1 and G5 groups respectively) and 'positioning' of the specimens inside the furnace (center or periphery of the refractory tray; G5C and G5P groups, respectively). The CIEL*a*b* parameters were recorded with a spectrophotometer and the color difference (ΔE 00 ) and translucency (TP 00 ) were calculated using CIEDE2000 equations. The step-stress fatigue test was performed with the veneer facing down (region of tensile stress concentration), 10 Hz frequency, initial tension of 20 MPa for 5,000 cycles, followed by steps of 10,000 cycles using a step size of 10 MPa, up to 100 MPa; data from strength and number of cycles for failure were recorded for statistical analysis. RESULTS: Unacceptable color differences (ΔE 00 >1.8) were observed comparing G5C vs. G1 (quantity) and G5C vs. G5P (positioning), meanwhile translucency parameters were not affected. Besides, only the 'quantity' factor influenced the fatigue performance (G1>G5C). None of the tested specimens survived beyond 90N and/or 75000 cycles. CONCLUSIONS: The quantity and position of the specimens during firing influence the final color of porcelain-veneered zirconia, and firing one specimen per cycle improved the fatigue performance of the bilayer system.

Influence of zirconia surface treatments of a bilayer restorative assembly on the fatigue performance.

PURPOSE: This study evaluated the influence of different surface treatments of zirconia used to enhance bonding with veneering porcelain, and thermocycling on the resistance to porcelain cracking and delamination during fatigue test. METHODS: Bilayer ceramic discs were made from zirconia blocks (IPS e.max Zircad MO, Ivoclar Vivadent - 0.7 mm thickness) and randomized into 8 groups (n= 15) according to two factors: 'zirconia surface treatment' (Control; Grinding - diamond bur; Air-abrasion - aluminum oxide particles; and Liner - application of a ceramic liner [IPS e.max Zirliner, Ivoclar Vivadent]); and 'thermocycling' (presence - 12,000 thermal cycles; 5-55ºC; or absence). The discs were veneered with porcelain (IPS e.max Ceram, Ivoclar Vivadent - 0.7 mm; totaling 1.4 mm thickness) according to ISO 6872:2015 for biaxial flexure strength testing. Fatigue tests (step-stress approach; 20 to 100 MPa; step of 10 MPa; 10,000 cycles per step; 10 Hz frequency) were run, followed by the data analysis (Kaplan-Meier and Mantel-Cox post-hoc tests). Analysis of roughness, topography, crystallographic phase arranges and fractography were also executed. RESULTS: The surface treatment and thermocycling did not influence the porcelain crack nor delamination resistance. When only comparing the surface treatments for crack resistance outcome, the liner application depicted the worst fatigue performance in comparison to grinding and air-abrasion, while all groups were similar for delamination. CONCLUSIONS: Neither the surface treatment of the zirconia nor the thermocycling influences the porcelain crack resistance or the resistance to delamination of the bilayer porcelain-veneered zirconia specimens.

Effect of zirconia surface treatment, resin cement and aging on the load-bearing capacity under fatigue of thin simplified full-contour Y-TZP restorations.

This study investigated the effect of zirconia surface treatment (air-abrasion with aluminum oxide or tribochemical silica coating) and aging on the fatigue behavior of thin monolithic Y-TZP (yttria-stabilized tetragonal zirconia polycrystal) restorations cemented with 2 types of resin cements, containing or not containing MDP, to a dentin-like substrate. Y-TZP ceramic (Zenostar T, diameter (Ø) 10 mm, 0.7 mm thick) and dentin-like discs (Ø 10 mm, 2.8 mm thick) were assigned into eight groups according to three factors: 'zirconia surface treatment' (aluminum oxide particles air-abrasion 'AO'; or tribochemical silica coating via silica-coated aluminum trioxide particles air-abrasion + silanization 'SC'); 'MDP-containing resin cement' (with: Panavia F2.0, 'MDP'; or without: Multilink Automix, 'nMDP'); and 'aging' (baseline; or aged - 'AG':12,000 thermal cycles + 60 days water storage). Y-TZP intaglio surface was conditioned and dentin-like substrate was etched with hydrofluoric acid prior to bonding. Aging was performed in half of the specimens before the fatigue testing (Staircase, 20 Hz; 250,000 cycles). Fractographic and topographic characteristics were analyzed by stereomicroscope and SEM. Prior to aging, no significant difference was found between the two surface treatments, irrespective to the cement. Samples bonded with resin cement containing MDP had a significant reduction in their fatigue failure load when Y-TZP was air-abraded with aluminum oxide particles and subjected to aging (MDP-AO = 2050.71A; MDP-AO/AG = 1756.67B). Other studied conditions were not affected by aging. Topographic images revealed a rougher surface for aluminum oxide air-abrasion. Fractography supports all failures as a radial crack starting at the Y-TZP intaglio surface. Bonded thin simplified Y-TZP restorations had a high load-bearing capacity, regardless of the studied factors. The MDP-containing resin cement applied on aluminum oxide air-abraded zirconia surface was not enough to maintain the fatigue performance after aging, while higher stability to aging was achieved by treating with the tribochemical silica coating method. When using MDP-free resin cement, the surface treatment and the aging did not impact the fatigue performance.

Polishing of Ground Y-TZP Ceramic is Mandatory for Improving the Mechanical Behavior.

It evaluated the effect of aging by Low Temperature Degradation (LTD), executed after post- processing surface treatments (polishing, heat treatment and glazing), on the surface characteristics (micromorphology and roughness) and on the structural stability (phase transformation and mechanical behavior-flexural strength and structural reliability) of a ground yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Discs of Y-TZP (VITA In-Ceram YZ) were manufactured (ISO:6872-2015; 15 mm in diameter and 1.2 ± 0.2 mm in thickness) and randomly assigned into 10 groups according two factors: "aging" in 2 levels (with or without) and "surface treatment" in 5 levels (Ctrl: as-sintered; Gr: grinding with coarse diamond bur; Gr + HT: grinding plus heat treatment; Gr + Pol: grinding plus polishing; Gr + Gl: grinding plus glazing). Roughness (n=30), biaxial flexural test (n=30), phase transformation (n=2), and surface topography (n=2) analyses were performed. Aging led to an intense increase in monoclinic (m) phase content for all the tested conditions, being the as-sintered samples (Ctrl= 65.6%) more susceptible to the t-m phase transformation. Despite of increasing the m-phase content, aging was not detrimental for characteristic strength (except to the grinding condition). There was no significant reduction in the Weibull modulus after surface treatments. Additionally, heat treatment and glazing after grinding led to a decrease in characteristic strength, while polishing presented the highest characteristic strength values. Thus, polishing is mandatory after grinding the Y-TZP ceramic, while performing glazing or heat-treatment alone after grinding lead to the worst mechanical performance.

Polishing of ground y-tzp ceramic is mandatory for improving the mechanical behavior

Abstract It evaluated the effect of aging by Low Temperature Degradation (LTD), executed after post- processing surface treatments (polishing, heat treatment and glazing), on the surface characteristics (micromorphology and roughness) and on the structural stability (phase transformation and mechanical behavior-flexural strength and structural reliability) of a ground yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Discs of Y-TZP (VITA In-Ceram YZ) were manufactured (ISO:6872-2015; 15 mm in diameter and 1.2 ± 0.2 mm in thickness) and randomly assigned into 10 groups according two factors: "aging" in 2 levels (with or without) and "surface treatment" in 5 levels (Ctrl: as-sintered; Gr: grinding with coarse diamond bur; Gr + HT: grinding plus heat treatment; Gr + Pol: grinding plus polishing; Gr + Gl: grinding plus glazing). Roughness (n=30), biaxial flexural test (n=30), phase transformation (n=2), and surface topography (n=2) analyses were performed. Aging led to an intense increase in monoclinic (m) phase content for all the tested conditions, being the as-sintered samples (Ctrl= 65.6%) more susceptible to the t-m phase transformation. Despite of increasing the m-phase content, aging was not detrimental for characteristic strength (except to the grinding condition). There was no significant reduction in the Weibull modulus after surface treatments. Additionally, heat treatment and glazing after grinding led to a decrease in characteristic strength, while polishing presented the highest characteristic strength values. Thus, polishing is mandatory after grinding the Y-TZP ceramic, while performing glazing or heat-treatment alone after grinding lead to the worst mechanical performance.

Resumo Este estudo avaliou o efeito do envelhecimento através da degradação a baixas temperaturas (low temperaturare degradation - LTD) após a realização de tratamentos de superfície pós- sinterização (polimento, tratamento térmico e glaze) nas características superficiais (micromorfologia e rugosidade), e na estabilidade estrutural (transformação de fase e comportamento mecânico - resistência flexural e confiabilidade estrutural) de uma cerâmica de zircônia tetragonal policristalina estabilizada por ítria (Y-TZP) desgastada. Discos de cerâmica Y-TZP (VITA In-Ceram YZ) foram confeccionados (ISO:6872-2015; 15mm de diâmetro e 1,2 ± 0,2mm de espessura) e randomicamente divididos em 10 grupos de acordo com dois fatores: "envelhecimento" (com e sem) e "tratamento de superfície" (Ctrl - sem tratamento; Gr - desgaste com ponta diamantada grossa; Gr + HT - desgaste mais tratamento térmico; Gr + Pol - desgaste mais polimento; Gr + Gl - desgaste mais glazeamento). Foram realizadas as análises de rugosidade (n=30), flexão biaxial (n=30), transformação de fase (n=2) e topografia de superfície (n=2). O envelhecimento levou a um aumento intenso no conteúdo de fase monoclínica (m) em todas as condições testadas, sendo observada uma maior susceptibilidade de transformação de fase t-m nas amostras do grupo controle (Ctrl= 65.6%). Apesar de provocar elevada transformação de fase, o envelhecimento não apresentou efeitos negativos nos desfechos avaliados. Não houve redução significativa do módulo de Weibull após os tratamentos. Além disso, o tratamento térmico e o glaze após desgaste levaram a uma redução da resistência característica, enquanto que o grupo polimento apresentou o mais alto valor de resistência característica. O glaze e o tratamento térmico geraram o pior desempenho mecânico, portanto a realização do polimento após desgaste de uma cerâmica Y-TZP é obrigatória.

The effect of extended glaze firing on the flexural fatigue strength of hard-machined ceramics.

STATEMENT OF PROBLEM: It is unclear whether an extended glaze firing could improve the long-term mechanical performance of densely sintered CAD-CAM ceramics. PURPOSE: The purpose of this in vitro study was to analyze the effect of an extended glaze firing on the flexural fatigue strength (FFS) of densely sintered milled (hard-machined) leucite-based (LEU) and lithium disilicate-based (DIS) ceramics. MATERIAL AND METHODS: Disks were machined from ceramic blocks and divided into 6 groups (n=20) according to the material, LEU or DIS, and to the applied glaze firing: manufacturer-recommended glaze (G group), extended glaze (EG group), and control/no firing (C group). The surface roughness of the disks was measured before and after firing by using a contact profilometer, and data were compared by paired sample tests. Specimens were submitted to fatigue by using the staircase test design in water (piston-on-3 balls; 500 000 cycles, 20 Hz, and sinusoidal loading). Mean (±SD) FFS values were then calculated and analyzed by using 1-way analysis of variance and post hoc Tukey test (α=.05). RESULTS: Surface roughness did not change after the firing (P>.05). The highest FFS value in both ceramics was obtained after EG firing (LEU-EG=80.52 ±6.3 MPa; DIS-EG=147.25 ±10.5 MPa), which was statistically superior to G firing (LEU-G=73 ±6.8 MPa, P=.003; DIS-G=134.34 ±15.6 MPa; P=.023) and C group (LEU-C=61.94 ±6.3 MPa; P<.001; DIS-C=134.13 ±17.3 MPa; P=.023). CONCLUSIONS: EG firing optimized the biaxial flexural fatigue strength of hard-machined leucite and lithium disilicate ceramics compared with conventional glaze firing.

Hydrofluoric acid concentrations: Effect on the cyclic load-to-failure of machined lithium disilicate restorations.

OBJECTIVES: To evaluate the effects of the etching with different hydrofluoric acid (HF) concentrations on the cyclic load-to-failure (CLf) of machined lithium disilicate crowns cemented to dentin analogue material. METHODS: Pairs of dentin analogue prosthetic preparations and lithium disilicate ceramic crowns with simplified and standardized designs were machined (n=18). The preparations were etched with 10% HF (60s), followed by primer application. The intaglio surface of the ceramic crowns was treated as follows: non-etched (control, CTRL); or etched for 20s with different HF concentrations - 3% (HF3), or 5% (HF5), or 10% (HF10). A silane coating was then applied onto the treated ceramic surfaces, and they were adhesively cemented to the preparations. To perform the fatigue tests (staircase approach), a hemispheric stainless-steel piston (Ø=40mm) applied cyclic loads in the center of the crowns under water (initial load: 720N; step-size: 70N; cycles: 500,000; frequency: 20Hz). Additionally, topographic, fractographic, and fractal analyses were carried out. The fatigue data were analyzed using the Dixon and Mood method. RESULTS: Although the topographic and fractal analyses depicted the action of HF etching altering the superficial complexity and topography, the preponderant topography pattern was established by machining on CAD/CAM. All groups showed similar CLf (in N) (CTRL=805.00±91.23; HF3=781.25±29.87; HF5=755.00±154.49; HF10=833.75±100.74). SIGNIFICANCE: Etching with different HF acid concentrations did not promote a deleterious effect on the cyclic load-to-failure of machined lithium disilicate crowns.

Internal adjustments decrease the fatigue failure load of bonded simplified lithium disilicate restorations.

OBJECTIVE: To investigate the effect of intaglio surface adjustment of simplified lithium disilicate ceramic restorations adhesively cemented to a dentin-like material on its fatigue behavior. METHODS: Ceramic discs (IPS e.max CAD) were prepared and an in-Lab simulation of machining roughness was performed by grinding with SiC paper (#60). Ceramic discs were divided into 4 groups according to the internal adjustment of the cementation surface: no adjustments (CTRL); adjustment with a medium (M), fine (F), or extra fine (FF) diamond bur. Dentin-like material discs were also produced. Ceramic disc intaglio surfaces were etched (5% hydrofluoric acid; 20s) and received a silane coating. Dentin-like material discs were etched (10% hydrofluoric acid; 1min) and received a primer coating. Pairs of ceramic/dentin-like material were adhesively cemented (Multilink Automix), and fatigue failure load tests were performed using the Staircase approach (250,000 cycles; 20Hz). Roughness, topographic and fractographic analyses were performed. Statistical analyses were carried out through ANOVA tests. RESULTS: All ground groups (M=521.3 N; F=536.9 N; FF=676.2 N) presented lower fatigue failure load values than the control (1241.6 N). M diamond bur created a rougher surface than F (Ra and Rz parameters). However, FF was similar to F and M for Ra, and similar to F for Rz. SIGNIFICANCE: Bur adjustments on the intaglio surface of simplified lithium disilicate ceramic restorations greatly decreased the fatigue failure load even using an extra-fine diamond bur. Care should be taken when internal adjustments are needed.

Effect of grinding and aging on subcritical crack growth of a Y-TZP ceramic.

This study aimed to investigate slow crack growth (SCG) behavior of a zirconia ceramic after grinding and simulated aging with low-temperature degradation (LTD). Complementary analysis of hardness, surface topography, crystalline phase transformation, and roughness were also measured. Disc-shaped specimens (15 mm Ø × 1.2 mm thick, n = 42) of a full-contour Y-TZP ceramic (Zirlux FC, Amherst) were manufactured according to ISO:6872-2008, and then divided into: Ctrl - as-sintered condition; Ctrl LTD - as-sintered after aging in autoclave (134°C, 2 bar, 20 h); G - ground with coarse diamond bur (grit size 181 µm); G LTD - ground and aged. The SCG parameters were measured by a dynamic biaxial flexural test, which determines the tensile stress versus stress rate under four different rates: 100, 10, 1 and 0.1 MPa/s. LTD led to m-phase content increase, as well as grinding (m-phase content: Ctrl - 0%; G - 12.3%; G LTD - 59.9%; Ctrl LTD - 81%). Surface topography and roughness analyses showed that grinding created an irregular surface (increased roughness) and aging did not promote any relevant surface change. There was no statistical difference on surface hardness among different conditions. The control group presented the lowest strength values in all tested rates. Regarding SCG, ground conditions were less susceptible to SCG, delaying its occurrence. Aging (LTD) caused an increase in SCG susceptibility for the as-sintered condition (i.e. G < G LTD < Ctrl < Ctrl LTD).

Fatigue failure load of two resin-bonded zirconia-reinforced lithium silicate glass-ceramics: Effect of ceramic thickness.

OBJECTIVES: To evaluate the effect of ceramic thickness on the fatigue failure load of two zirconia-reinforced lithium silicate (ZLS) glass-ceramics, adhesively cemented to a dentin analogue material. METHODS: Disc-shaped specimens were allocated into 8 groups (n=25) considering two study factors: ZLS ceramic type (Vita Suprinity - VS; and Celtra Duo - CD), and ceramic thickness (1.0; 1.5; 2.0; and 2.5mm). A trilayer assembly (ϕ=10mm; thickness=3.5mm) was designed to mimic a bonded monolithic restoration. The ceramic discs were etched, silanized and luted (Variolink N) into a dentin analogue material. Fatigue failure load was determined using the Staircase method (100,000 cycles at 20Hz; initial fatigue load ∼60% of the mean monotonic load-to-failure; step size ∼5% of the initial fatigue load). A stainless-steel piston (ϕ=40mm) applied the load into the center of the specimens submerged in water. Fractographic analysis and Finite Element Analysis (FEA) were also performed. RESULTS: The ceramic thickness influenced the fatigue failure load for both ZLS materials: Suprinity (716N up to 1119N); Celtra (404N up to 1126N). FEA showed that decreasing ceramic thickness led to higher stress concentration on the cementing interface. SIGNIFICANCE: Different ZLS glass-ceramic thicknesses influenced the fatigue failure load of the bonded system (i.e. the thicker the glass ceramic is, the higher the fatigue failure load will be). Different microstructures of the ZLS glass-ceramics might affect the fatigue behavior. FEA showed that the thicker the glass ceramic is, the lower the stress concentration at the tensile surface will be.

Effect of Grinding and Multi-Stimuli Aging on the Fatigue Strength of a Y-TZP Ceramic

Abstract This study aimed to investigate the effect of grinding and multi-stimuli aging on the fatigue strength, surface topography and the phase transformation of Y-TZP ceramic. Discs were manufactured according to ISO-6872:2008 for biaxial flexure testing (diameter: 15 mm; thickness: 1.2 mm) and randomly assigned considering two factors "grinding" and "aging": C- control (as-sintered); CA- control + aging; G- ground; GA- ground + aging. Grinding was carried out with coarse diamond burs under water-cooling. Aging protocols consisted of: autoclave (134°C, 2 bars pressure, 20 hours), followed by storage for 365 days (samples were kept untouched at room temperature), and by mechanical cycling (106 cycles by 20 Hz under a load of 50% from the biaxial flexure monotonic tests). Flexural fatigue strengths (20,000 cycles; 6 Hz) were determined under sinusoidal cyclic loading using staircase approach. Additionally, surface topography analysis by FE-SEM and phase transformation analysis by X-ray Diffractometry were performed. Dixon and Mood methodology was used to analyze the fatigue strength data. Grinding promotes alterations of topographical pattern, while aging apparently did not alter it. Grinding triggered t-m phase transformation without impacting the fatigue strength of the Y-TZP ceramic; and aging promoted an intense t-m transformation that resulted in a toughening mechanism leading to higher fatigue strength for as-sintered condition, and a tendency of increase for ground condition (C < CA; G = GA). It concludes that grinding and aging procedures did not affect deleteriously the fatigue strength of the evaluated Y-TZP ceramic, although, it promotes surface topography alterations, except to aging, and t-m phase transformation.

Resumo Este estudo objetivou investigar o efeito do desgaste e envelhecimento (estímulos combinados) na resistência à fadiga, topografia superficial e transformação de fase de uma cerâmica Y-TZP. Discos para teste de flexão biaxial foram confeccionados segundo as normas da ISO-6872:2008 (15 mm Ø; 1,2 mm espessura) e randomicamente distribuídos de acordo com os fatores "desgaste" e "envelhecimento": C- controle (sinterizado); CA- controle envelhecido; G- desgaste; GA- desgaste envelhecido. O desgaste foi feito com pontas diamantadas de granulação grossa sob irrigação com água. Os protocolos de envelhecimento consistiram em: autoclave (134°C, 2 bar de pressão, 20 horas), 365 dias armazenados em temperatura ambiente, e ciclagem mecânica (106 ciclos a 20 Hz em um intervalo de carga de até 50% da carga monotônica observada em testes estáticos). A resistência à fadiga foi determinada para 20.000 ciclos à 6 Hz sob carregamento sinusoidal através do método de escada. Adicionalmente, análises de topografia superficial em microscopia eletrônica de varredura e de transformação de fase por difração de raios-X foram executadas. A metodologia de Dixon e Mood foi usada para analisar os dados de resistência à fadiga. Foi observado que o desgaste promove uma alteração de padrão topográfico superficial; enquanto o envelhecimento aparentemente não demonstra influência. Em relação à transformação de fase e resistência à fadiga, o desgaste desencadeou um aumento de fase m sem impactar na resistência à fadiga da cerâmica Y-TZP; já o envelhecimento promoveu uma intensa transformação de fase, resultando no mecanismo de tenacificação, que gerou um aumento na resistência à fadiga para a condição sinterizada e uma tendência a aumento na condição desgaste (C < CA; G = GA). Os dados elucidam que o desgaste e o envelhecimento não impactaram negativamente na resistência à fadiga da cerâmica Y-TZP, apesar de promoverem alterações de topografia superficial e intensa transformação de fase de t-m respectivamente.

Effect of Grinding and Multi-Stimuli Aging on the Fatigue Strength of a Y-TZP Ceramic.

This study aimed to investigate the effect of grinding and multi-stimuli aging on the fatigue strength, surface topography and the phase transformation of Y-TZP ceramic. Discs were manufactured according to ISO-6872:2008 for biaxial flexure testing (diameter: 15 mm; thickness: 1.2 mm) and randomly assigned considering two factors "grinding" and "aging": C- control (as-sintered); CA- control + aging; G- ground; GA- ground + aging. Grinding was carried out with coarse diamond burs under water-cooling. Aging protocols consisted of: autoclave (134°C, 2 bars pressure, 20 hours), followed by storage for 365 days (samples were kept untouched at room temperature), and by mechanical cycling (106 cycles by 20 Hz under a load of 50% from the biaxial flexure monotonic tests). Flexural fatigue strengths (20,000 cycles; 6 Hz) were determined under sinusoidal cyclic loading using staircase approach. Additionally, surface topography analysis by FE-SEM and phase transformation analysis by X-ray Diffractometry were performed. Dixon and Mood methodology was used to analyze the fatigue strength data. Grinding promotes alterations of topographical pattern, while aging apparently did not alter it. Grinding triggered t-m phase transformation without impacting the fatigue strength of the Y-TZP ceramic; and aging promoted an intense t-m transformation that resulted in a toughening mechanism leading to higher fatigue strength for as-sintered condition, and a tendency of increase for ground condition (C < CA; G = GA). It concludes that grinding and aging procedures did not affect deleteriously the fatigue strength of the evaluated Y-TZP ceramic, although, it promotes surface topography alterations, except to aging, and t-m phase transformation.