Resistance to bond degradation between dual-cure resin cements and pre-treated sintered CAD-CAM dental ceramics

Objective: To evaluate the bond stability of resin cements when luted to glass-reinforced alumina and zirconia CAD/CAM dental ceramics. Study design: Eighteen glass-infiltrated alumina and eighteen densely sintered zirconia blocks were randomly conditioned as follows: Group 1: No treatment; Group 2: Sandblasting (125 µm Al2O3-particles); and Group 3: Silica-coating (50 µm silica-modified Al2O3-particles). Composite samples were randomly bonded to the pre-treated ceramic surfaces using different resin cements: Subgroup 1: Clearfil Esthetic Cement (CEC); Subgroup 2: RelyX Unicem (RXU); and Subgroup 3: Calibra (CAL). After 24 h, bonded specimens were cut into 1 ± 0.1 mm2 sticks. One-half of the beams were tested for microtensile bond strength (MTBS). The remaining one-half was immersed in 10 % NaOCl aqueous solution (NaOClaq) for 5 h before testing. The fracture pattern and morphology of the debonded surfaces were assessed with a field emission gun scanning electron microscope (FEG-SEM). A multiple ANOVA was conducted to analyze the contributions of ceramic composition, surface treatment, resin cement type, and chemical challenging to MTBS. The Tukey test was run for multiple comparisons (p < 0.05). Results: After 24 h, CEC luted to pre-treated zirconia achieved the highest MTBS. Using RXU, alumina and zirconia registered comparable MTBS. CAL failed prematurely, except when luted to sandblasted zirconia. After NaOClaq storage, CEC significantly lowered MTBS when luted to zirconia or alumina. RXU decreased MTBS only when bonded to silica-coated alumina. CAL recorded 100 % of pre-testing failures. Micromorphological alterations were evident after NaOClaq immersion. Conclusions: Resin-ceramic interfacial longevity depended on cement selection rather than on surface pre-treatments. The MDP-containing and the self-adhesive resin cements were both suitable for luting CAD/CAM ceramics. Despite both cements being prone to degradation, RXU luted to zirconia or untreated or sandblasted alumina showed the most stable interfaces. CAL experimented spontaneous debonding in all tested groups. Key words:CAD/CAM ceramic, alumina, zirconia, resin cement, surface pre-treatment, sandblasting, silica-coating, chemical aging, bond degradation, microtensile bond strength.     

Influence of sandblasting granulometry and resin cement composition on microtensile bond strength to zirconia ceramic for dental prosthetic frameworks

ObjectivesTo evaluate the effect of the particle size of sandblasting and the composition of the resin cement on the microtensile bond strength (MTBS) to zirconia.MethodsForty zirconia blocks (Cercon, Dentsply) were polished and randomly treated as follows: Group 1 (NT): no treatment; Group 2 (APA-I): airborne particle abrasion (Cobra, Renfert) using 25-μm aluminium-oxide (Al₂O₃)-particles; Group 3 (APA-II): APA with 50-μm Al₂O₃-particles; and Group 4 (APA-III): APA using 110-μm Al₂O₃-particles. Ceramic blocks were duplicated in composite resin. Samples of each pretreatment group were randomly divided into two subgroups depending on the resin cement used for bonding the composite disks to the treated zirconia surfaces. Subgroup 1 (PAN), which was a 10-MDP-containing luting system, used Clearfil Ceramic Primer plus Panavia F 2.0 (Kuraray) and Subgroup 2 (BIF) used Bifix SE (VOCO) self-adhesive cement. After 24 h, bonded specimens were cut into 1 ± 0.1 mm² sticks. MTBS values were obtained using a universal testing machine (cross-head speed = 0.5 mm/min). Failure modes were recorded and the interfacial morphology of the debonded microbars was SEM-assessed. Two-way ANOVA, Student–Newman–Keuls tests, and the step-wise linear regression analysis were performed with the MTBS being the dependent variable (p < 0.05).ResultsDespite the sandblasting granulometry, PAN bonded to air-abraded surfaces attained the highest MTBS and frequently showed mixed fractures. BIF recorded no significant differences in MTBS depending on the conditioning method, and registered the highest rates of premature and adhesive failures.ConclusionsThe 10-MDP-containing luting system seems to be the most suitable to bond zirconium-oxide ceramic, mainly after sandblasting.     

Influence of surface treatments and resin cement selection on bonding to densely-sintered zirconium-oxide ceramic

ObjectivesTo evaluate the effect of surface conditioning on the microtensile bond strength of zirconium-oxide ceramic to dual-cured resin cements.MethodsEighteen cylinder-shaped zirconium-oxide ceramic blocks (Cercon^® Zirconia, Dentsply) were treated as follows: (1) Sandblasting with 125 μm aluminum-oxide (Al₂O₃) particles; (2) tribochemical silica coating using 50 μm Al₂O₃ particles modified by silica; (3) no treatment. Each ceramic cylinder was duplicated in composite resin (Tetric Evo Ceram, Ivoclar-Vivadent) using a silicon mold. Composite cylinders were bonded to conditioned ceramics using: (1) Calibra (Densply Caulk); (2) Clearfil Esthetic Cement (Kuraray); (3) Rely × Unicem (3 M ESPE). After 24 h bonded specimens were cut into microtensile sticks that were loaded in tension until failure. Data were analyzed using two-way ANOVA and Student–Newman–Keuls test for multiple comparisons (p < 0.05). Failure mode was recorded and the interfacial morphology of debonded specimens was observed using a scanning electron microscope (SEM). Surface topography and ceramic average surface roughness were analyzed under an atomic force microscope (AFM).ResultsSignificant changes in zirconia surface roughness occurred after sandblasting (p < 0.001). Bond strength of Clearfil cement to zirconia was significantly higher than that of Rely × Unicem and Calibra, regardless of the surface treatment (p < 0.001). When using Calibra, premature failures occurred in non-treated and silica coated zirconia surfaces.SignificanceThe phosphate monomer-containing luting system (Clearfil Esthetic Cement) is recommended to bond zirconia ceramics and surface treatments are not necessary.     

Tensile bond strength between tooth-colored porcelain and sandblasted zirconia framework

PurposeThe purpose of this study was to examine the bond strength between tooth-colored porcelain and sandblasted zirconia framework.MethodsThe surfaces of zirconia specimens that had been cut into a size suitable for a bending test were sandblasted at three different pressures (0.2, 0.4 and 0.6 MPa). The surface roughness of each specimen was measured and then a 3-point bending test was performed. After that, other zirconia specimens simulating a crown framework were fabricated and their surfaces were sandblasted. Three types of tooth-colored porcelain were fired onto the surface of those zirconia specimens, and the tensile bond strength between the two substances was examined.ResultsWhen the sandblasting pressure was increased, the surface roughness of zirconia specimens tended to become, but the flexural strength remained unchanged. The specimens simulating a zirconia framework had a higher strength of bond when sandblasted at 0.4 or 0.6 MPa than when blasted at 0.2 MPa. The zirconia specimens sandblasted at a pressure of 0.4 MPa had a bond strength to tooth-colored porcelain of 37.7–49.5 MPa.ConclusionWhen sandblasted at a pressure of 0.4 MPa, the zirconia specimens developed a strong bond with the tooth-colored porcelain, regardless of the type of porcelain.     

Misfit and microleakage of implant-supported crown copings obtained by laser sintering and casting techniques,luted with glass-ionomer,resin cements and acrylic/urethane-based agents

ObjectivesThis study evaluated the marginal misfit and microleakage of cement-retained implant-supported crown copings.MethodsSingle crown structures were constructed with: (1) laser-sintered Co–Cr (LS); (2) vacuum-cast Co–Cr (CC) and (3) vacuum-cast Ni–Cr–Ti (CN). Samples of each alloy group were randomly luted in standard fashion onto machined titanium abutments using: (1) GC Fuji PLUS (FP); (2) Clearfil Esthetic Cement (CEC); (3) RelyX Unicem 2 Automix (RXU) and (4) DentoTemp (DT) (n = 15 each). After 60 days of water ageing, vertical discrepancy was SEM-measured and cement microleakage was scored using a digital microscope. Misfit data were subjected to two-way ANOVA and Student–Newman–Keuls multiple comparisons tests. Kruskal–Wallis and Dunn's tests were run for microleakage analysis (α = 0.05).ResultsRegardless of the cement type, LS samples exhibited the best fit, whilst CC and CN performed equally well. Despite the framework alloy and manufacturing technique, FP and DT provide comparably better fit and greater microleakage scores than did CEC and RXU, which showed no differences.ConclusionsDMLS of Co–Cr may be a reliable alternative to the casting of base metal alloys to obtain well-fitted implant-supported crowns, although all the groups tested were within the clinically acceptable range of vertical discrepancy. No strong correlations were found between misfit and microleakage. Notwithstanding the framework alloy, definitive resin-modified glass-ionomer (FP) and temporary acrylic/urethane-based (DT) cements demonstrated comparably better marginal fit and greater microleakage scores than did 10-methacryloxydecyl-dihydrogen phosphate-based (CEC) and self-adhesive (RXU) dual-cure resin agents.     

Operator vs. material influence on clinical outcome of bonded ceramic inlays

ObjectiveThe aim of the present study was to clinically evaluate the suitability of Definite Multibond and Definite ormocer resin composite for luting of Cergogold glass ceramic inlays in a two-center trial involving two dentists.MethodsThirty-nine patients received 98 Cergogold inlays with at least one inlay luted with Definite Multibond/Definite (n = 45) and at least one inlay luted with Syntac/Variolink Ultra (n = 53) in a split mouth design. Treatments were carried out in two private practices by two operators (Operator A: n = 38; Operator B: n = 60). Forty-four cavities required caries profunda treatment, 23 cavities exhibited no enamel at the cervical margin. At baseline (2 months), and after 6, 14, 27, and 51 months of clinical service, the restorations were investigated according to modified USPHS criteria.ResultsThe drop-out rate was 3% after 4 years. After 48 months of clinical service, 21 restorations in 16 patients (9 luted with Definite, 12 with Variolink; 2 placed by operator A and 19 by operator B) had to be replaced due to inlay fracture (n = 11), tooth fracture (n = 4), hypersensitivities (n = 3), or marginal gap formation (n = 3). Seventy-seven inlays were in good condition (survival rate 89.9%, median survival time 4.2 years (95% confidence interval ±0.25; survival analysis by Kaplan–Meier algorithm). Survival rate after 4 years was 97.4% for operator A, and 75.4% for operator B (p = 0.002; Log Rank/Mantel-Cox) resulting in annual failure rates of 0.6% and 6.2%, respectively. The operators did not differently judge the clinical behaviour of the luting procedures (Mann–Whitney U-test, p > 0.05). Independent of the operator and the used luting system, the following criteria significantly changed over time: color match, marginal integrity, tooth integrity, inlay integrity, sensitivity, hypersensitivity, and X-ray control (p < 0.05; Friedman test). Significant differences between operators over the whole period were computed for the criteria marginal integrity, tooth integrity, and inlay integrity (p < 0.05, Mann–Whitney test). Differences between luting materials were only present during single recalls.SignificancesFor luting of ceramic inlays, only slight differences between the two luting systems were detectable. The operator influence on clinical outcome was clearly proven.     

The development and testing of glaze materials for application to the fit surface of dental ceramic restorations

ObjectivesThe aims of the study were to develop and test overglaze materials for application to the fit surface of dental ceramic restorations, which could be etched and adhesively bonded and increase the flexural strength of the ceramic substrate.MethodsThree glaze materials were developed using commercial glass powders (P25 and P54, Pemco, Canada). P25 (90 wt%) was mixed with P54 (10 wt%) to produce (P25/P54). P54 (90 wt%) was mixed with P25 (10 wt%) to produce (P54/P25). P25 (90 wt%) was mixed with 10 wt% of an experimental glass powder (P25/frit). Eighty-two disc specimens (14 mm × 2 mm) were produced by heat pressing a leucite glass–ceramic and were sandblasted with 50 μm glass beads. Group 1 control specimens (10) were sandblasted. Groups 2–4 (10 per group) were coated using P25/frit (Group 2), P25/P54 (Group 3) and P54/P25 (Group 4) overglazes before sintering. Groups 1–4 were etched for 2 min using 9.5% HF (Gresco, USA). Composite cylinders (Marathon^® v, Den-Mat) were light cured and bonded to the glazed and prepared disc surfaces and groups water stored for 8 days. Groups were tested using shear bond strength (SBS) testing at 0.5 mm/min. Disc specimens (42) were tested using the biaxial flexural strength (BFS) test at a crosshead speed of 0.15 mm/min. Group 1 was tested as sandblasted (21) and Group 2 (21) after coating the tensile surface with P25/frit. Xrd, Eds and Sem analyzes were carried out.ResultsMean SBS (MPa ± S.D.) were: Group 1: 10.7 ± 2.1; Group 2: 9.8 ± 1.9; Group 3: 1.8 ± 1.0 and Group 4: 2.6 ± 1.7. Groups 1 and 2 were statistically different to Groups 3 and 4 (p < 0.001), but there was no difference between Groups 1 and 2 and 3 and 4 (p > 0.05). The mean BFS (MPa ± S.D.) of the overglazed Group 2 (200.2 ± 22.9) was statistically different (p < 0.001) to Group 1 (150.4 ± 14.3).SignificanceThe P25/frit overglaze significantly (p < 0.001) increased the biaxial flexural strength of the leucite glass–ceramic substrate and produced comparable shear bond strengths to an etched and bonded control. The application of etched overglaze materials to dental glass–ceramic and ceramic substrates may be useful in adhesive dentistry.     

Curing potential and color stability of different resin-based luting materials

PurposeTo determine the curing potential and color stability of resin-based luting materials for aesthetic restorations.Material and MethodsFour resin-based luting agents were tested: traditional dual-activated resin cement (RelyX ARC, ARC), amine-free dual-activated resin cement (RelyX Ultimate, ULT), light-activated resin cement (RelyX Veneer, VEN), and pre-heated restorative resin composite (Filtek Supreme, PHC). Degree of C = C conversion was determined by infrared spectroscopy (n = 3) with direct light exposure or with interposition of 1.5-mm-thick ceramic (e.max Press HT) between the luting material and light. The curing potential considered the ratio between these two scenarios. Color difference (n = 6) was determined by CIELAB (ΔE_ab) and CIEDE2000 (ΔE₀₀) methods, by spectrophotometer measurements made 24 h after photoactivation and 90 days after storage in water. Data was submitted to ANOVA and Tukey’s test (α = 0.05).ResultsThe luting agents affected both conversion and color stability. With ceramic, ARC produced the highest conversion among the tested groups (75 ± 1%) and the pre-heated composite (PHC) the lowest one (51 ± 3%), but the curing potential was similar for all materials. ULT produced lower ΔE_ab than ARC. PHC presented the lowest color difference when considered both CIELAB and CIE2000 methods (ΔE_ab 2.1 ± 0.4; ΔE₀₀ 1.6 ± 0.2).SignificanceAll luting strategies presented high curing potential. Amine-free dual-activated material was able to reduce color difference than that formulated with the amine component. Pre-heated composite produced the least color variation after storage.     

Tensile bond strength of cast commercially pure titanium dowel and cores cemented with three luting agents

PurposeThe purpose of this study was to compare the tensile strength of commercially pure titanium dowels and cores cemented with zinc phosphate or resin cements.MethodsTwenty-one extracted human canines were endodontically treated. The root preparations were accomplished using Largo reamers (10 mm in depth and 1.7 mm in diameter). Acrylic resin patterns for the dowel and cores were made, and specimens were cast in commercially pure titanium (n = 7) and divided in three groups: TZ–CP Ti dowels luted with zinc phosphate luting agent, TP–CP Ti dowels luted with Panavia F and TR–CP Ti dowels luted with RelyX U100. Tensile strengths were measured in a universal testing machine at a crosshead speed of 0.5 mm/min. The results (N) were statistically analyzed by ANOVA and Tukey tests (α = 0.01).ResultsThe ANOVA indicated that there were significant differences among the groups tested. A Tukey multiple comparison procedure was performed and revealed statistically significant higher retention values for the dowel luted with RelyX U100 when compared with zinc phosphate or Panavia F.ConclusionCast commercially pure titanium dowels and cores fixed with RelyX U100 cement presented superior bond strength retention when compared to zinc phosphate and Panavia F.     

Effect of types of luting agent on push-out bond strength of zirconium oxide posts

ObjectiveThe aim of this study was to investigate the effect of different luting agents on the bond strength of zirconium oxide posts in root canals after artificial ageing.Material and methodsThirty single-rooted extracted teeth were collected. Post spaces were prepared. Custom milled zirconium oxide posts (Cercon, Degudent) were fabricated. Specimens were divided into 3 groups (n = 10), according to the luting agents used: group RA, conventional resin luting agent (RelyX ARC); group RU, self-adhesive resin luting agent (RelyX Unicem); and group Z, zinc phosphate luting agent (DeTrey). Specimens were subjected to thermocycling and water storage at 37 °C. Specimens were horizontally sectioned into three sections and subjected to a push-out test with 0.5 mm/min crosshead speed. The failure mode was assessed by scanning electron microscopy. Data were analysed by using 2-way ANOVA.ResultsThe following bond strength values were obtained: group RA – 8.89 MPa, group RU – 10.30 MPa and group Z – 9.31 MPa. There was no significant difference in bond strength among the groups (P = 0.500). Adhesive failure mode at the cement/post bonded interface was seen in 100%, 66.67% and 83.3% of examined sections in groups RA, RU and Z, respectively. There was no significant difference in bond strength among different root regions (P = 0.367).ConclusionThe type of luting agent had no significant effect on the push-out bond strength of zirconium oxide posts after artificial ageing.Clinical significanceConventional luting agents, such as zinc phosphate cement, seem to provide comparable retention to resin luting agents for cementing custom milled zirconium oxide posts.     

Impact of thermal misfit on shear strength of veneering ceramic/zirconia composites

ObjectivesThermal misfit is discussed as one reason for chipping of veneered zirconia restorations. The aim of the investigation was to assess the effect of thermal misfit on the shear strength of zirconia/veneering ceramic composites.MethodsShear strengths of 12 different veneering ceramic/zirconia composites were measured (n = 10). The veneering ceramics were fired onto polished Y-TZP. In order to create a strong thermal mismatch, one of the veneering ceramics was intended for use on alumina and one for the metal–ceramic technique. The glass transition temperatures of the veneering ceramics and the coefficients of thermal expansion of all ceramics were measured (n = 6). Statistical analysis was performed with one-way ANOVA and a post hoc Bonferroni test (p < 0.05).ResultsShear strength ranged from 21.9 ± 6.2 to 31.0 ± 7.1 MPa. The ceramic for the metal–ceramic technique showed spontaneous debonding. The differences in the coefficients of thermal expansion of core and veneer (Δα) were calculated. In addition the differences between glass transition temperatures of the veneering ceramics and room temperature (ΔT) as the effective temperature range for stress formation were calculated. Highest shear strength was observed when ΔαΔT ≈ 1000 × 10^?6.ConclusionsThermal expansion and glass transition temperature of the veneering ceramic have an impact on the shear strength of veneer/zirconia composites.     

Effect of finishing/polishing techniques and low temperature degradation on the surface topography,phase transformation and flexural strength of ultra-translucent ZrO2 ceramic

ObjectiveTo investigate the effect of different surface finishing and polishing regimes and low temperature degradation on flexural strength, phase transformation and surface topography of ultra-translucent ZrO₂ ceramic.Methods300 (n = 15/group) of conventional zirconia (Z: Ice Zirkon Transluzent) and ultra-translucent zirconia (UT: Prettau Anterior) bar-specimens were made and divided according to the "Finishing/Polishing" - (C — Control, B — diamond rubber polishers, P — adjusting with burs, PB — adjusting with burs + diamond polishers, PG — adjusting with burs + glaze), "Low temperature Degradation (LTD)" (with or without a treatment at 127 °C, 1.7 bar/24 h). Then, a 3-point mini flexural test was performed in a universal testing machine (1 mm/min, 500 kgf load cell). SEM, EDS, XDR, AFM, optical profilometry and Weibull analysis were performed. Data were analyzed by 3-way ANOVA and Tukey’s post-test (5%).ResultsGroups ZPB_D (1670 ± 253 MPa), ZB_D (1664 ± 217 MPa), and ZB (1655 ± 3678 MPa) showed significantly higher flexural strength than the UTPG group (372 ± 56 MPa). The Weibull modulus was significantly higher for the ZP_D group compared to the UB, UC_D, UP_D and UPB_D, while UTB, UTC_D and UTP_D had the lowest value. Monoclinic phases were observed only in the conventional zirconia groups and were more evident after LTD. Diamond rubber polishers presented less roughness for both zirconias.SignificanceThe use of diamond rubber polishers is the most suitable finishing/polishing method for zirconia ceramic restorations and that final glazing reduces the fracture resistance of these materials.     

The effect of a ceramic coating on the cpTi–porcelain bond strength

ObjectivesTo investigate the bond strength between cpTi and low fusing porcelains after different treatments.Methods72 patterns were covered with a ceramic coating and invested with phosphate-bonded material (group A), another 72 were invested with magnesia material (group B) and all cast with cpTi. 31 solid castings were selected from each group. The castings of group B were ground and sandblasted, while the castings of group A were only sandblasted. Aluminum content of the metal surface was determined by EDS and castings were submitted to a 3-point bending test to determine the modulus of elasticity (E). The porcelains Duceratin Plus, Noritake Ti22 and Triceram were applied respectively and specimens were submitted to a 3-point bending test. The fracture mode and the remaining porcelain were determined by optical microscopy and SEM/EDS. Bond strength and fracture mode were calculated by two-way ANOVA.ResultsThe E of groups A and B was 98.3 GPa and 98.6 GPa respectively. The bond strength was 26 ± 3 MPa (Duceratin Plus), 28 ± 3 MPa (Noritake Ti22), 27 ± 2 MPa (Triceram) for group A and 24 ± 1 MPa, 29 ± 2 MPa, 27 ± 1 MPa for group B respectively. No significant differences were found for the same porcelain between the two groups (p < 0.05). A significant difference was found between Duceratin Plus and Noritake Ti22, for group B (p < 0.05). The mode of failure was mainly adhesive for all specimens. A significant reduction in aluminum was recorded in all subgroups.SignificanceThe special coating of patterns makes the Ti casting procedure inexpensive, without reducing the metal–ceramic bond strength.     

Effect of in vitro aging on the flexural strength and probability to fracture of Y-TZP zirconia ceramics for all-ceramic restorations

ObjectivesDental zirconia restorations should present long-term clinical survival and be in service within the oral environment for many years. However, low temperature degradation could affect their mechanical properties and survival. The aim of this study was to investigate the effect of in vitro aging on the flexural strength of yttrium-stabilized (Y-TZP) zirconia ceramics for ceramic restorations.MethodsOne hundred twenty bar-shaped specimens were prepared from two ceramics (ZENO Zr (WI) and IPS e.max^® ZirCAD (IV)), and loaded until fracture according to ISO 6872. The specimens from each ceramic (n_x = 60) were divided in three groups (control, aged for 5 h, aged for 10 h). One-way ANOVA was used to assess statistically significant differences among flexural strength values (P < 0.05). The variability of the flexural strength values was analyzed using the two-parameter Weibull distribution function, which was applied for the estimation of Weibull modulus (m) and characteristic strength (σ₀). The crystalline phase polymorphs of the materials (tetragonal, t, and monoclinic, m, zirconia) were investigated by X-ray diffraction (XRD) analysis, Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy.ResultsA slight increase of the flexural strength after 5 h, and a decrease after 10 h of aging, was recorded for both ceramics, however statistically significant was for the WI group (P < 0.05). Both ceramics presented a t → m phase transformation, with the m-phase increasing from 4 to 5% at 5 h to around 15% after 10 h.SignificanceThe significant reduction of the flexural strength after 10 h of in vitro aging, suggests high fracture probability for one of the zirconia ceramics tested.     

Fatigue testing of two porcelain–zirconia all-ceramic crown systems

ObjectiveTo evaluate the mouth-motion step-stress fatigue behavior of two porcelain–zirconia all-ceramic crown systems.MethodsThe average dimensions of a mandibular first molar crown were imported into CAD software; a tooth preparation was modeled by reducing proximal walls by 1.5 mm and occlusal surface by 2.0 mm. The CAD-based tooth preparation was made by rapid prototyping and used as a master die to fabricate all-ceramic crowns with 1.0 mm porcelain veneered on 0.5 mm Y-TZP cores (LAVA veneer + LAVA frame, 3M/ESPE, and Vita veneer + CERCON frame, Dentsply). Crowns were cemented on aged (60 days in water) composite (Z100, 3M/ESPE) reproductions of the die. Three crowns from the LAVA group were subjected to single cycle load to failure for stress profile design; remainder subjected to step-stress mouth-motion fatigue (three step-stress profiles). All mechanical testing was performed by sliding a WC indenter of 6.25 mm diameter 0.7 mm lingually down the mesio-distal cusp. Master Weibull curves and reliability for missions of 50,000 cycles at 200 N load were calculated (Alta Pro 7, Reliasoft).ResultsSingle load to failure showed fractures through the zirconia core. Reliability for a 200 N × 50K cycle mission was not significantly different between systems. In fatigue, failure occurred by formation of large chips within the veneer originating from the contact area without core exposure.ConclusionsLAVA and CERCON ceramic systems present similar fatigue behavior; fatigue loading of both systems reproduces clinically observed failure modes.     

Innovations in bonding to zirconia-based materials. Part II: Focusing on chemical interactions

ObjectivesThe zirconia–resin bond strength was enhanced using novel engineered zirconia primers in combination with selective infiltration etching as a surface pre-treatment. The aim of this study was to evaluate the effect of artificial aging on the chemical stability of the established bond and to understand the activation mechanism of the used primers.MethodsSelective infiltration etched zirconia discs (Procera; NobelBiocare) were coated with one of four novel engineered zirconia primers containing reactive monomers and were bonded to resin-composite discs (Panavia F2.0). Fourier transform infrared spectroscopy (FT-IR) was carried out to examine the chemical activation of zirconia primers from mixing time and up to 60 min. The bilayered specimens were cut into microbars (1 mm² in cross-section area) and zirconia–resin microtensile bond strength (MTBS) was evaluated immediately and after 90 days of water storage at 37 °C. Scanning electron microscopy (SEM) was used to analyze the fracture surface.ResultsThere was a significant drop in MTBS values after 90 days of water storage for all tested zirconia primers from ca. 28–41 MPa to ca. 15–18 MPa after completion of artificial aging. SEM revealed increase in percentage of interfacial failure after water storage. FTIR spectra suggested adequate activation of the experimental zirconia primers within 1 h of mixing time.SignificanceThe novel engineered zirconia primers produced initially high bond strength values which were significantly reduced after water storage. Long-term bond stability requires developing more stable primers.     

Effect of pulpal pressure on the microtensile bond strength of luting resin cements to human dentin

ObjectivesThe objectives of this study were to examine the effect of pulpal pressure on the microtensile bond strength (mTBS) of luting resin cements to human dentin and the permeability of dentin surfaces pre-treated with an adhesive and a self-etching primer.MethodsCylindrical composite blocks were luted with resin cements (RelyX ARC, 3M ESPE: ARC; Panavia F, Kuraray Medical Inc.: PF; RelyX Unicem, 3M ESPE: UN) in the absence or presence of simulated pulpal pressure. The application of Adper Single Bond 2 (3M ESPE) and ED primer 2.0 (Kuraray) was performed under 0 cm H₂O. After each resin cement was applied, the pulpal pressure group was subjected to 20 cm H₂O of hydrostatic pressure for 10 min during the initial setting period. Testing for mTBS was performed on 0.9 mm × 0.9 mm sectioned beams after 24 h water-storage. Scanning electron microscopy was performed to investigate the fractured surfaces after mTBS testing and additional dentin surfaces that were treated by an etchant, ED primer 2.0 and UN. Fluid permeability was measured on dentin surfaces that were applied with Adper Single Bond 2 and ED primer 2.0.ResultsApplication of pulpal pressure reduced mTBS significantly in groups ARC and PF. Porous bonding interfaces due to water permeability through the cured adhesive were observed on fractured surfaces. Dentin surfaces that were applied with the adhesive and the primer were more permeable than smear layer-covered dentin. The mTBS of UN was significantly lower than ARC and PF regardless of the absence/presence of pulpal pressure.SignificanceFluid permeation during the initial setting period deteriorated the bonding quality of resin cements.     

Effect of silane and MDP-based primers on physico-chemical properties of zirconia and its bond strength to resin cement

ObjectiveTo evaluate the effect of surface treatments on yttria-tetragonal zirconia polycrystal (Y-TZP) characteristics and on resin-mediated zirconia bond.MethodsY-TZP slabs were grit blasted with 45 μm alumina or with 30 μm silica-coated alumina particles. The chemical treatments were: no-chemical treatment (NC), silane-containing primer (SP), MDP (10-Methacryloyloxydecyl dihydrogen phosphate) and silane-containing primer (MPS), MDP-containing primer (MP) and MDP and silane-containing adhesive (MPA). Contact angle as a function of surface roughness (θ_m) and surface roughness parameter (Sdr) were measured using Fringe Projection Phase Shifting (FPPS). Surface free energy (γ_s^TOT) was calculated with a goniometer. Chemical interaction between primers/adhesive and zirconia was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS). Resin cement microshear bond strength (μSBS) was analyzed at either 24-h or 8-months water storage (37 °C). θ_m values, Sdr values, γ_s^TOT and μSBS values were analyzed using Analysis of variance (ANOVA) and post hoc Tukey test (α = 0.05).ResultsChemical treatment had an effect (p < 0.001) on all surface parameters analyzed: θ_m, γ_s^TOT and Sdr. MP-treated group showed higher incidence of P–O–Zr bonds than the other groups, indicating more chemical linkages. Grit blasting (p < 0.001) and the interaction chemical treatment*storage (p < 0.001) did not affect μSBS; all silane-containing primers showed significant drop in μSBS after aging.SignificanceMDP and/or silane-based solutions affect the physicochemical properties of blasted-zirconia. An MDP-based primer is fundamental to achieve a stable resin-zirconia bonding, but the chemical reactivity of MDP is impaired when this molecule is present in a multicomponent system.     

Surface characterization of dental ceramics and initial streptococcal adhesion in vitro

ObjectivesThe aim of this in vitro study was to investigate the surface properties of dental ceramic materials belonging to different ceramic classes, and to correlate the findings to the initial adherence of three oral streptococcal strains.MethodsRectangular specimens were prepared from different ceramic materials (glass/lithium disilicate glass/glass-infiltrated zirconia/partially sintered zirconia/hipped zirconia ceramic) and polished; surface roughness (Ra) was determined. Glass plates were used as a control. Specimens were incubated with phosphate-buffered saline or an artificial saliva (protein mixture; 2 h, 37 °C). Surface free energy (γ^t) and its polar (γ^p) and disperse (γ^d) contribution were determined prior to and after artificial saliva exposure. Uncoated and protein-coated specimens were incubated with Streptococcus gordonii DSMZ 6777, Streptococcus oralis DSMZ 20068 or Streptococcus sanguinis DSMZ 20068 suspension for 2.5 h at 37 °C (n = 15 for each treatment and strain). Adherent streptococci were quantified fluorometrically.ResultsThe lithium disilicate glass ceramic showed the highest values for Ra; the lowest values were found for the glass ceramic, the partially sintered zirconia and the hipped zirconia ceramic. Protein coating caused a significant increase in γ^t and γ^p, but not in the control material. The control material showed higher values for streptococcal adhesion than all ceramic materials. After protein coating, only slight and random differences in streptococcal adhesion were found between the various ceramic materials.SignificanceDental ceramic materials show differences in terms of Ra, γ^t and initial streptococcal adhesion; however, correlations between surface properties and streptococcal adhesion were poor.     

Influence of curing modes on the degree of conversion and mechanical parameters of dual-cured luting agents

PurposeTo investigate the effects of different curing modes, including tack cure, on the degree of conversion (DC) and mechanical parameters of dual-cured luting agents for all-ceramic restorations.MethodsImmediate light curing, intermittent light curing (2-s tack cure and a 1-min interval before the main cure), delayed light cuing (2-min delay) and chemical or no light curing were used to cure two dual-cured luting agents, RelyX Unicem and PermaCem 2.0, through a 1.5-mm thick lithium disilicate ceramic slide. DC (n = 3), micro-hardness (n = 5), shrinkage strain (n = 4) and shrinkage stress (n = 3) were measured under the aforementioned curing modes. The data were analyzed using two-way ANOVA and post-hoc Tukey HSD test, with the level of significance set at α = 0.05.ResultsFor both luting agents, all the light-curing modes produced similar final DC, but using chemical cure only could significantly reduce the DC. The mechanical parameters followed a similar pattern. There were positive but nonlinear correlations between DC and the other mechanical parameters, with the increase in these parameters with DC being slower initially.ConclusionsProvided adequate light curing is applied to a dual-cured luting agent, delaying the light curing or using a tack cure first to facilitate seating of a restoration may not have a significant impact on the luting agent’s final degree of conversion. However, using chemical cure only may result in inadequate cure of the luting agent and is recommended only for highly opaque restorations.