Effect of cleaning protocol on silica deposition and silica-mediated bonding to Y-TZP

ObjectivesTo evaluate the effect of cleaning methods on the deposition of silica on yttria-stabilized zirconium dioxide (Y-TZP) surface and on the silane-silica mediated bond strength between Y-TZP and resin cement.MethodsY-TZP slabs were air-abraded with 30 μm silica-coated alumina particles and distributed in three groups: no cleaning, cleaning with a stream of oil-free air/water spray for 5 s and cleaning with an ultrasonic bath in water for 10 min. The distribution of Si on the Y-TZP surfaces was recorded using energy dispersive spectroscopy (EDS). After the treatment was applied, Y-TZP slabs (n = 20) received a primer application and resin cement cylinders were built on the surface. After storage (24 h) in water storage or 3 months plus thermocycling; n = 10), microshear bond strength test (μSBS) was performed. X- ray Photoelectron Spectroscopy (XPS) characterized the chemical bonds between the silica layer and the silane-containing primer. Data were analyzed using ANOVA and Tukey test, as well as Weibull analysis (α = 0.05).ResultsCleaning method had a significant effect on the amount of Si deposited on zirconia surface (p < 0.001) and, consequently, on bond strength (p < 0.001). Storage/aging also had a significant effect on bond strength (p < 0.001). Low values of Weibull moduli for bond strength were observed for all groups after aging. XPS showed silane-silica chemical interaction for all groups.SignificanceThe silica deposited by tribochemical coating to Y-TZP was removed by the cleaning methods evaluated, compromising bond strength. Stability of the bonding is also a concern when no cleaning method is applied.     

Acidic pH weakens the bonding effectiveness of silane contained in universal adhesives

Objectives

Some silane-containing universal adhesives were introduced that a separate ceramic primer was unnecessary to glass-ceramic bonding because of incorporated silane. We aimed to investigate the effectiveness of silane in universal adhesives with acidic media.

Surface characterisation and bonding of Y-TZP following non-thermal plasma treatment

Objectives(1) To chemically characterise Y-TZP surface via X-ray photoelectron spectroscopy (XPS) and evaluate the surface energy levels (SE) after non-thermal plasma (NTP). (2) To test the microtensile bond strength (MTBS) of Y-TZP bonded to cured composite disks, after a combination of different surface conditioning methods.MethodsTwenty-four Y-TZP discs (13.5 mm × 4 mm) were obtained from the manufacturer and composite resin (Z-100) discs with similar dimensions were prepared. All discs were polished to 600 grit and divided into 8 groups (n = 3 disks each), four control (non-NTP treated) and four experimental (NTP treated for 10 s) groups. All groups received one of the four following treatments prior to cementation with Rely × Unicem cement: sand-blasting (SB), a Clearfil ceramic primer (MDP), sand-blasting + MDP (SBMDP), or baseline (B), no treatment. SE readings and surface roughness parameters were statistically analysed (ANOVA, Tukey's, p < 0.05). Mixed model and paired samples t-tests were used to compare groups on MTBS.ResultsXPS showed increase in O and decrease in C elements after NTP. The polar component increased for BP (42.20 mN/m) and SBP (43.77 mN/m). MTBS values for groups BP (21.3 MPa), SBP (31 MPa), MDPP (30.1 MPa) and SBMDPP (32.3 MPa) were significantly higher in specimens treated with NTP than their untreated counterparts B (9.1 MPa), SB (14.4 MPa), MDP (17.8 MPa) and SBMDP (24.1 MPa).Conclusions(1) Increase of O and decrease of C led to higher surface energy levels dictated by the polar component after NTP; (2) NTP application increased MTBS values of Y-TZP surfaces.     

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.     

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.     

Graded structures for damage resistant and aesthetic all-ceramic restorations

ObjectivesClinical studies revealed several performance deficiencies with alumina- and zirconia-based all-ceramic restorations: fracture; poor aesthetic properties of ceramic cores (particularly zirconia cores); and difficulty in achieving a strong ceramic–resin-based cement bond. We aim to address these issues by developing a functionally graded glass/zirconia/glass (G/Z/G) structure with improved damage resistance, aesthetics, and cementation properties.MethodsUsing a glass powder composition developed in our laboratory and a commercial fine zirconia powder, we have successfully fabricated functionally graded G/Z/G structures. The microstructures of G/Z/G were examined utilizing a scanning electron microscopy (SEM). The crystalline phases present in G/Z/G were identified by X-ray diffraction (XRD). Young's modulus and hardness of G/Z/G were derived from nanoindentations. Critical loads for cementation radial fracture in G/Z/G plates (20 mm × 20 mm, 1.5 or 0.4 mm thick) bonded to polycarbonate substrates were determined by loading with a spherical indenter. Parallel studies were conducted on homogeneous yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) controls.ResultsThe G/Z/G structure consists of an outer surface aesthetic glass layer, a graded glass–Y-TZP layer, and a dense Y-TZP interior. The Young's modulus and hardness increase from surface to interior following power-law relations. For G/Z/G plates of 1.5 and 0.4 mm thick, critical loads for cementation radial fracture were 1990 ± 107 N (mean ± S.D., n = 6) and 227 ± 20 N (mean ± S.D., n = 6), respectively, which were ～30 and 50% higher than those for their monolithic Y-TZP counterparts (1388 ± 90 N for 1.5 mm and 113 ± 10 N for 0.4 mm thick; mean ± S.D., n = 6 for each thickness). A 1-sample t-test revealed significant difference (p < 0.001) in critical loads for radial fracture of G/Z/G and homogeneous Y-TZP for both specimen thicknesses.SignificanceOur results indicate that functionally graded G/Z/G structures exhibit improved damage resistance, aesthetics, and potentially cementation properties compared to homogeneous Y-TZP.     

Thermo and mechanical cycling and veneering method do not influence Y-TZP core/veneer interface bond strength

ObjectivesThe purpose of this study was to evaluate the influence of thermal and mechanical cycling and veneering technique on the shear bond strength of Y-TZP (yttrium oxide partially stabilized tetragonal zirconia polycrystal) core–veneer interfaces.Materials and methodsCylindrical Y-TZP specimens were veneered either by layering (n = 20) or by pressing technique (n = 20). A metal ceramic group (CoCr) was used as control (n = 20). Ten specimens for each group were thermal and mechanical cycled and then all samples were subjected to shear bond strength in a universal testing machine with a 0.5 mm/min crosshead speed. Mean shear bond strength (MPa) was analysed with a 2-way analysis of variance and Tukey's test (p < 0.05). Failure mode was determined using stereomicroscopy and scanning electron microscopy (SEM).ResultsThermal and mechanical cycling had no influence on the shear bond strength for all groups. The CoCr group presented the highest bond strength value (p < 0.05) (34.72 ± 7.05 MPa). There was no significant difference between Y-TZP veneered by layering (22.46 ± 2.08 MPa) or pressing (23.58 ± 2.1 MPa) technique. Failure modes were predominantly adhesive for CoCr group, and cohesive within veneer for Y-TZP groups.ConclusionsThermal and mechanical cycling, as well as the veneering technique does not affect Y-TZP core–veneer bond strength.Clinical significanceDifferent methods of veneering Y-TZP restorations would not influence the clinical performance of the core/veneer interfaces.     

Effects of extreme cooling methods on mechanical properties and shear bond strength of bilayered porcelain/3Y-TZP specimens

ObjectivesThis study investigated the effect of extreme cooling methods on the flexural strength, reliability and shear bond strength of veneer porcelain for zirconia.MethodsVita VM9 porcelain was sintered on zirconia bar specimens and cooled by one of the following methods: inside a switched-off furnace (slow), at room temperature (normal) or immediately by compressed air (fast). Three-point flexural strength tests (FS) were performed on specimens with porcelain under tension (PT, n = 30) and zirconia under tension (ZT, n = 30). Shear bond strength tests (SBS, n = 15) were performed on cylindrical blocks of porcelain, which were applied on zirconia plates. Data were submitted to one-way ANOVA and Tukey's post hoc tests (p < 0.05). Weibull analysis was performed on the PT and ZT configurations.ResultsOne-way ANOVA for the PT configuration was significant, and Tukey's test revealed that fast cooling leads to significantly higher values (p < 0.01) than the other cooling methods. One-way ANOVA for the ZT configuration was not significant (p = 0.06). Weibull analysis showed that normal cooling had slightly higher reliability for both the PT and ZT configurations. Statistical tests showed that slow cooling decreased the SBS value (p < 0.01) and showed less adhesive fracture modes than the other cooling methods.Clinical SignificanceSlow cooling seems to affect the veneer resistance and adhesion to the zirconia core; however, the reliability of fast cooling was slightly lower than that of the other methods.     

Making yttria-stabilized tetragonal zirconia translucent

ObjectiveThe aim of this study was to provide a design guideline for developing tetragonal yttria-stabilized zirconia with improved translucency.MethodsThe translucency, the in-line transmission in particular, of 3 mol.% yttria-stabilized tetragonal zirconia (3Y-TZP) has been examined using the Rayleigh scattering model. The theory predicts that the in-line transmission of 3Y-TZP can be related to its thickness with grain size and birefringence the governing parameters. To achieve a threshold value of translucency, the critical grain size of 3Y-TZP was predicted for various thicknesses (0.3–2.0 mm). The threshold value was defined by a measured average in-line transmission value of a suite of dental porcelains with a common thickness of 1 mm. Our theoretical predictions were calibrated with one of the very few experimental data available in the literature.ResultsFor a dense, high-purity zirconia, its in-line transmission increased with decreasing grain size and thickness. To achieve a translucency similar to that of dental porcelains, a nanocyrstalline 3Y-TZP structure was necessitated, due primarily to its large birefringence and high refractive index. Such a grain size dependence became more pronounced as the 3Y-TZP thickness increased. For example, at a thickness of 1.3 mm, the mean grain size of a translucent 3Y-TZP should be 82 nm. At 1.5 mm and 2 mm thicknesses, the mean grain size needed to be 77 nm and 70 nm, respectively.SignificanceA promising future for zirconia restorations, with combined translucency and mechanical properties, can be realized by reducing its grain size.     

Impact of high-speed sintering,layer thickness and artificial aging on the fracture load and two-body wear of zirconia crowns

ObjectiveTo investigate the impact of high-speed sintering, layer thickness and artificial aging in a chewing simulator on the fracture load (FL) and two-body wear (2BW) of 4Y-TZP crowns.Methods4Y-TZP crowns (Ceramill Zolid HT+, Amann Girrbach AG) in three different layer thicknesses (0.5, 1.0, 1.5; N = 192, n = 64/group) were manufactured using CAD/CAM technology and sintered at 1580 °C (high-speed sintering) or 1450 °C (control group). Specimens were polished in two-steps and bonded to standardized CoCr abutments with Multilink Automix (Ivoclar Vivadent). 2BW after 6000 thermo- and 1,200,000 chewing-cycles employing enamel antagonists was determined using best fit machining. FL was tested before and after artificial aging. Univariate ANOVAs, post hoc Scheffé, unpaired t-, Kruskal–Wallis- and Mann–Whitney-U-test were computed (p < 0.05).ResultsHigh-speed sintering resulted in less 2BW of the zirconia than the control group (p = 0.013). High-speed sintering (p = 0.001–0.006) and an increase in layer thickness (p < 0.001–0.012) resulted in higher FL values, while artificial aging led to a reduction of FL (p < 0.001).SignificanceAs high-speed sintering resulted in less two-body wear of the zirconia and comparable or even higher fracture load results than the control group, this cost- and time efficient alternative presents promising mechanical results.     

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.     

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.     

Translucency,flexural strength,fracture toughness,fracture load of 3-unit FDPs,Martens hardness parameter and grain size of 3Y-TZP materials

ObjectiveThis investigation tested pre-shaded 3Y-TZP materials on optical, mechanical and structural properties and calculated correlations between these properties.MethodsSeven A2-shaded 3Y-TZP zirconia materials were investigated on translucency (T) via UV–vis-spectrophotometer, fracture load of 3-unit FDPs (FL), biaxial flexural strength (FS), Chevron-Notch Beam (CNB), fracture toughness (K_IC) and Martens parameter (hardness: HM and indentation modulus: E_IT). FL, FS and K_IC were measured in a universal testing machine. The grain size was evaluated by scanning electron microscopy (SEM). Data was analyzed using one-way ANOVA followed by post hoc Scheffé, Kruskal–Wallis-, Mann–Whitney-U- and Pearson-test (p < 0.05).ResultsFor translucency, negative correlations were found with results of facture load (R = −0.444, p < 0.001) and K_IC (R = −0.503, p < 0.001). While a positive correlation was found between translucency and flexural strength (R = 0.238, p = 0.019), between fracture load and E_IT (R = 0.227, p < 0.029), between fracture load and K_IC (R = 0.362, p < 0.001) as well as between fracture load and the grain size (R = 0.598, p = 0.007). While the grain size positively correlated with E_IT (R = 0.534, p = 0.017) as well as E_IT with HM (R = 0.720, p < 0.001).SignificanceDespite of being based on the same raw material, tested zirconia materials significantly differed regarding optical, mechanical (except biaxial flexural strength and Martens hardness) and structural properties. Materials with highest optical properties were those with lowest mechanical properties (CER, COP).     

Indentation size effect of Y-TZP dental ceramics

ObjectiveThe purpose of this study was to investigate and analyze the indentation size effect (ISE) in Vickers hardness of monolithic yttria partially stabilized zirconia (Y-TZP) dental ceramics without and with the addition of dental dye A3. The ISE is analyzed using the Mayer law, a proportional specimen resistance (PSR) model and a modified proportional specimen resistance (MPSR) model.MethodsTwo samples of Y-TZP dental ceramics, trade names BruxZir (provided by Glidewell Laboratories, CA, USA), were investigated. The first sample was polished Y-TZP and the second sample was polished Y-TZP with the addition of dental dye A3, by VITA Classical Shade Guide. The Vickers hardness was measured under the following loads: 0.49 N, 0.98 N, 1.96 N, 4.90, 9.81 N and 29.42 N. Thirty indentations were made on each sample, under each load. Relationships between the applied load, F, and the resulting indentation size, d, have been analyzed by the Mayer law, the PSR model and the MPSR model.ResultsThe Meyer index (n) for both Y-TZP dental ceramics is less than 2, which indicates that hardness is dependent on test loads. The PSR model and the MPSR model were used to calculate “true” Vickers hardness or load-independent hardness.SignificanceAll applied mathematical models are suitable for the data analysis, which is confirmed with high correlation coefficients, but the best correlation between measured values and mathematical models was achieved with the MPSR model with a correlation coefficient of 0.9999.     

Effect of sintering time on biaxial strength of zirconium dioxide

ObjectivesAim of this study was to evaluate effect of sintering time on mechanical properties of yttrium partially stabilized zirconia (Y-TZP) (ICE Zirkon, ZirkonZahn, Italy).MethodsFifty-six zirconia discs were divided into two groups. Discs of the first group were sintered in sintering oven (ZirkonZahn) at 20–1500 °C temperature using rise time of 3 h and kept at 1500 °C for 2 h. Discs of the second group were sintered at 20–1500 °C using rise time of 1 h 40 min and kept at 1500 °C for 1 h. Half of the discs (n = 15) from both groups were thermocycled in distilled water for 20 000 cycles (5–55 °C). Biaxial flexural strength of the discs (diameter 19.0 mm, thickness 1.6 mm) were measured dry at room temperature. Surface microhardness (VHN) was also measured. X-Ray diffraction analysis was performed to evaluate the ratio of tetragonal to monoclinic phase in thermocycled discs. The data was calculated using Weibull and ANOVA analysis.ResultsNo statistically significant difference (p > 0.05) was found between the groups in terms of sintering time or thermocycling. The biaxial flexural strength of the groups varied from 995 MPa to 1127 MPa. Surface microhardness varied from 1478 to 1532. The relative amount of the monoclinic phase was higher when zirconia was thermocycled and stored in water compared to control discs, which had no monoclinic phase at all.SignificanceVariation in the sintering time from 1.6 h to 3.0 h did not influence mechanical properties of Y-TZP zirconia.     

Mechanical properties,aging stability and translucency of speed-sintered zirconia for chairside restorations

ObjectiveTo evaluate the performance of zirconia ceramics sintered in a speed sintering induction furnace by comprehensive understanding of their optical and mechanical properties, microstructure, phase composition and aging stability, in comparison to ceramics sintered in a conventional furnace.MethodsSpeed sintered (SS) Katana STML_SS (Kuraray Noritake) (total thermal cycle/sintering time/dwell temperature: 30 min/16 min/1560 °C) and CEREC Zirconia (CEREC Zr_SS) (Dentsply Sirona) (15 min/2 min/1578 °C) were compared to conventionally sintered (CS) Katana STML_CS (6.8 h/2 h/1550 °C) and inCoris TZI_CS (4 h/2 h/1510 °C). The translucency parameter (TP) and contrast ratio (CR) were measured with a spectrophotometer. The chemical composition of the materials was determined by XRF and phase composition was characterized using XRD. Hydrothermal aging behavior was evaluated by measuring the tetragonal-to-monoclinic ZrO₂ phase transformation after accelerated hydrothermal aging in steam at 134 °C. The indentation fracture toughness, Vickers hardness and biaxial strength of the sintered ceramics were assessed.ResultsSpeed and conventionally sintered zirconia revealed similar density, microstructure, average strength and hydrothermal aging stability. Both Katana STML_SS/CS 5Y-PSZ ceramics were characterized with a higher content of cubic phase (≈53 wt%), which resulted in a higher amount of Y₂O₃ in the remaining tetragonal ZrO₂ phases compared to the 3Y-TZP CEREC Zr_SS and inCoris TZI_CS (8 and 20 wt%, respectively). The sintering program did not affect the hydrothermal aging behavior of Katana STML_SS and CEREC Zr_SS. TP of Katana STML_SS (TP ≈ 32) was not affected by speed sintering, while the translucency of CEREC Zr_SS (TP = 14) was significantly reduced. Hardness, fracture toughness and Weibull characteristic strength of Katana STML_SS and CEREC Zr_SS also reached the optimal level, but speed sintering substantially lowered their mechanical reliability.SignificanceSpeed sintering of 3Y-TZP and 5Y-PSZ in a speed sintering induction oven appeared suitable for clinical applications. However, further studies should focus on improving of translucency and mechanical reliability of the speed-sintered zirconia ceramics.     

Importance of tetragonal phase in high-translucent partially stabilized zirconia for dental restorations

ObjectivesFor the use of partially stabilized zirconia (PSZ) as high-translucent zirconia, the importance of cubic phase (c-ZrO₂) is commonly emphasized without much attention for the remaining tetragonal phase (t-ZrO₂). The aim is to understand whether the crystal structure and microstructure of t-ZrO₂ have paramount influences on the properties of PSZ.MethodsTwo grades of 5 mol% yttria-stabilized PSZ ceramics were prepared by different processing routes. A 5 mol % yttria co-precipitated zirconia (T5Y) was compared with a 3 and 8 mol% yttria-stabilized powder mixture grade with a bimodal grain size distribution (B5Y). The phase composition and lattice parameters were studied with x-ray diffraction (XRD) and Rietveld analysis. Mechanical properties were compared in terms of hardness, toughness and biaxial bending strength with Weibull analysis. Their translucency and aging stability were also characterized, and the microstructure before and after aging were followed by scanning electron microscopy (SEM).ResultsT5Y and B5Y having similar phase composition (about 40% t- and 60% c-ZrO₂) showed the same basic properties (density, hardness and toughness), but the lattice parameters of t-ZrO₂ and the concomitant microstructure were completely different. The t-ZrO₂ phase in T5Y had a higher yttria content and a lower tetragonality (c/a) of 1.0126 ± 0.0002, whereas the t-ZrO₂ phase in B5Y was comparable to that in conventional 3Y-TZPs with a tetragonality of 1.0153 ± 0.0002. Consequently, B5Y showed a lower strength with lower Weibull modulus, being less translucent and more aging susceptible as compared to T5Y. The translucency and aging susceptibility of B5Y were even comparable to those of conventional 3Y-TZP.SignificanceNot only the phase composition with high cubic phase content but also the lattice parameters and the yttria content in the remaining t-ZrO₂ played a determinant role for PSZs to be used as ‘high-translucent’ zirconia.     

Effect of loading conditions on the fracture toughness of zirconia

PurposeA Vickers hardness indenter was pressed into yttria-stabilized zirconia (Y-TZP) by the indentation fracture method (IF method).MethodsThe effect on the calculated Vickers hardness, fracture toughness values, and indentation fracture load (9.8, 49, 98, 196, and 294 N) was examined to deduce the optimum conditions of the IF method. Calculated Vickers hardness and fracture toughness values were analyzed with one-way analysis of variance and then multiple comparisons (Scheffe). The appearance of on indentation and cracks was also evaluated using a scanning electron microscopy (SEM).ResultsIndentation of Y-TZP was generated by 9.8 and 49 N of indentation fracture load, however cracks could not be confirmed with the microscope attached to the Vickers hardness tester. Both indentation and cracks were observed at 98, 196 and 294 N of indentation fracture load obtained values of 7.1 and 6.8 MPam^1/2. Cracks noted at the 98 N were not clear, whereas the 196 and 294 N showed especially clear cracks. Due to the hardness of zirconia and the light loads, fracture toughness values for 9.8, 49, and 98 N could not be calculated. There was no significant difference between 196 and 294 N, when calculated fracture toughness values were analyzed with multiple comparisons. SEM revealed clear indentation and cracks, that extended linearly, but no chips or fractures were observed. Surface changes were observed at 196 and 294 N that are presumed to be accompanied by phase transition around the cracks.ConclusionsOptimum experimental conditions of the indentation fracture load in the IF method were determined as 196 and 294 N.     

Evaluation of the interaction of chlorhexidine and MDP and its effects on the durability of dentin bonding

ObjectiveThis study aimed to evaluate the potential interaction of chlorhexidine (CHX) and 10-methacryloyloxydecyl dihydrogen phosphate (MDP) and its effects on the durability of dentin bonding.MethodsTwo commercial adhesives were tested: a MDP-free adhesive (Single Bond 2, SB2) and a MDP-containing adhesive (Single Bond Universal, SBU). Teeth were randomly assigned to six groups and tested for micro-tensile bond strength (μTBS): Ctr, direct bonding with SB2; CHX, CHX conditioning and SB2; MDP, MDP conditioning and SB2; CHX + MDP, combined CHX and MDP conditioning and SB2; SBU, direct bonding with SBU; CHX + SBU, CHX conditioning and SBU. The potential interaction of CHX and MDP was assessed by measuring nanoleakage, in situ zymography, and chemoanalytic characterization via Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and nuclear magnetic resonance (NMR). Specimens for μTBS and nanoleakage tests were first subjected to water storage for 24 h or 6 months.ResultsThe initial μTBS values of the Ctr and CHX groups were significantly lower than those of the other four groups (P < 0.05). Water storage for 6 months significantly weakened all groups (P < 0.05), with the Ctr group showing the lowest μTBS. This group also showed more obvious nanoleakage than the other five groups. In situ zymography revealed that the Ctr group showed the strongest fluorescence and that the CHX + MDP group showed greater fluorescence than either CHX or MDP group. FTIR, XPS, and NMR indicated that MDP can interact with hydroxyapatite. NMR detected no Ca²⁺ salt peak for MDP when it was combined with CHX.SignificanceThe application of either CHX or MDP alone can improve dentin bond durability. However, CHX may interfere with the formation of MDP–Ca salts.     

Effect of water aging on microtensile bond strength of dual-cured resin cements to pre-treated sintered zirconium-oxide ceramics

ObjectivesTo evaluate the hydrolytic stability of different dual-cure resin cements when luted to zirconia ceramic.MethodsEighteen cylinder-shaped zirconia blocks (Cercon Zirconia, Dentsply) were conditioned with: Group 1, no treatment; Group 2, sandblasting (125 μm alumina–Al₂O₃-particles); Group 3, tribochemical silica coating (50 μm silica-modified Al₂O₃ particles). Ceramic blocks were duplicated in composite resin (Tetric Evo Ceram, Ivoclar-Vivadent). Composite disks were luted to pre-treated ceramic surfaces using: (1) Clearfil Esthetic Cement (CEC; Kuraray); (2) Rely X Unicem (RXU; 3M ESPE); (3) Calibra (CAL; Dentsply Caulk). After 24 h, bonded samples were cut into microtensile sticks (1 mm²). Half of the sticks were loaded in tension until failure (cross-head speed of 0.5 mm/min). The remaining half was tested after 6 months of water storage at 37 °C. Data was analyzed with three-way ANOVA and Tukey’s test (P <0.05). Fractographic analysis was performed by SEM.ResultsAfter 24 h, bond strength of CEC to zirconia was significantly higher than that of RXU and CAL, independently from the ceramic pre-treatment (P <0.001). Using CAL, all samples failed prematurely except when luting to sandblasted surfaces. After 6 months of water aging, bond strength of CEC significantly decreased. RXU did not significantly alter bond strengths. Adhesion of sandblasted specimens luted with CAL fell over time. Micromorphological alterations were evident after water storage.SignificanceResin–ceramic interfacial longevity depended on cement selection rather than on surface pre-treatments. CEC and RXU were both suitable for luting zirconia. Water aging played an important role in the durability of zirconia-to-composite chemical bonds.