Preparation and filling of small oval root canals: influence of file system and sealer.

OBJECTIVE: To carry out a morphometric analysis of small oval root canals prepared with different instruments (part 1) and filled with different sealers (part 2). METHOD AND MATERIALS: Ninety extracted mandibular incisors with small oval root canals were instrumented with Self-Adjusting File (n = 45), XP-endo Finisher (n = 15), GentleFile (n = 15), or Reciproc (n = 15). All groups of part 1 were filled with AH Plus (n = 15 each). For part 2 (including group Self-Adjusting File/AH Plus) teeth instrumented with Self-Adjusting File were additionally filled with GuttaFlow Bioseal (n = 15) or Total Fill BC sealer (n = 15). All sealers were placed with a lentulo and filled with master point and additional points. Serial cuts were made at 1-mm intervals up to 10 mm. Total root canal area, percentage of gutta-percha filled area (PGFA), sealer, voids, and debris were evaluated using interactive image analysis software. RESULTS: Preparation with Reciproc caused significantly wider canals than with Self-Adjusting File, GentleFile, or XP-endo Finisher, but also resulted in the greatest PGFA and lowest percentage of sealer (P ≤ .05). Following XP-endo Finisher, the significantly greatest percentage of debris (30%) was found 1 mm from the apex (P ≤ .05). Regarding different sealers, only minor differences were found (GuttaFlow Bioseal: less percentage of sealer at 2 and 3 mm levels [P ≤ .05]). CONCLUSION: Within the limits of this study Reciproc caused the greatest substance loss, but also the most favorable PGFA. The apical debris accumulation with XP-endo Finisher needs further investigation. The sealers under investigation performed equally well.

Evaluation of wear behavior of dental restorative materials against zirconia in vitro.

OBJECTIVES: To evaluate two-body wear (2BW) and three-body wear (3BW) of different CAD/CAM and direct restorative materials against zirconia using a dual-axis chewing simulator and an ACTA wear machine. METHODS: 3 CAD-CAM resin-based composite or polymer infiltrated ceramic network blocs, 1 lithium disilicate CAD-CAM ceramic (LS2), 3 direct resin composites, amalgam and bovine enamel were tested. For 2BW, 8 flat specimens per material were produced, grinded, polished, stored wet (37 °C, 28d) and tested (49 N, 37 °C, 1,200,000 cycles) against zirconia. For 3BW, specimens (n = 10) were stored accordingly, and tested against a zirconia antagonist wheel (3Y-TZP, d = 20 mm, h = 6 mm; 200,000 cycles, F = 15 N, f = 1 Hz, 15% slip) in millet seed suspension. Wear resistance was analysed in a 3D optical non-contact profilometer, measuring vertical wear depth and volume loss for 2BW and mean wear depth and roughness (Ra) for 3BW. Vickers hardness (15 s, HV2) was measured. Statistical analysis was performed using non-parametric tests (Mann-Whitney-U test, p < 0.05). RESULTS: 2BW and 3BW have a different impact on material surfaces. Similar wear resistance was observed for direct and indirect resin based materials with analogous filler configurations in both methods. Bovine enamel exhibited the best wear resistance in 2BW, but the least wear resistance in 3BW against zirconia. Regarding 2BW, a direct/indirect composite material pair of the same manufacturer showed the significantly highest mean volume losses (2.72/2.85 mm³), followed by LS2 (1.41 mm³). LS2 presented the best wear resistance in 3BW (mean wear depth 2.85 µm), combined with the highest mean Vickers hardness (598 MPa). No linear correlation was found between Vickers hardness and both wear testing procedures. The zirconia antagonists showed no recordable signs of wear. SIGNIFICANCE: Dental restorative materials behave differently in 2BW and 3BW laboratory testing. Vickers hardness testing alone cannot hold for a correlation with wear behavior of materials. Micromorphological investigation of material composition can reveal insights in wear mechanisms related to variations in filler technologies.

Influence of Simulated Oral Conditions on Different Pretreatment Methods for the Repair of Glass-Ceramic Restorations.

PURPOSE: The present study investigated the influence of simulated intraoral conditions (increased temperature and humidity) on two different surface pretreatment methods to repair a lithium-disilicate glass-ceramic (LDS). MATERIALS AND METHODS: A total of 540 rectangular lithium-disilicate glass-ceramic bars were manufactured (3 x 7 x 9 mm; IPS e.max CAD, Ivoclar Vivadent). Further specimen preparation was performed in an incubator with controlled relative humidity (RH) and temperature to simulate three different environmental settings: laboratory conditions (LC, n = 180, 23°C, 50% RH), rubber-dam conditions (RC, n = 180, 30°C, 50% RH) or oral conditions (OC, n = 180, 32°C, 95 ± 5% RH). One-third of the bars under each condition (n = 60) were grit blasted (GBL) with alumina (35 µm at 1 bar pressure for 10 s and a working distance of 4 ± 1 cm) and primed (60 s, Monobond Plus, Ivoclar Vivadent). Another third (n = 60) were pretreated with a self-etching glass-ceramic primer (MEP, Monobond Etch & Prime, Ivoclar Vivadent). One group without surface pretreatment (n = 60, NoPT) served as a control. All pretreated surfaces were coated with Heliobond (Ivoclar Vivadent). Two bars from the same pretreatment method were luted perpendicular to each other with a resin composite to form a square adhesion area of 9 mm2 (TetricEvo Ceram, Ivoclar Vivadent), and light cured for 20 s on each side (1200 mW/cm2, Bluephase 20i, Ivoclar Vivadent). All specimens were stored for 24 h in distilled water at 37°C. Half of the specimens from each environmental setting and pretreatment method (n = 15) were thermocycled (TC, 5000 cycles, 5/55°C, 30-s dwell time), and tensile bond strength (TBS) testing was performed for all groups using an x-bar rope-assisted set-up. Data were statistically analyzed using two-way ANOVA (a = 0.05) with Bonferroni adjustment. RESULTS: Regardless of the environmental and storage conditions (24 h or TC), MEP showed a significantly higher mean TBS than GBL. A decrease in TBS was recorded in specimens under OC compared to RC and LC for both pretreatment methods independent of the storage condition. No significant difference in mean TBS was found between RC and LC within the MEP pretreatment group for the 24 h stored and thermocycled specimens. For all MEPs and GBLs, TC reduced the mean TBS in all environmental conditions. The NoPT groups showed no adhesion regardless of environmental or storage conditions. CONCLUSIONS: Increased temperature and high humidity significantly reduced TBS. However, MEP was less sensitive to environmental influences than GBL, which makes it a promising candidate for intraoral ceramic repair. These findings suggest that clinical intraoral repair of lithium-disilicate glass-ceramics should be performed using a rubber-dam, primarily when using GBL.

Toughening by revitrification of Li2SiO3 crystals in Obsidian® dental glass-ceramic.

As a predominantly lithium-metasilicate-containing glass-ceramic, Obsidian® (Glidewell Laboratories, USA) has a peculiar composition and microstructure among other dental lithium silicates, warranting an evaluation of the crystallization process to establish relationships between microstructural evolution and mechanical properties. Blocks of the pre-crystallized material were processed into slices measuring 12 × 12 × 1.5 mm3 and subjected to the mandatory crystallization firing by interruption the heating ramp at temperatures between 700 °C and 820 °C (dwell time between 0 min and 10 min). The crystallization peaks of the base and the pre-crystallized glass were obtained by differential scanning calorimetry (DSC). The coefficient of thermal expansion and the glass transition temperature were derived from differential thermal analysis (DTA). X-ray diffraction (XRD) was performed to quantify and characterize the crystal phase fraction, whose microstructural changes were visualised using FE-SEM. The ball-on-three-balls surface crack in flexure method was used to track the evolution of fracture toughness. The microstructural evolution during crystallization firing was characterized by two regimes of growth: (i) the progressive revitrification (dissolution) of the 5 µm-sized Li2SiO3 polycrystals manifested at the boundaries of nanometric single coherent scattering domains (CSDs); (ii) the non-isothermal period is marked by an Ostwald ripening process characterized by the growth of the single crystalline structures into 0.5 µm polycrystals. The decrease in the crystal fraction of Li2SiO3 crystals from 41 vol.% to 37 vol.% is accompanied by the formation of a small amount of Li3PO4 (6 vol.%), maintaining the total crystal phase fraction mostly constant. The KIc accompanied the reverse trend of crystallinity, departing from 1.63 ± 0.02 MPa√m at the pre-crystallized stage to 1.84 ± 0.06 MPa√m after 10 min at 820 °C in a linear trend. Toughening appeared counter-intuitive in view of the decreasing crystal fraction and size, to rather relate to the relaxation of the residual stresses in the interstitial glass due to the spheroidization of the initially anisotropic, elongated Li2SiO3 crystals into round, nearly equiaxed particles, as let suggest from the disappearance of the extensive microcracking.

Inner marginal strength of CAD/CAM materials is not affected by machining protocol.

PURPOSE: Here we aimed to compare two machining strategies regarding the marginal strength of CAD/CAM materials using a hoop-strength test in model sphero-cylindrical dental crowns, coupled with finite element analysis. MATERIALS AND METHODS: Five CAD/CAM materials indicated for single posterior crowns were selected, including a lithium disilicate (IPS e.max® CAD), a lithium (di)silicate (Suprinity® PC), a polymer-infiltrated ceramic scaffold (Enamic®), and two indirect resin composites (Grandio® Blocs and Lava™ Ultimate). A sphero-cylindrical model crown was built on CAD Software onto a geometrical abutment and machined using a Cerec MC XL system according to the two available protocols: rough-fast and fine-slow. Specimens were fractured using a novel hoop-strength test and analyzed using the finite element method to obtain the inner marginal strength. Data were evaluated using Weibull statistics. RESULTS: Machining strategy did not affect the marginal strength of any restorative material tested here. Ceramic materials showed a higher density of chippings in the outer margin, but this did not reduce inner marginal strength. IPS e.max® CAD showed the statistically highest marginal strength, and Enamic® and Lava™ Ultimate were the lowest. Grandio® Blocs showed higher performance than Suprinity® PC. CONCLUSIONS: The rough-fast machining strategy available in Cerec MC XL does not degrade the marginal strength of the evaluated CAD/CAD materials when compared to its fine-fast machining strategy. Depending on the material, resin composites have the potential to perform better than some glass-ceramic materials.

Fracture toughness of dental incremental composite-composite interfaces at elevated temperatures.

The aim of the present laboratory study was to mechanically characterize the interface between two dental resin-based composite (RBC) increments, and to investigate if elevated temperatures have an influence on the quality of the interface mimicking clinical filling procedure. Four RBCs (CLEARFIL MAJESTY™ Posterior, Kuraray (CMP)/Filtek™ Supreme XTE, 3M (FSX)/Grandio®SO, VOCO (GSO)/VisCalor® bulk, VOCO (VCB)) were tested with a fracture toughness test using Chevron notched beams (KI,CNB) at 23, 37 and 54 °C. KI,CNB specimens (3 × 4x25mm) with a V-shaped notch at the incremental interface were loaded until failure in a 4-point bending set-up. Failure modes were characterized using light microscopy, microstructural interface was analyzed using SEM. Statistical analysis was performed using Kolmogorov-Smirnoff test, two-way ANOVA and Tukey Post-Hoc test (p = 0.05). Mean KI,CNB ranged between 0.73 ±0.14 MPam0.5 (VCB, 23 °C) and 1.11 ± 0.11 MPam0.5 (FSX, 23 °C). The tested conventional highly filled RBCs presented fracture toughness at the incremental interface comparable to the cohesive strength of the bulk materials. VCB showed reduced interfacial fracture toughness at 23 and 37 °C, but performed well at elevated temperature of 54 °C.

Filling of small oval root canals: influence of sealer placement and filling technique.

Objectives: The aim of this study was to carry out a morphometric analysis of small oval root canals filled with GuttaFlow 2 sealer (Coltène/Whaledent) using different methods of sealer placement and different root canal filling techniques.
Method and materials: Eighty extracted mandibular incisors with small oval root canals were instrumented with the Self-Adjusting File (Redent Nova). GuttaFlow 2 was placed using a lentulo spiral, paper point, master point, or sonically activated CanalBrush (Coltène/Whaledent), followed by the placement of a master point and accessory points (M?P+) (part 1). GuttaFlow 2 was placed using a lentulo spiral without a gutta-percha point, together with a single point, with a chloroform-dipped master point, or the latter with accessory points (ChMP+) (part 2). Serial cuts were made at 1-mm intervals up to 10 mm. The percentages of gutta-percha filled area (PGFA), sealer, voids, and debris were evaluated using interactive image analysis software.
Results: For part 1 of the study (sealer placement), significant differences regarding PGFA at 2 and 5 mm from the apex were found, whereas for part 2 (filling technique), significant differences were found at all levels besides 2 and 4 mm (Kruskal-Wallis test, P = .05). ChMP+ reached 85% PGFA at 3 mm from the apex, but only 30% near the apex. The MP+ groups showed a relatively equal distribution of PGFA by 60% to 80% at different levels. GuttaFlow 2 without a gutta-percha point exhibited significantly more voids and debris than the other groups (Kruskal-Wallis test, P = .05).
Conclusion: Within the limits of this study, MP+ could be recommended for clinical use. The presence of voids and debris for the group without a gutta-percha point needs further investigation.

Viscosity and stickiness of dental resin composites at elevated temperatures.

OBJECTIVE: To investigate the influence of pre-heating different classes of dental resin composites on viscosity and stickiness at five different temperatures. METHODS: Six flowable, five conventional packable, and one thermo-viscous bulk-fill resin composites were heated up to 54°C in a plate-plate rheometer to determine their complex viscosity. Normal force measurements were carried out for the six packable materials to determine the unplugging force and unplugging work (stickiness) over the same temperature range. Data were analyzed using Kolmogorov-Smirnoff test, one-way ANOVA and Tukey Post Hoc test with α=0.05 as level of significance. RESULTS: At 23°C packable composites showed viscosity between 6.75 and 19.14kPas, while flowable composites presented significantly lower viscosities between 1.31 and 2.20kPas. Pre-heating led to a drop of 30-82% in the viscosity of packable materials. The thermo-viscous material dropped to the level of flowables at 45 and 54°C thus behaving as a packable composite at room temperature with flowable-like viscosity at higher temperatures. No statistically significant differences for viscosity were observed among flowable composites at any temperature. The unplugging force decreased for packable composites, while their unplugging work generally increased at elevated temperature. At 23°C unplugging force was measured between 7.50 and 19.18N, while pre-heating up to 54°C led to values between 2.9 and 6.2N. Regarding unplugging work at 23°C the calculated values were between 3.0 and 8.9×10-3J and at 54°C between 8.8 and 13.0×10-3J. SIGNIFICANCE: Pre-heating significantly reduced viscosity of highly viscous resin composites, while no influence was shown for flowable composites. In general stickiness, measured as unplugging work, increased at elevated temperatures. The thermo-viscous material showed low viscosity comparable to flowable composites at 45 and 54°C, yet its stickiness did not increase significantly compared to the values at 23°C.

Low-temperature degradation increases the cyclic fatigue resistance of 3Y-TZP in bending.

OBJECTIVE: Due to past failures of orthopedic 3Y-TZP femoral implants linked to accelerated tetragonal-to-monoclinic phase transformation (t → m), the susceptibility to 'low-temperature degradation' or 'ageing' of 3Y-TZP has been advertised as detrimental to its long-term structural stability. However, no systematic mechanistic experiments on the fatigue resistance of aged 3Y-TZP under cyclic loading can support such statement. In this study, we aim to clarify this issue. METHODS: Here we evaluate the subcritical crack growth behavior of 3Y-TZP under cyclic loading after 0-50 h of accelerated ageing in an autoclave at 134 °C. The same 3Y-TZP sintered at two different temperatures (1450 °C or 1650 °C) allows for the comparison of materials containing grains with different susceptibilities to transformation. The volume fraction of surface transformed grains was measured using Raman spectroscopy, and the depth of the transformed surface layer from trenches milled with a Focus-Ion Beam. The fracture toughness before and after ageing was determined using the Chevron-notch Beam method. The quasi-static flexural strength was measured in dry conditions and the cyclic lifetime in water at 10 Hz and R-ratio = 0.3 in 4-point-bending at different applied stresses. The fatigue parameter n was derived from 3 different methods, namely SN curves, crack velocity plots and Weibull distributions. RESULTS: The progression of transformation showed linear kinetics with higher rates for the 3Y-TZP sintered at 1650 °C. Accelerated transformation induced severe crack formation within the transformed layer with parallel orientation to the surface plane, which supposedly behaved as the critical crack size population governing fracture. The stress intensity factor within the transformed layer was increased due to compressive stresses. Consequently, the fatigue parameter n increased consistently from 5 to 50 h of ageing, regardless of the derivation method, suggesting an increased resistance against crack growth during cyclic loading in bending. SIGNIFICANCE: Our results do not support the long suggested negative clinical implications of LTD regarding mechanical performance, to the contrary, LTD seems to increase the resistance against subcritical crack growth in a humid environment in bending.

New Approaches in Bonding to Glass-Ceramic: Self-Etch Glass-Ceramic Primer and Universal Adhesives.

PURPOSE: To investigate the tensile bond strength of silane-containing universal adhesives and self-etch glass-ceramic primer to lithium disilicate glass ceramics (LS2). MATERIALS AND METHODS: 960 rectangular LS2 bars (7 mm x 3 mm x 9 mm, IPS e.max CAD, Ivoclar Vivadent) were manufactured and divided into 4 groups (n = 240). Group 1 was etched with ~5% hydrofluoric acid (HF) for 20 s (VITA Ceramics Etch, Vita Zahnfabrik), group 2 was etched with ~5% HF for 20 s and silanized (ESPE Sil, 3M Oral Care), group 3 was pre-treated with a self-etching glass-ceramic primer (Monobond Etch & Prime, Ivoclar Vivadent, and group 4 received no pre-treatment. Three universal adhesives (iBOND Universal, Heraeus Kulzer; Scotchbond Universal Adhesive, 3M Oral Care; Futurabond U, Voco) were applied to the differently pre-treated surfaces, with Heliobond (Ivoclar Vivadent) serving as control. The bars from each group were paired and luted perpendicularly, forming a square bonded area of 9 mm2, using Variolink II (Ivoclar Vivadent) with a constant pressure of 10 N, followed by light curing (40 s at 800 mW/cm2, Elipar Trilight, 3M Oral Care). The resulting specimens were stored for 24 h at 37°C in distilled water. Half of the specimens of each group were submitted to tensile bond strength testing, the other half were thermocycled ([TC] 5000 cycles, 5°C/55°C, 30-s dwell time) before testing. Data were analyzed using three-way ANOVA (α = 0.05). RESULTS: Group 2 (HF etched and silanized) and group 3 (self-etching glass-ceramic primer) reached significantly higher mean bond strengths than did groups 1 (only HF etched) and 4 (no pre-treatment). CONCLUSION: Additional silanization of HF-etched LS2 statistically signficantly improved the tensile bond strength of the silane-containing universal adhesive (Scotchbond Universal). The self-etching glass-ceramic primer Monobond Etch & Prime achieved mean bond strengths that did not differ significantly from HF-etched and silanized specimens.

In vitro lifetime of zirconium dioxide-based crowns veneered using Rapid Layer Technology.

Rapid Layer Technology (RLT) uses computer-aided design/computer-aided manufacturing (CAD/CAM) to manufacture a veneer layer that is adhesively bonded to the zirconia framework, avoiding firing steps during the fabrication process and thus preventing build-up of residual stresses. This work studied, using sliding contact fatigue, the in vitro lifetime of restorations produced using RLT compared with restorations produced using conventional veneering techniques. Zirconia copings were veneered with a conventional hand-layering method (VM9) using a fast (n = 16) or a slow (n = 16) cooling protocol, or with RLT. For the latter, the veneers were CAD/CAM fabricated using a feldspathic reinforced-glass (Vitablocs Mark II; n = 16) or a polymer-infiltrated reinforced-glass network (Enamic; n = 16) and adhesively bonded to the zirconia frameworks. Crowns thus obtained were submitted to sliding contact fatigue against a steatite indenter in a chewing simulator until failure. A Kaplan-Meier survival analysis was conducted. None of the hand-layered restorations survived after a 2 × 106 -cycle interval, whereas no fractures in the RLT groups were observed. Vitablocs Mark II veneers survived for a longer testing period (3.5 × 106 cycles) than their Enamic counterparts (2.5 × 106 cycles) owing to their superior wear behavior. The RLT represents an efficient method to veneer zirconia frameworks by reducing processing steps and, more importantly, increasing the lifetime of the restorations.

Mechanical and hydrolytic degradation of an Ormocer®-based Bis-GMA-free resin composite.

OBJECTIVES: The aim of the study was to evaluate the mechanical stability of bisphenol A-glycidyl methacrylate (Bis-GMA) and Ormocer-based resin composites before and after water absorption and to examine water saturation. MATERIAL AND METHODS: Disc-shaped specimens of the Bis-GMA (Grandio SO, Voco) and the Ormocer-based (Admira Fusion, Voco) dental resin composites were produced, stored in water, and weighed after pre-determined times to measure the absorbed water. Bend bars were produced and stored for 24 h in dry conditions as well as in distilled water for 14 days or 60 days at 37 °C. The initial flexural strength (FS) under quasi-static loading and flexural fatigue strength (FFS) under cyclic loading were determined under 4-point bending. Fracture toughness (KIc) of both composites was measured using the single-edge-V-notch-beam (SEVNB) technique after the same storage conditions under 3-point bending. RESULTS: Within the first 14 days, storage conditions did not affect the initial FS of Grandio SO, while a significant drop in initial FS was observed for Admira Fusion after 2 weeks in water and most of the water was absorbed within this time. FFS for the Bis-GMA composite was not reduced before 2 months in water, whereas for the Ormocer®-based composite, there has been a significant decrease in strength after cyclic fatigue already at 2 weeks of water storage. KIc of Admira Fusion decreased significantly after both storage periods, while KIc of Grandio SO decreased only significantly after 2 weeks of water storage. CONCLUSION: All mechanical properties of the Bis-GMA composite were superior to those of the Ormocer®-based material, except water sorption. CLINICAL SIGNIFICANCE: Water storage seems to have a much more pronounced effect on the mechanical properties of Ormocer®-based dental composites in comparison to Bis-GMA-based composites.

Hygroscopic expansion of self-adhesive resin cements and the integrity of all-ceramic crowns.

OBJECTIVE: Low pH neutralization and subsequent remnant hydrophilicity can lead to hygroscopic expansion of self-adhesive resin cements (SARCs) after water storage. The aim of this in vitro study was to investigate the effects of hygroscopic expansion of SARCs, used as luting and partial core build-up material, on integrity and cement gap thickness increase of all-ceramic CAD/CAM crowns. METHODS: Human third molars (n=48) were prepared and anatomical all-ceramic CAD/CAM crowns were manufactured (VITABLOCS Mark II, VITA Zahnfabrik). Crowns internal surfaces were HF etched and silanized. The prepared teeth with their respective crowns were divided into 6 groups (n=8). In groups 1, 3 and 5 the coronal dentin was removed to simulate a partial core build-up. Groups 1 and 2 were luted with iCEM (Heraeus Kulzer), 3 and 4 with RelyX Unicem 2 Automix (3M), 5 and 6 with Variolink Esthetic DC (Ivoclar Vivadent). All specimens were dual cured and stored in distilled water at 37°C. Crown integrity was controlled at baseline and in regular intervals until 180 days. Cement gap thickness was measured using an optical 3D scanner (ATOS Triple scan, GOM) at baseline and after 180 days. Crown integrity was statistically analysed using Kaplan-Meier survival analysis and cement gap thickness increase using two-way ANOVA (α=0.05). RESULTS: After 180 days storage, crack formation was observed in all specimens of group 1 (mean survival time of 85.5 days), in one specimen of group 2 and in two specimens of group 4. Two-way ANOVA analysis revealed a statistically significant interaction between material type and build-up on cement gap size increase for iCEM. SIGNIFICANCE: Within the limits of this study, the application of SARCs with low pH neutralization as partial build-up material under CAD/CAM crowns is not recommended for clinical use.

Chairside CAD/CAM materials. Part 3: Cyclic fatigue parameters and lifetime predictions.

OBJECTIVES: Chemical and mechanical degradation play a key role on the lifetime of dental restorative materials. Therefore, prediction of their long-term performance in the oral environment should base on fatigue, rather than inert strength data, as commonly observed in the dental material's field. The objective of the present study was to provide mechanistic fatigue parameters of current dental CAD/CAM materials under cyclic biaxial flexure and assess their suitability in predicting clinical fracture behaviors. METHODS: Eight CAD/CAM materials, including polycrystalline zirconia (IPS e.max ZirCAD), reinforced glasses (Vitablocs Mark II, IPS Empress CAD), glass-ceramics (IPS e.max CAD, Suprinity PC, Celtra Duo), as well as hybrid materials (Enamic, Lava Ultimate) were evaluated. Rectangular plates (12×12×1.2mm3) with highly polished surfaces were prepared and tested in biaxial cyclic fatigue in water until fracture using the Ball-on-Three-Balls (B3B) test. Cyclic fatigue parameters n and A* were obtained from the lifetime data for each material and further used to build SPT diagrams. The latter were used to compare in-vitro with in-vivo fracture distributions for IPS e.max CAD and IPS Empress CAD. RESULTS: Susceptibility to subcritical crack growth under cyclic loading was observed for all materials, being more severe (n≤20) in lithium-based glass-ceramics and Vitablocs Mark II. Strength degradations of 40% up to 60% were predicted after only 1 year of service. Threshold stress intensity factors (Kth) representing the onset of subcritical crack growth (SCG), were estimated to lie in the range of 0.37-0.44 of KIc for the lithium-based glass-ceramics and Vitablocs Mark II and between 0.51-0.59 of KIc for the other materials. Failure distributions associated with mechanistic estimations of strength degradation in-vitro showed to be useful in interpreting failure behavior in-vivo. The parameter Kth stood out as a better predictor of clinical performance in detriment to the SCG n parameter. SIGNIFICANCE: Fatigue parameters obtained from cyclic loading experiments are more reliable predictors of the mechanical performance of contemporary dental CAD/CAM restoratives than quasi-static mechanical properties.

Mixed-mode fracture toughness of texturized LS2 glass-ceramics using the three-point bending with eccentric notch test.

Here we use the 3-point bending with eccentric notch test (3-PBEN) to investigate the fracture behavior of a pressable and a CAD/CAM lithium disilicate (LS2) glass-ceramics under combined mode-I and mode-II loading. The effect of the bulk texturization in the beams of the pressable LS2 is made visible through the fracture trajectory following the most energetically favorable path dictated by the crystallite alignment. The CAD/CAM LS2 shows an isotropic fracture mode but increasing fracture energy with mode-II contribution, similar to the pressable variant.

Chairside CAD/CAM materials. Part 1: Measurement of elastic constants and microstructural characterization.

OBJECTIVE: A deeper understanding of the mechanical behavior of dental restorative materials requires an insight into the materials elastic constants and microstructure. Here we aim to use complementary methodologies to thoroughly characterize chairside CAD/CAM materials and discuss the benefits and limitations of different analytical strategies. METHODS: Eight commercial CAM/CAM materials, ranging from polycrystalline zirconia (e.max ZirCAD, Ivoclar-Vivadent), reinforced glasses (Vitablocs Mark II, VITA; Empress CAD, Ivoclar-Vivadent) and glass-ceramics (e.max CAD, Ivoclar-Vivadent; Suprinity, VITA; Celtra Duo, Dentsply) to hybrid materials (Enamic, VITA; Lava Ultimate, 3M ESPE) have been selected. Elastic constants were evaluated using three methods: Resonant Ultrasound Spectroscopy (RUS), Resonant Beam Technique (RBT) and Ultrasonic Pulse-Echo (PE). The microstructures were characterized using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Raman Spectroscopy and X-ray Diffraction (XRD). RESULTS: Young's modulus (E), Shear modulus (G), Bulk modulus (B) and Poisson's ratio (ν) were obtained for each material. E and ν reached values ranging from 10.9 (Lava Ultimate) to 201.4 (e.max ZirCAD) and 0.173 (Empress CAD) to 0.47 (Lava Ultimate), respectively. RUS showed to be the most complex and reliable method, while the PE method the easiest to perform but most unreliable. All dynamic methods have shown limitations in measuring the elastic constants of materials showing high damping behavior (hybrid materials). SEM images, Raman spectra and XRD patterns were made available for each material, showing to be complementary tools in the characterization of their crystal phases. SIGNIFICANCE: Here different methodologies are compared for the measurement of elastic constants and microstructural characterization of CAD/CAM restorative materials. The elastic properties and crystal phases of eight materials are herein fully characterized.

Self-adhesive resin cements: pH-neutralization, hydrophilicity, and hygroscopic expansion stress.

OBJECTIVES: The objective of the study was to investigate the relationship between pH-neutralization, hydrophilicity, and free hygroscopic expansion stress of self-adhesive resin cements (SARCs) after storage in artificial saliva. MATERIALS AND METHODS: The SARCs RelyX Unicem Automix 2 (RX2, 3 M ESPE), iCEM (iCEM, Heraeus) and Maxcem Elite (MCE, Kerr) were under investigation in this study. Cylinders (height × diameter, 6 × 4mm) were prepared from each material and stored in artificial saliva (7d at 37 °C). Cylinder height was measured at baseline and after 7 days. After storage, the compression modulus was measured to calculate the free hygroscopic expansion stress. For pH-neutralization and hydrophilicity assessment, disks (height × diameter, 1 × 1.5 mm) were prepared, covered with electrolyte, and monitored over 24 h at 37 °C. Hydrophilicity was assessed using the static sessile drop technique at baseline and at different time intervals up to 24 h. Data were analyzed using one-way ANOVA and post hoc Student-Newman-Keuls test (S-N-K, α = 0.05). RESULTS: After 24 h, RX2 (pH24h 4.68) had a significantly higher (p < 0.05) pH-value than MCE (pH24h 4.2) and iCEM (pH24h 3.23). iCEM showed the significantly highest hydrophilicity (p < 0.05) after 24 h (θ24h 85.02°), while MCE resulted lower (θ24h 113.01°) in comparison with RX2 (θ24h 108.11°). The resulting hygroscopic expansion stress of iCEM (29.15 MPa) was significantly higher (p < 0.05) compared to RX2 (14.5 MPa) and MCE (21.02 MPa). CONCLUSIONS: The material with lowest pH-neutralization capacity displayed higher hydrophilicity after 24 h and higher hygroscopic expansion stress after 7 days compared to those with high pH-neutralization. CLINICAL SIGNIFICANCE: Remnant hydrophilicity due to low pH-neutralization of SARCs could lead to cement interface stress build-up and long-term failure of silicate ceramic restorations.

Chairside CAD/CAM materials. Part 2: Flexural strength testing.

OBJECTIVE: Strength is one of the preferred parameters used in dentistry for determining clinical indication of dental restoratives. However, small dimensions of CAD/CAM blocks limit reliable measurements with standardized uniaxial bending tests. The objective of this study was to introduce the ball-on-three-ball (B3B) biaxial strength test for dental for small CAD/CAM block in the context of the size effect on strength predicted by the Weibull theory. METHODS: Eight representative chairside CAD/CAM materials ranging from polycrystalline zirconia (e.max ZirCAD, Ivoclar-Vivadent), reinforced glasses (Vitablocs Mark II, VITA; Empress CAD, Ivoclar-Vivadent) and glass-ceramics (e.max CAD, Ivoclar-Vivadent; Suprinity, VITA; Celtra Duo, Dentsply) to hybrid materials (Enamic, VITA; Lava Ultimate, 3M ESPE) have been selected. Specimens were prepared with highly polished surfaces in rectangular plate (12×12×1.2mm3) or round disc (Ø=12mm, thickness=1.2mm) geometries. Specimens were tested using the B3B assembly and the biaxial strength was determined using calculations derived from finite element analyses of the respective stress fields. Size effects on strength were determined based on results from 4-point-bending specimens. RESULTS: A good agreement was found between the biaxial strength results for the different geometries (plates vs. discs) using the B3B test. Strength values ranged from 110.9MPa (Vitablocs Mark II) to 1303.21MPa (e.max ZirCAD). The strength dependency on specimen size was demonstrated through the calculated effective volume/surface. SIGNIFICANCE: The B3B test has shown to be a reliable and simple method for determining the biaxial strength restorative materials supplied as small CAD/CAM blocks. A flexible solution was made available for the B3B test in the rectangular plate geometry.

Descriptions of crack growth behaviors in glass-ZrO2 bilayers under thermal residual stresses.

OBJECTIVES: This study was intended to separate residual stresses arising from the mismatch in coefficients of thermal expansion between glass and zirconia (ZrO2) from those stresses arising solely from the cooling process. Slow crack growth experimentes were undertaken to demonstrate how cracks grow in different residual stress fields. METHODS: Aluminosilicate glass discs were sintered onto ZrO2 to form glass-ZrO2 bilayers. Glass discs were allowed to bond to the ZrO2 substrate during sintering or prevented from bonding by means of coating the ZrO2 with a thin boron nitrade coating. Residual stress gradients on "bonded" and "unbonded" bilayers were assessed using birefringence measurements. Unbonded glass discs were further tested under biaxial flexure in dynamic fatigue conditions in order to evaluate the effect of residual stress on the slow crack growth behavior. RESULTS: When fast-ccoling was induced, residual tensile stresses on the glass increased significantly on the side toward the ZrO2 substrate. By allowing the bond between glass and ZrO2, those tensile stresses observed in unbonded specimens are overwhelmed by the contraction mismatch stresses between the ZrO2 substrate and the glassy overlayer. Specimens containing residual tensile stresses on the bending surface showed a time-dependent strength increase in relation to stress-free annealed samples in the dynamic biaxial bending test, with this effect being dependent on the magnitude of the residual tensile stress. The phenomenon observed is explained here on the basis of the water toughening effect, in which water diffuses into the glass promoting local swelling. An additional residual tensile stress at the crack tip adds an applied-stress-independent (Kres) term to the total tip stress intensity factor (Ktip), increasing the stress-enhanced diffusion and the shielding of the crack tip through swelling of the crack faces. SIGNIFICANCE: Residual stresses in the glass influence the crack growth behavior of veneered-ZrO2 bilayered dental prostheses. The role of water in crack growth might be of higher complexity when residual stresses are present in the glass layer.

Spatial distribution of residual stresses in glass-ZrO2 sphero-cylindrical bilayers.

Residual stresses arising from inhomogeneous cooling after sintering have shown to play a preponderant role in the higher incidence of chippings observed for glass-zirconia dental prostheses. Still, current descriptions of their nature and distribution have failed to reconcile with clinical findings. Therefore, an axisymmetric sphero-cylindrical bilayer model was used in this study to determine the effect of the cooling rate on the final spatial distribution of residual stresses. Zirconia frameworks with two different radii (1.6 and 3.2mm) were CAD/CAM fabricated. Subsequent glass overlays with two different thickness ratios (1:1 and 2:1) were generated and heat pressed onto the zirconia substrates. The obtained structures were submitted to a last firing process and fast- (45°C/s) or slow-cooled (0.5°C/s) to room temperature. Unbonded bilayers were produced by firing glass overlays onto boron nitride coated zirconia. Thin sagittal and transversal sections were obtained from the specimens to assess residual stress distribution by means of light birefringence. The applied cooling rates did not affect distribution or magnitude of radial residual stresses (sagittal sections), whereas increased hoop stress magnitudes were measured (transversal sections) in fast-cooled specimens. A distinct stress nature was observed for the hoop stress component of unbonded overlays after fast cooling. Interaction between stress components seems to govern the final stress distribution, highlighting the importance of a multiaxial assessment of this problem in three-dimensional structures.