Glass science behind lithium silicate glass-ceramics.

OBJECTIVES: Lithium silicate-based glass ceramics have evolved as a paramount restorative material in restorative and prosthetic dentistry, exhibiting outstanding esthetic and mechanical performance. Along with subtractive machining techniques, this material class has conquered the market and satisfied the patients' needs for a long-lasting, excellent, and metal-free alternative for single tooth replacements and even smaller bridgework. Despite the popularity, not much is known about the material chemistry, microstructure and terminal behaviour. METHODS: This article combines a set of own experimental data with extensive review of data from literature and other resources. Starting at manufacturer claims on unique selling propositions, properties, and microstructural features, the aim is to validate those claims, based on glass science. Deep knowledge is mandatory for understanding the microstructure evolution during the glass ceramic process. RESULTS: Fundamental glass characteristics have been addressed, leading to formation of time-temperature-transformation (TTT) diagrams, which are the basis for kinetic description of the glass ceramic process. Nucleation and crystallization kinetics are outlined in this contribution as well as analytical methods to describe the crystalline fraction and composition qualitatively and quantitatively. In relation to microstructure, the mechanical performance of lithium silicate-based glass ceramics has been investigated with focus on fracture strength versus fracture toughness as relevant clinical predictors. CONCLUSION: Fracture toughness has been found to be a stronger link to initially outlined manufacturer claims, and to more precisely match ISO recommendations for clinical indications.

Long-term stability of aerophilic metallic surfaces underwater.

Aerophilic surfaces immersed underwater trap films of air known as plastrons. Plastrons have typically been considered impractical for underwater engineering applications due to their metastable performance. Here, we describe aerophilic titanium alloy (Ti) surfaces with extended plastron lifetimes that are conserved for months underwater. Long-term stability is achieved by the formation of highly rough hierarchically structured surfaces via electrochemical anodization combined with a low-surface-energy coating produced by a fluorinated surfactant. Aerophilic Ti surfaces drastically reduce blood adhesion and, when submerged in water, prevent adhesion of bacteria and marine organisms such as barnacles and mussels. Overall, we demonstrate a general strategy to achieve the long-term stability of plastrons on aerophilic surfaces for previously unattainable underwater applications.

Development of Y-TZP/MWCNT-SiO2 nanocomposite for dental protheses.

Y-TZP/MWCNT-SiO2 nanocomposite was synthesized by co-precipitation and hydrothermal treatment methods. After the characterization of the MWCNT-SiO2 powder, specimens were obtained from the synthesized material Y-TZP/MWCNT-SiO2 by uniaxial pressing for a second characterization and later comparison of its optical and mechanical properties with the conventional Y-TZP. The MWCNT-SiO2 was presented in bundles of carbon nanotubes coated by silica (mean length: 5.10 ± 1.34 µm /D90: 6.9 µm). The composite manufactured was opaque (contrast ratio: 0.9929 ± 0.0012) and had a white color with a slightly difference from the conventional Y-TZP (ΔE00: 4.4 ± 2.2) color. The mechanical properties of Y-TZP/MWCNT-SiO2: vickers hardness (10.14 ± 1.27 GPa; p = 0.25) and fracture toughness (4.98 ± 0.30 MPa m1/2; p = 0.39), showed no significant difference from the conventional Y-TZP (hardness: 8.87 ± 0.89; fracture toughness: 4.98 ± 0.30 MPa m1/2). However, for flexural strength (p = 0.003), a lower value was obtained for Y-TZP/MWCNT-SiO2 (299.4 ± 30.5 MPa) when compared to the control Y-TZP (623.7 ± 108.8 MPa). The manufactured Y-TZP/MWCNT-SiO2 composite presented satisfactory optical properties, however the co-precipitation and hydrothermal treatment methods need to be optimized to avoid the formation of porosities and strong agglomerates, both from Y-TZP particles and MWCNT-SiO2 bundles, which lead to a significant decrease in the material flexural strength.

Edge chipping damage in lithium silicate glass-ceramics induced by conventional and ultrasonic vibration-assisted diamond machining.

OBJECTIVES: Diamond machining of lithium silicate glass-ceramics (LS) induces extensive edge chipping damage, detrimentally affecting LS restoration functionality and long-term performance. This study approached novel ultrasonic vibration-assisted machining of pre-crystallized and crystallized LS materials to investigate induced edge chipping damage in comparison with conventional machining. METHODS: The vibration-assisted diamond machining was conducted using a five-axis ultrasonic high-speed grinding/machining machine at different vibration amplitudes while conventional machining was performed using the same machine without vibration assistance. LS microstructural characterization and phase development were performed using scanning electron microscopy (SEM) and x-ray diffraction (XRD) techniques. Machining-induced edge chipping depths, areas and morphology were also characterized using the SEM and Java-based imaging software. RESULTS: All machining-induced edge chipping damages resulted from brittle fractures. The damage scales, however, depended on the material microstructures; mechanical properties associated with the fracture toughness, critical strain energy release rates, brittleness indices, and machinability indices; and ultrasonic vibration amplitudes. Pre-crystallized LS with more glass matrix and lithium metasilicate crystals yielded respective 1.8 and 1.6 times greater damage depths and specific damage areas than crystallized LS with less glass matrix and tri-crystal phases in conventional machining. Ultrasonic machining at optimized amplitudes diminished such damages by over 50 % in pre-crystallized LS and up to 13 % in crystallized LS. SIGNIFICANCE: This research highlights that ultrasonic vibration assistance at optimized conditions may advance current dental CAD/CAM machining techniques by significant suppression of edge chipping damage in pre-crystallized LS.

Speed-sintering and the mechanical properties of 3-5 mol% Y2O3-stabilized zirconias.

Ever faster workflows for the fabrication of all-ceramic restorations are of high economic interest. For that purpose, sintering protocols have been optimized for use in modern sintering furnaces, the so-called speed-sintering. However, conventional furnaces are still the most widely used equipment to sinter zirconia restorations. In this in-vitro study, we evaluated the feasibility of a speed-sintering protocol using a conventional sintering furnace to sinter different dental zirconias (stabilized with 3 mol% up to 5.4 mol% Y2O3) in comparison to a conventional sintering program. The properties evaluated were Young's modulus, Poisson's ratio, density, biaxial flexural strength, and fracture toughness. We show here that despite differences being dependent on material, the physical and mechanical properties of speed-sintered zirconia are comparable to those obtained by the conventional sintering.

A step toward bio-inspired dental composites.

This feasibility study aimed to develop a new composite material of aligned glass flakes in a polymer resin matrix inspired by the biological composite nacre. The experimental composite was processed by an adapted method of pressing a glass flake and resin monomer system. By pressing and allowing the excess monomer to flow out, the long axis of the flakes was aligned. The resultant anisotropic composite with silanized and non-silanized glass flakes were subjected to fracture toughness tests. We observed increasing fracture toughness with increasing crack extension (Δa) known as resistance curve (R-curve) behavior. Silanized specimens had higher stress intensity KR-Δa over non-silanized specimens, whereas non-silanized specimens had a much lower Young's modulus, and higher nonlinear plastic-elastic JR-Δa R-curve. In comparison with conventional composites, flake-reinforced composites can sustain continued crack growth for more significant extensions. The primary toughening mechanism seen in flake-reinforced composites was crack deviation and crack branching. We produced an anisotropic model of glass flake-reinforced composite showing elevated toughening potential and a prominent R-curve effect. The feasibility of flake reinforcement of dental composites has been shown using a relatively efficient method. The use of a biomimetic, nacre-inspired reinforcement concept might guide further research toward improvement of dental restorative materials.

Determination of Water Content in Direct Resin Composites Using Coulometric Karl Fischer Titration.

This study evaluated the water content and sorption of direct composites over 60 days using coulometric Karl Fischer titration (KFT). Plate-shaped specimens (10 × 10 × 1 mm3 of thickness) were built up using the composites Clearfil Majesty Posterior (CM), Grandio SO (GS), and Filtek Supreme XT (FS). Water contents were determined in non-stored specimens (control) or after storage in distilled water for up to 60 days (n = 5). The amount of water transferred from the specimens heated at 200 °C (isothermal mode) was measured in the Coulometer. The water content of non-stored specimens ranged from 0.28 to 1.69 wt% (5.6 to 31.2 µg/mm3) for GS and FS, respectively. The highest values of water sorption were observed for FS (25.3 µg/mm3 after 60 days). GS and CM showed similar water sorption after 60 days (≈9 µg/mm3), but an ultimate higher water content was observed for CM (0.9 wt%; 22.0 µg/mm3) than GS (0.7 wt%; 14.8 µg/mm3). Except for CM, no significant water sorption was observed between 21 and 60 days of storage. Since all composites presented some base water content, water sorption data alone do not account for the ultimate water content in direct resin-based composites.

On the assignment of quartz-like LiAlSi2O6 - SiO2 solid solutions in dental lithium silicate glass-ceramics: Virgilite, high quartz, low quartz or stuffed quartz derivatives?

OBJECTIVES: Here we aim to provide a background on X-Ray Diffraction analysis of quartz-like crystal structures with varying amounts of Al3+ and Li+ substitution, existing confusions on their nomenclature and its implications for novel lithium silicate glass-ceramics. METHODS: We reviewed the literature dealing with modifications of the quartz crystal structure and their stuffed LiAlSi2O6 derivates, LiAlSi2O6 - SiO2 solid solutions, the terminology of such phases and criteria used to define the structure known as virgilite. Based on this information, we attempted to allocate the quartz-like phases found in CEREC TesseraTM, InitialTM LiSi Block and Amber® Mill in the range of LiAlO2 - SiO2 solid solutions. For this purpose, their lattice parameters obtained from Rietveld refinement were compared with the lattice parameters of members of the corresponding solid solutions with defined SiO2 molar fraction found in the literature. RESULTS: Based on the lattice parameters available for low quartz, high quartz and its stuffed derivatives, including LiAlSi2O6 and the mineral virgilite, a plot of the a- and c-parameters vs. the mol% SiO2 related to LiAlO2 was constructed with the literature data and the data found for the three dental lithium silicates. As per the definitions of virgilite as either LixAlxSi3-xO6, with 0.5 < x < 1 or especially as members of the LiAlSi2O6 - SiO2 solid-solution series with more than 50 mol% LiAlSi2O6, the crystal structures in CEREC TesseraTM, InitialTM LiSi Block and Amber® Mill failed to fall within the ranges of mol% SiO2 confined for virgilite. SIGNIFICANCE: Based on available literature and definitions, the quartz-like phases found in the three dental lithium silicates should be addressed as stuffed (probably low) quartz solid solutions instead of "virgilite". However determined by mineralogical practices, the term "virgilite" for parts of the LiAlSi2O6 - SiO2 solid solution is ambiguous and can be considered as arbitrary.

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.

Fracture toughness of 3Y-TZP ceramic measured by the Chevron-Notch Beam method: A round-robin study.

OBJECTIVE: This interlaboratory round robin test investigated the robustness of the Chevron-Notch Beam (CNB) test method and the effect of the processing and testing variations on the fracture toughness of a dental 3Y-TZP ceramic. METHODS: The round robin test was performed precisely following the procedures recommended in ISO 24370:2005 and applied on a commercial 3Y-TZP ceramic (product information). A total of 335 test specimens with dimensions 3×4 x 45 mm³ was equally distributed among 10 participating laboratories of varying experience in fracture toughness testing. A standard operating procedure was defined with either narrow processing tolerances or alternative (wider) processing tolerances (as proposed in ISO 24370). Fracture toughness data (series 2) was analyzed using one way ANOVA followed by post hoc Tukey HSD test and 95% Confidence Intervals (CI) were computed (p < 0.05). A further, preceding round-robin (series 1) test was conducted with - more possible variations of test conditions regarding CNB notch processing and storage conditions. Those results are summarized in the supplement and discussed with the actual ISO 24370 test. RESULTS: Fracture toughness of the 3Y-TZP ceramic material, summarized over all laboratories was measured to KIc = 4.48 ± 0.11 MPam0.5 for the standard processing tolerance and KIc = 4.55 ± 0.31 MPam0.5 for the alternative tolerance. The results revealed a significant influence of cutting offset and notch geometry on KIc when using CNB method. The test medium also has a significant influence on KIc in terms of reduced fracture toughness under the influence of water. With defined testing conditions the number of valid tests and reduced standard deviation increased. In case of strictly following such standard operation procedures, KIc can be determined with high reliability. There is no difference between the involved laboratories, but significant influence of cutting offset on KIC was observed. SIGNIFICANCE: The CNB method is suitable method for determination of KIc on fine-grained ceramics such as 3Y-TZP ceramic. By using tighter tolerances for processing and testing, i.e. closely following the ISO 24370 procedure, a highly-precise evaluation of fracture toughness with low data variation is achievable. The information of the storage medium should always be reported along with the data. CNB fracture toughness testing is an alternative method compared to Single-edge V-notch beam (SEVNB), especially for fine-grained ceramics.

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.

A split-Chevron-Notched-Beam sandwich specimen for fracture toughness testing of bonded interfaces.

The realization that the use of strength tests as a means to probe the bonding performance of adhesive systems to dental restorative materials suffers from inherent drawbacks has shifted efforts towards devising viable and valid fracture toughness test for that purpose. Here we introduce a new procedure to produce split-Chevron-Notched-Beam specimens that need not undergo sawing or notching after bonding, thus sparing the interface from pre-stresses. We evaluate the formal geometric factor considering the influence of the use of different materials having different elastic properties, and show that the results obtained fall within reasonable ranges measured by other established compliance calibrated methods. We demonstrate the application of this new approach for dentin-luting composite and zirconia-luting composite interfaces for different adhesive systems and pre-treatment procedures in order to probe the sensitivity of the method to different bond qualities.

Coulometric titration of water content and uptake in CAD/CAM chairside composites.

OBJECTIVES: This study aimed to evaluate the water content and uptake of CAD/CAM chairside composites over 60 days using coulometric Karl Fischer (KF) titration. METHODS: Rectangular plates (10 ×10×1 mm3 of thickness) were cut from the blocks of composites Cerasmart 270 (CS), Katana Avencia (KA), Grandio Blocs (GB), and Lava Ultimate (LU). Specimens were stored in distilled water for up to 60 days at 37 °C, and non-stored specimens were used as a control (n = 5). Specimens were isothermally heated at 200 °C, and the water content was evaporated and transferred to the titration cell throughout a nitrogen gas flow. The KF coulometer determined the percentage of water in each specimen. Data were analyzed by 2-way ANOVA and Tukey`s test (α = 0.05). RESULTS: The water content of non-stored specimens ranged from 0.29 to 1.66 wt% (6.9-32.9 µg/mm3) for GB and LU, respectively. The water content increased underwater storage (0.82-2.96 wt% after 60 days). The extend of water sorption (11.9-26.1 µg/mm3) among the materials was directly related to their base water content. No additional water content increase was observed after 7 (LU and KA) or 21 (GB and CS) days. Measuring the water content in wt% or µg/mm3 affected the ranking of materials when KA and CS were analyzed. SIGNIFICANCE: Composites with higher base water content also presented higher water sorption. KF titrationshowed to be a reliable method to measure the water sorption of composites, including their base water content.

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.

Grasping the Lithium hype: Insights into modern dental Lithium Silicate glass-ceramics.

OBJECTIVES: Lithium-based glass-ceramics are currently dominating the landscape of dental restorative ceramic materials, with new products taking the market by storm in the last years. Though, the difference among all these new and old products is not readily accessible for the practitioner, who faces the dilemma of reaching a blind choice or trusting manufacturers' marketing brochures. To add confusion, new compositions tend to wear material terminologies inherited from vanguard dental lithium disilicates, disregarding accuracy. Here we aim to characterize such materials for their microstructure, crystalline fraction, glass chemistry and mechanical properties. METHODS: Eleven commercial dental lithium-based glass ceramics were evaluated: IPS e.max® CAD, IPS e.max® Press, Celtra® Duo, Suprinity® PC, Initial™ LiSi Press, Initial™ LiSi Block, Amber® Mill, Amber® Press, N!CE®, Obsidian® and CEREC Tessera™. The chemical composition of their base glasses was measured by X-Ray Fluorescence Spectroscopy (XRF) and Inductive Coupled Plasma Optical Emission Spectroscopy (ICP-OES), as well as the composition of their residual glass by subtracting the oxides bound in the crystallized fraction, characterized by X-Ray Diffraction (XRD) and Rietveld refinement, and quantified accurately using the G-factor method (QXRD). The crystallization behavior is revealed by differential scanning calorimetry (DSC) curves. Elastic constants are provided from Resonant Ultrasound Spectroscopy (RUS) and the fracture toughness measured by the Ball-on-Three-Balls method (B3B- K Ic). The microstructure is revealed by field-emission scanning electron microscopy (FE-SEM). RESULTS: The base glasses showed a wide range of SiO2 /Li2O ratios, from 1.5 to 3.0, with the degree of depolymerization dropping from ½ to 2/3 of the initial connectivity. Materials contained Li2SiO3+Li3PO4, Li2SiO3+Li3PO4+Li2Si2O5, Li2Si2O5+Li3PO4+ Cristobalite and/or Quartz and Li2Si2O5+Li3 PO4+LiAlSi2O6, in crystallinity degrees from 45 to 80 vol%. Crystalline phases could be traced to their crystallization peaks on the DSC curves. Pressable materials and IPS e.max® CAD were the only material showing micrometric phases, with N!CE® and Initial™ LiSi Block showing solely nanometric crystals, with the rest presenting a mixture of submicrometric and nanometric particles. Fracture toughness from 1.45 to 2.30 MPa√m were measured, with the linear correlation to crystalline fraction breaking down for submicrometric and nanometric crystal phases. SIGNIFICANCE: Dental lithium-based silicate glass-ceramics cannot be all put in the same bag, as differences exist in chemical composition, microstructure, crystallinity and mechanical properties. Pressable materials still perform better mechanically than CAM/CAM blocks, which loose resistance to fracture when crystal phases enter the submicrometric and nanometric range.

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.

Mechanical degradation of contemporary CAD/CAM resin composite materials after water ageing.

OBJECTIVE: The aim of the present study was to assess the effect of water storage on the quasi-static properties and cyclic fatigue behavior of four contemporary CAD/CAM resin composite materials. METHODS: The CAD/CAM resin composites Grandio Blocs, LavaTM Ultimate, CerasmartTM and Brilliant Crios, as well as the direct resin composite Grandio SO, were evaluated. Rectangular plates were cut from the blocks or fabricated using a silicon mold to obtain specimens for fracture toughness (KIc, n = 10), biaxial strength (σ0, n = 30) and cyclic fatigue testing (n = 30). Half of the specimens was stored for 24 h in dry conditions and the other half was aged for 60 days in distilled water at 37 °C. KIc was determined using the Compact-Tension (C(T)) method and σ0 and cyclic fatigue were tested using the Ball-on-Three-Balls assembly. Additional disc-shaped specimens (n = 5) were produced to obtain water sorption curves of the materials. Weibull statistics and two-way ANOVA with Tukey's post-hoc test were used for data assessment. RESULTS: The highest water sorption was observed for LavaTM Ultimate (42.6 µg/mm3), whereas Grandio SO displayed the lowest uptake (14 µg/mm3). A statistically significant drop in KIc and σ0 was measured for all materials after water storage, except for the σ0 of CerasmartTM. Water ageing had a dissimilar effect on the cyclic fatigue behavior, increasing the slow crack growth susceptibility of LavaTM Ultimate, but decreasing it for CerasmartTM and Brilliant Crios. SIGNIFICANCE: Contemporary CAD/CAM resin composites are susceptible to water driven degradative processes, although differences in filler content and resin matrix constitution play an important role in how it impacts their mechanical properties.

Fractography of clinical failures of indirect resin composite endocrown and overlay restorations.

OBJECTIVES: Compare failure modes and fracture origins using fractography on recovered clinically fractured parts of indirect resin composite endocrowns and overlay restorations on endodontically treated teeth (ETT). METHODS: Four endocrowns (3 molars, 1 premolar) and one overlay (molar) adhesively luted on ETT were recovered after fracturing during function. The time in service ranged between 4 and 48 months. The composite materials were (i) CAD/CAM LAVA Ultimate (N = 1), (ii) Premise Indirect (N = 2), and (iii) Colombus (N = 2). Fractography was performed by means of digital microscopy and SEM. Occlusal surfaces were checked for signs of fatigue degradation and contact wear. Cuspal plane angles were measured from profiles obtained from 3D digital microscope images with respect to the horizontal plane of the occlusal central crown groove. RESULTS: All five cases showed a wedge-opening mode I fracture, splitting the crown and tooth in two parts through the crown's central groove. Classic brittle fracture features (arrest lines, twist and wake hackle) were easily identified on the fracture surfaces. Multiple origins were located along the central groove in conjunction with the presence of fatigue cracks. Contact wear surfaces showed pitting and cracking. Cuspal plane angles were around 30-35°, except a 50° palatal cusp slope for the Lava Ultimate overlay. SIGNIFICANCE: Fractography on clinical fractures of resin composites was enlightening. Occlusal surface fatigue degradation from cyclic loading, mode I fracture from applied mastication forces on cuspal planes, and stress concentration within the crown's central groove, indicate limitations of use of these materials for endocrowns in posterior teeth.