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.

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.

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.

Antagonist wear of monolithic zirconia crowns after 2 years.

OBJECTIVES: The aim of this study was to evaluate the amount of wear on the antagonist occlusal surfaces of clinically placed monolithic zirconia premolar and molar crowns (LAVA Plus, 3M ESPE). MATERIALS AND METHODS: Fourteen in situ monolithic zirconia crowns and their opposing antagonists (n = 26) are the subject of an ongoing clinical trial and have been clinically examined at baseline and after 24 months. Silicone impressions were taken and epoxy replicas produced for qualitative SEM analysis and quantitative analysis using optical profilometry. Based on the baseline replicas, the follow-up situation has been scanned and digitally matched with the initial topography in order to calculate the mean volume loss (in mm3) as well as the mean maximum vertical loss (in mm) after 2 years in service. RESULTS: The mean volume loss for enamel antagonist contacts (n = 7) was measured to 0.361 mm3 and the mean of the maximum vertical loss to 0.204 mm. The mean volume loss for pure ceramic contacts (n = 10) was measured to 0.333 mm3 and the mean of the maximum vertical loss to 0.145 mm. The wear rates on enamel contacts were not significantly different from those measured on ceramic antagonists. CONCLUSIONS: Based on the limitations of this study, it can be concluded for the monolithic zirconia material LAVA Plus that the measured wear rates are in consensus with other in vivo studies on ceramic restorations. Further, that no significant difference was found between natural enamel antagonists and ceramic restorations as antagonists. The monolithic zirconia restorations do not seem to be affected by wear within the first 2 years. CLINICAL RELEVANCE: The monolithic zirconia crowns (LAVA Plus) show acceptable antagonist wear rates after 2 years in situ, regardless of natural enamel or ceramics as antagonist materials.

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.

Antagonist wear by polished zirconia crowns.

AIM: The aim of this in vivo study was to measure antagonist wear caused by polished monolithic posterior zirconia crowns over a 24-month period using the intraoral digital impression (IDI) technique. MATERIALS AND METHODS: Thirteen zirconia crowns were placed in nine patients. The crowns and adjacent teeth were captured using an intraoral scanner (Lava C.O.S.). The corresponding antagonist teeth and the respective neighboring teeth were also scanned. Scanning was performed immediately after the restoration (baseline) as well as 12 and 24 months after crown placement. Geomagic Qualify software was used to superimpose the follow-up data sets onto the corresponding baseline data set, identify wear sites, and measure maximum vertical height loss in each individual wear site. Overall antagonist wear was then determined as the mean of wear rates measured in all of the individual antagonist units. In addition, wear rates in enamel and ceramic antagonists were analyzed as part of the scope of this study. RESULTS: The maximum mean wear with standard deviation (SD) in the overall sample with a total of nine patients, 13 antagonist units, and 98 evaluable wear sites was 86 ± 23 µm at 12 months, and 103 ± 39 µm at 24 months. The maximum mean wear in the enamel antagonist subgroup was 87 ± 41 µm at 12 months, and 115 ± 71 µm at 24 months; and in the ceramic antagonist subgroup 107 ± 22 µm at 12 months, and 120 ± 27 µm at 24 months. CONCLUSIONS: The wear rates determined in this study are comparable to those of existing studies. The IDI technique of wear analysis can be carried out in a practical manner and produces useful results.

Optical profilometry versus intraoral (handheld) scanning.

AIM: The aim of this study was to evaluate the difference in maximum height loss values obtained from datasets based on optical profilometry and intraoral scanning. Additionally, two analysis applications were tested with respect to their correspondence. MATERIALS AND METHODS: To obtain baseline data, the occlusal surface of a metal phantom tooth was scanned by optical profilometry [WLP] and an intraoral scanner [IOS]. Then, wear was simulated at two locations of the tooth, three times each ([wear1], [wear2], and [wear3]), and the surface was captured after each status of wear, applying [WLP] and [IOS]. The maximum vertical height loss was evaluated by comparing the 3D datasets of [WLP] and [IOS] at [wear1], [wear2], and [wear3] with the baseline data of [WLP] and [IOS], respectively. For this purpose, two commercially available applications, Geomagic Qualify and Oracheck, were used. RESULTS: Apart from one outlier of 16% difference between the data obtained from [WLP] and [IOS], the maximum difference was 12.6%, which was equal to a metrical value of 15 µm. For the corresponding values, which were calculated with Geomagic Qualify and Oracheck at identical wear facets, maximum differences between +7% and -6.7% were obtained. CONCLUSIONS: According to this in vitro study, the wear measurement on the basis of [IOS] seems to be a cost-effective, quick, and easily applicable tool for clinical screening purposes, with an acceptable reliability. With respect to the minor variations between each other, the Geomagic Qualify and Oracheck measurement applications are equivalent.

Are resin composites suitable replacements for amalgam? A study of two-body wear.

OBJECTIVES: Wear resistance is an important property of the dental materials, particularly for large restorations in the posterior regions and for the patients suffering from parafunctional activities. Additionally, the wear resistance of flowable composite resin materials is a clinical concern, although they are popular among dentists because of their easy handling. The aims of the present study were to evaluate the wear resistance of nine composite resins both condensable (G-aenial posterior, Venus, GrandioSO, Tetric EvoCeram, Ceram X duo, Filtek Supreme XTE) and new-generation flowable resin composites (G-aenial Universal Flo, GrandioSO Flow and GrandioSO Heavy Flow) and to compare these results with amalgam. MATERIALS AND METHOD: Eight specimens of each material were subjected to two-body wear tests, using a chewing simulator. The wear region of each material was examined under profilometer, measuring the vertical loss (µm) and the volume loss (mm(3)) of the materials. Additionally, SEM analysis was performed to assess surfaces irregularities. RESULTS: The results showed significant difference of the vertical loss and the volume loss of the examined materials (p < 0.001). Although amalgam had the best wear resistance, two condensable resin composites (GrandioSO, Ceram X duo) and all flowable materials had no significant difference with amalgam. GrandioSO had the highest wear resistance and Filtek Supreme XTE the lowest wear resistance. CONCLUSION: The majority of resin composites had good wear resistance and similar to amalgam. CLINICAL RELEVANCE: Based on the in vitro measurements of two-body wear resistance, the new resin composites could replace amalgam for restorations placed in occlusal stress-bearing regions. New-generation flowable resin materials may also be used in occlusal contact restorations.

Self-adhesive resin cements: adhesive performance to indirect restorative ceramics.

PURPOSE: To evaluate the bonding performance of self-adhesive resin cements to zirconia and lithium disilicate in self- and dual-curing modes before and after thermocycling. MATERIALS AND METHODS: Rectangular bars (3 mm high, 3 mm wide, 9 mm long) were manufactured from zirconia (Vita In-Ceram YZ for inLab, VITA) and lithium disilicate blocks (IPS e.max Press, Ivoclar Vivadent) (n=240 per material). Zirconia bars were sandblasted (35 µm Al2O3, 1.5 bar pressure). Lithium disilicate bars were HF etched (20 s, IPS Ceramic Etching Gel, Ivoclar Vivadent) and silanized with ESPE Sil (3M ESPE). Forty bars of zirconia were luted in twos perpendicular to each other as were 40 bars of lithium disilicate using RelyX Unicem Automix 2 (3M ESPE), G-Cem LinkAce (GC Europe) or Maxcem Elite (Kerr) in self- or dual-curing mode. Half of the specimens from each material were submitted to tensile bond strength (TBS) testing after 24-h storage in distilled water at 37°C, and half underwent TBS testing after thermocycling (5000 cycles, 5°C/55°C, 30-s dwell time). Bond strength values for each bonding substrate were analyzed using one-way ANOVA (Student-Newman- Keuls, α=0.05). RESULTS: On zirconia, dual-curing resulted in significantly (p<0.05) higher tensile bond strengths compared to self-curing, with the exception of RelyX Unicem 2 after thermocycling. Thermocycling significantly (p<0.05) reduced the tensile bond strength of Maxcem Elite to zirconia in both curing modes. The TBS of self-adhesive cements to lithium disilicate showed no significant (p>0.05) difference between the different curing modes and after thermocycling. CONCLUSION: For most of the investigated self-adhesive cements, bond strengths to zirconia were increased by dual curing; this was not true for lithium disilicate. For luting on zirconia with self-adhesive cements, dual curing is strongly recommended in clinical situations.

Fatigue strength of bilayer yttria-stabilized zirconia after low-temperature degradation.

This study examined the impact of interfacial interactions on bilayer yttria-stabilized zirconia (YSZ) used in dental restorations. In-house bilayer structures of 3YSZ and 5YSZ composition underwent hydrothermal degradation to compare the properties of control and low-temperature degradation (LTD) treated groups. Biaxial flexural strength via piston-on-three-balls, staircase fatigue strength over 106 cycles at 15 Hz, phase characterization and quantification through XRD and Rietveld refinement, and fractography were conducted. Weibull analysis was employed to determine the Weibull modulus and characteristic strength. Results demonstrated an enhancement in the mechanical performance of 3YSZ composition after LTD treatment, whereas the mechanical properties of 5YSZ remained largely unaffected post-degradation. Fractographic analysis revealed that failure originated at the surface tensile location across all specimen groups. These findings offer insights into the mechanical behavior of bilayer zirconia structures and reinforce the significance of hydrothermal treatment in enhancing their performance, particularly in the case of 3Y compositions.

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.

Biomimetically- and hydrothermally-grown HAp nanoparticles as reinforcing fillers for dental adhesives.

PURPOSE: Differently prepared hydroxyapatite (HAp) nanoparticles were incorporated into the adhesive solution of a commercial adhesive system in order to evaluate the effect on microtensile bond strength to dentin. MATERIALS AND METHODS: HAp nanoparticles (20 to 70 nm) were prepared by different processes (biomimetic and hydrothermal) and incorporated into the adhesive of the Adper Scotchbond Multi-Purpose (SBMP) system at various concentrations. Control (unfilled) and experimental groups (filled) were applied onto flat mid-coronal human dentin. Composite crowns were built up and cut into beams with a cross-sectional area of 0.65 ± 0.05 mm2. Specimens were fractured in tension and examined with a scanning electron microscope (SEM) for fractographic analysis. Microtensile bond strength (µTBS) data were analyzed using a two-way ANOVA and modified LSD test at a = 0.05. Analysis of the nanofiller distribution and ultramorphological characterization of the interface was performed by transmission electron microscopy (TEM). RESULTS: HAp nanoparticle incorporation into the adhesive of SBMP significantly influenced µTBS to dentin depending on the fillers and the concentration used. A significant increase of the mechanical strength was obtained for the adhesives containing 1% (wt/vol) biomimetic and 5% hydrothermal silanized HAp particles, while the other particle fractions did not influence µTBS significantly. 10% (wt/vol) HAp particles significantly lowered the µTBS irrespective of the particle type used. TEM micrographs revealed nanoparticle dispersion through the adhesive layer but no deposition on or penetration into the hybrid layer. CONCLUSIONS: HAp nanoparticle incorporation into SBMP increased bond strength to dentin by cohesively reinforcing the interface adhesive layer. At a concentration of 10% (wt/vol), nanofiller incorporation had a negative effect on bond strength.

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.

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.

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.

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.

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.

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.

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.