Michael Wendler

Bonding performance of universal adhesives in different etching modes

OBJECTIVES The aim of this study was to compare the microtensile bond strength (μTBS) and resin penetration into dentine of three universal adhesives (UAs) applied in two different etching modes (i.e. self-etch or etch-and-rinse). The effect of thermocycling on the μTBS was also evaluated. METHODS The occlusal third of sound human molars was removed and the exposed surfaces were treated with three UAs (Futurabond Universal, Scotchbond Universal Adhesive and All-Bond Universal) in self-etch or etch-and-rinse mode. Two one-step self-etch adhesives (Futurabond DC and Futurabond M) were applied on additional teeth as reference. After composite build up, the specimens were stored for 24 h in distilled water at 37 °C or thermocycled for 5000 cycles. Composite/dentine beams were prepared (1 mm(2)) and μTBS test was performed. Data was analyzed using three-way ANOVA and Tukeys test (α=0.05). One additional tooth was prepared for each group for evaluation of infiltration ability into dentine by dyeing the adhesives with a fluorochrome (Rhodamine B). After longitudinal sectioning, the generated interfaces were examined under confocal laser scanning microscopy. RESULTS The addition of an etching step did not significantly affect the μTBS of none of the UAs, when compared to their self-etch application mode. All pre-etched specimens showed considerably longer resin tags and thicker hybrid layers. Thermocycling had no significant effect on the μTBS of the UAs. CONCLUSIONS Application of an etching step prior to UAs improves their dentine penetration, but does not affect their bond strength to dentine after 24h or after thermocycling for 5000 cycles. CLINICAL SIGNIFICANCE Similar bond strength values were observed for the UAs regardless of application mode, which makes them reliable for working under different clinical conditions.

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 Youngs modulus (E), Shear modulus (G), Bulk modulus (B) and Poissons 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.

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.

Characterization of residual stresses in zirconia veneered bilayers assessed via sharp and blunt indentation

OBJECTIVES The present study evaluated the effect of the coefficient of thermal expansion (CTE) mismatch and the cooling protocol on the distribution of residual stresses and crack propagation in veneered zirconia bilayers. METHODS Ceramic discs with two different CTEs (Vita VM9 and Lava Ceram) were fired onto zirconia plates and cooled following a slow (0.5°C/s) or a fast (45°C/s) cooling protocol. The residual stress distribution throughout the veneer thickness was assessed by means of depth-wise Vickers indentation after sequentially sectioning the bilayers parallel compared to normal to the interface. A mathematical solution for the residual stress distribution was used as reference. Additionally, Hertzian cone crack propagation in the veneers was induced by cyclic contact loading and measured at different number of cycles to estimate the crack growth rate. RESULTS The higher CTE mismatch of the VM9 group generated an important stress gradient with high compressive residual stresses near the interface, hindering the crack propagation. The low CTE mismatch group (Lava Ceram) developed only a slight stress gradient and higher cone crack growth rates. No differences were observed between the two cooling protocols applied regarding stress magnitude and crack propagation behavior. SIGNIFICANCE The CTE mismatch has a predominant role in the generation of residual stress gradients within the veneer, which directly influences contact-induced crack propagation. Based on the results, the cooling protocol had no significant effect on the residual stress distribution in zirconia-veneer bilayers.

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 materials 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.

Practical and theoretical considerations on the fracture toughness testing of dental restorative materials

BACKGROUND An important tool in materials research, development and characterization regarding mechanical performance is the testing of fracture toughness. A high level of accuracy in executing this sort of test is necessary, with strict requirements given in extensive testing standard documents. Proficiency in quality specimen fabrication and test requires practice and a solid theoretical background, oftentimes overlooked in the dental community. AIMS In this review we go through some fundamentals of the fracture mechanics concepts that are relevant to the understanding of fracture toughness testing, and draw attention to critical aspects of practical nature that must be fulfilled for validity and accuracy in results. We describe our experience with some testing methodologies for CAD/CAM materials and discuss advantages and shortcomings of different tests in terms of errors in testing the applicability of the concept of fracture toughness as a single-value material-specific property.

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.

Repair Bond Strength of Aged Resin Composite after Different Surface and Bonding Treatments

The aim of this study was to compare the effect of different mechanical surface treatments and chemical bonding protocols on the tensile bond strength (TBS) of aged composite. Bar specimens were produced using a nanohybrid resin composite and aged in distilled water for 30 days. Different surface treatments (diamond bur, phosphoric acid, silane, and sandblasting with Al2O3 or CoJet Sand), as well as bonding protocols (Primer/Adhesive) were used prior to application of the repair composite. TBS of the specimens was measured and the results were analyzed using analysis of variance (ANOVA) and the Student–Newman–Keuls test (α = 0.05). Mechanically treated surfaces were characterized under SEM and by profilometry. The effect of water aging on the degree of conversion was measured by means of FTIR-ATR spectroscopy. An important increase in the degree of conversion was observed after aging. No significant differences in TBS were observed among the mechanical surface treatments, despite variations in surface roughness profiles. Phosphoric acid etching significantly improved repair bond strength values. The cohesive TBS of the material was only reached using resin bonding agents. Application of an intermediate bonding system plays a key role in achieving reliable repair bond strengths, whereas the kind of mechanical surface treatment appears to play a secondary role.

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.