Ultrasonic monitoring of the setting of glass-ionomer luting cements

This study used ultrasonic measurements to monitor the setting behaviour, and changes in the elastic modulus, of glass–ionomer cements. The ultrasonic equipment comprised a pulser–receiver, transducers, and an oscilloscope. The two-way transit time through the mixing cement disk was divided by two, in order to account for the down-and-back travel path, and then multiplied by the sonic velocity within the material. The sonic velocities of the longitudinal and shear waves were used to determine the elastic modulus. In the earliest stages of the setting process, most of the ultrasound energy was absorbed by the cements and the second echoes were relatively weak. As the cements hardened, the sound velocities increased until they reached a plateau. The changes in sound velocities differed among the glass–ionomer cements tested. The mean elastic moduli of the specimens ranged from 2.6 to 6.2 GPa after 15 min, from 13.4 to 20.4 GPa after 24 h, and from 11.4 to 22.4 GPa after 1 month. The ultrasonic method used in this study has considerable potential for determining the setting processes of luting cements.     

Ultrasonic measurement of the effects of light irradiation and presence of water on the polymerization of self‐adhesive resin cement

Self‐adhesive resin cements are useful in restorations because they reduce the number of clinical steps involved in the restoration process. This study evaluated, using ultrasonic measurements, the influence of light irradiation and the presence of water on the polymerization behavior and elastic modulus of a self‐adhesive resin cement. A self‐adhesive resin cement (RelyX Unicem 2 Automix) or a resin cement (RelyX ARC) was inserted into a transparent mold on a sample stage, and the presence of water and effect of light‐irradiation were evaluated. The transit time of a sonic wave through the cement disk was divided by the specimen thickness to obtain the sonic velocity, and longitudinal and shear waves were used to determine the elastic modulus. When the resin cements were light‐irradiated, the sonic velocity rapidly increased and plateaued at 2,500–2,700 m s^?1. When the cements were not irradiated, the rates of increase in the sonic velocity were reduced. When water was applied to the sample stage, the sonic velocity was reduced. The elastic modulus values of the specimens ranged from 9.9 to 15.9 GPa after 24 h. The polymerization behavior of self‐adhesive resin cements is affected by the polymerization mode and the presence of water.     

The effect of bleaching on the elastic modulus of bovine enamel

The purpose of this study was to determine the elastic modulus of enamel during bleaching procedure with the use of an ultrasonic device. Enamel sections were obtained from freshly extracted bovine incisors. Specimens were exposed to 10% carbamide peroxide for two hours, followed by an application of a fluoride-containing toothpaste for five minutes and stored in artificial saliva (pH 7.0). An ultrasonic device was used to measure the sound velocities of longitudinal and shear waves as well as elastic modulus. The mean elastic modulus of bleached enamel decreased with time, from 15.5 GPa to 10.1 GPa. Conversely, the elastic modulus of bleached enamel followed by application of a fluoride-containing toothpaste increased with time, from 15.2 GPa to 20.2 GPa. Results of this study indicated that a decrease in elastic modulus associated with bleaching occurred, and that fluoride-containing toothpaste reversed this effect.     

Determination of elastic modulus of the components at dentin-resin interface using the ultrasonic device

The purpose of this study was to determine the elastic moduli of the components at resin-dentin interface with the use of an ultrasonic device. Dentin plates were obtained from freshly extracted bovine incisors with a shape in rectangular form. Resin composites and bonding agents were polymerized and trimmed in the same shape as the dentin specimens. The ultrasonic equipment employed in this study was comprised of a Pulser-Receiver, transducers, and an oscilloscope. Each elastic modulus was determined by measuring the longitudinal and shear wave sound velocities. The mean elastic modulus of mineralized dentin was 17.4 GPa, while that of demineralized dentin was 1.4 GPa. When the demineralized dentin was immersed in bonding agents, the elastic modulus changed to 3.7-4.7 GPa, and these values were significantly higher than those of demineralized dentin. A gradient in elastic modulus was detected as the analysis shifted from the dentin side to the resin composite.     

Determination of elastic modulus of demineralized resin-infiltrated dentin by self-etch adhesives

The purpose of this study was to determine ultrasonically the changes in elastic modulus of demineralized adhesive-infiltrated dentin. Dentin disks were obtained from bovine incisors and shaped into a rectangular form. The specimens were immersed in single-step self-etch adhesives, then stored in distilled water and run through thermal cycles between 5 and 60 degrees C. The longitudinal and shear wave sound velocities and the elastic modulus were determined using ultrasonic equipment composed of a pulser-receiver, transducers, and an oscilloscope. After 24 h of storage, the elastic modulus of mineralized dentin was 16.9 GPa and that of demineralized dentin was 2.1 GPa. The immersion of demineralized dentin in adhesives significantly increased the elastic modulus to 3.3-5.9 GPa. After 30,000 thermal cycles, the elastic modulus of dentin was 32.4 GPa, whereas that of demineralized adhesive infiltrated dentin was 3.1-4.1 GPa. Thermal stresses did not cause adhesive-infiltrated demineralized dentin to deteriorate, as measured by elastic modulus.     

Flexural Strength, Elastic Modulus, and pH Profile of Self-etch Resin Luting Cements

Purpose: To determine the flexural strength, modulus of elasticity, and 24‐hour pH profile of three self‐etching resin luting cements and to obtain comparative data for representative conventional resin and resin‐modified glass ionomer luting cements. Materials and Methods: Three self‐etching resin luting cements [RelyX Unicem (3M ESPE), Maxcem (Kerr), Embrace Wetbond (Pulpdent)] were tested and compared with two conventional resin cements [RelyX ARC (3M ESPE), Linkmax (GC)] plus two resin‐modified glass ionomer luting cements [Fuji Plus (GC), RelyX Luting Plus (3M ESPE)]. Flexural strength and modulus of elasticity were determined using bar‐shaped specimens (2 × 2 × 25 mm³) at 24 hours, using an Instron universal testing machine. Setting pH was measured using a flat‐surface pH electrode at 0, 2, 5, 15, and 30 minutes and 1, 2, 4, 6, and 24 hours after mixing. Testing was performed under both dual‐cured and self‐cured conditions for all dual‐cure cements. Data analysis included ANOVA and Tukey's test (p < 0.05). Results: The self‐etching cements showed similar flexural strength to the conventional resin cements, except for Embrace Wetbond self‐cured, which was considerably lower. Modulus of elasticity results were both higher and lower than for conventional resin cements. All photopolymerized conventional and self‐etch dual‐cure cements showed markedly higher flexural strength and modulus than when solely self‐cured. The resin‐modified glass ionomer cements were characterized by lower flexural strength and elastic modulus. Self‐etching resin cements showed lower initial pH (2.0 to 2.4) than conventional resin cements (4.8 to 5.2) and a wide range of final pH values (3.9 to 7.3) at 24 hours. One self‐etching cement (Unicem) revealed a unique pH profile characterized by a more rapid rise in pH to neutrality both when dual‐cured (15 minutes) and when auto‐cured (1 hour). Conclusions: The self‐etching resin cements evaluated in this study displayed disparate properties and cannot be considered a homogeneous group. Flexural strength properties were most uniform and were similar to those of the conventional resin cements, whereas moduli of elasticity showed greater variation. Setting pH profiles differed, depending on the brand and mode of cure, even within the same category of luting cement. All cements with dual‐cure capability, both conventional and self‐etch, showed significantly superior properties when photopolymerized.     

Use of an ultrasonic device for the determination of elastic modulus of dentin

The mechanical properties of dentin substrate are one of the important factors in determining bond strength of dentin bonding systems. The purpose of this study was to determine the elastic modulus of dentin substrate with the use of an ultrasonic device. The dentin disks of about 1 mm thickness were obtaining from freshly extracted human third molars, and the dentin disk was shaped in a rectangular form with a line diamond point. The size and weight of each specimen was measured to calculate the density of the specimen. The ultrasonic equipment employed in this study was composed of a Pulser-Receiver (Model 5900PR, Panametrics), transducers (V155, V156, Panametrics) and an oscilloscope. The measured two-way transit time through the dentin disk was divided by two to account for the down-and-back travel path, and then multiplied by the velocity of sound in the test material. Measuring the longitudinal and share wave sound velocity determine elastic modulus. The mean elastic modulus of horizontally sectioned specimens was 21.8 GPa and 18.5 GPa for the vertically sectioned specimens, and a significant difference was found between the two groups. The ultrasonic method used in this study shows considerable promise for determination of the elastic modulus of the tooth substrate.     

Mechanical properties of new self-adhesive resin-based cement

PurposeThe aim of this study was to compare the bonding strength, flexural strength, elastic modulus, water absorption and the expansion after water storage of new self-adhesive resin cements to commercially available dental cements.MethodsTwo types (hand-mix and auto-mix) of new self-adhesive resin cements (SAC-H and SAC-A, Kuraray Medical), one conventional resin cement (Panavia F2.0), three self-adhesive resin cements (Relyx Unicem, Maxcem and G-Cem), and two resin-modified glass-ionomer cements (Fuji Luting S and Vitremer) were used. Shear bond strengths, flexural strengths and elastic moduli (ISO 4049), water absorption (ISO 4049), and the expansion rate after water storage were investigated.ResultsBoth SAC-H and SAC-A provided adhesion to enamel and dentin, and had the same bond strength to gold alloy and zirconia as conventional resin cements. SAC-H and SAC-A had greater flexural strengths (86.4–93.5 MPa) than commercial self-adhesive resin cements or glass-ionomer cements. The elastic moduli of self-adhesive and glass-ionomer cements were 5.2–7.4 GPa and 2.3–3.4 GPa, respectively. The water absorption of SAC-H and SAC-A (26.3–27.7 μg/mm³) were significantly lower than commercial self-adhesive resin cements. SAC-H and SAC-A showed significantly lower expansion rates (0.17–0.26%) than commercial self-adhesive cements and glass-ionomer cements after 4 weeks water storage.ConclusionsIt is suggested that the new self-adhesive resin cements exhibited a favorable bonding capability and mechanical properties.     

Mechanical properties of dental luting cements

STATEMENT OF PROBLEM: Dental luting cements fail by microcrack formation and bacterial ingress or by gross failure and crown dislodgment. Both of these failure modes are related to mechanical properties and deformation. PURPOSE: This study evaluated those mechanical properties of cements. METHODS AND MATERIAL. Elastic modulus for 8 representative cements (zinc phosphate, polycarboxylate, glass ionomer, encapsulated glass ionomer, resin-modified glass ionomer, resin composite, and adhesive resin composite) was measured by using a nondestructive technique and evaluated for cement type and storage time (1 hour, 1 day, 1 week, 1 month, 1 year) by 2-way ANOVA (P <.05). Compressive properties (proportional limit, resilience, and toughness), ultimate strengths (compressive, diametral tensile, and flexural), and flexural toughness were determined and evaluated by 2-way ANOVA for 2 crosshead testing rates (5 and 0.5 mm/min) and cement type (P <.05). RESULTS: Cements varied with respect to elastic moduli, compressive proportional limit, compressive resilience, compressive strength, compressive toughness, diametral tensile strength, flexural strength, and flexural toughness. Storage time affected the elastic moduli of different materials in different ways. Elastic moduli of polycarboxylate and glass ionomer cements increased over time, whereas the other materials changed little after the first day. Crosshead rate only significantly affected compressive proportional limit and resilience. CONCLUSIONS: Luting cements differed considerably with respect to mechanical properties.     

Effects of sonic toothbrush use on permanent dental luting cements

The aim of this project was to assess the effects of sonic toothbrushes on commonly used permanent luting cements. While results showed differences between the tensile bond strengths of the three cements, the differences were similar between the two groups: sonic and nonsonic toohbrush exposure. These findings suggest that the sonic toothbrush had no significant effect on the tensile bond strengths of any of the three tested cements.     

Evaluation of adhesive defects using an ultrasonic pulse-reflection technique

The purpose of this study was to examine the application of an ultrasonic pulse-reflection technique for the evaluation of adhesive defects. First, the sonic velocities in the enamel and dentin of human molars and bovine incisors were measured with a pulsar receiver attached to an ultrasonic transducer. The identification of the dentino-enamel junction and pulp-dentin interface using the ultrasonic method based on intrinsic sonic velocities showed good agreement with the actual measured thicknesses. Next, a cemented restoration with artificial faults was prepared. Half of the Au-Ag-Pd alloy plate area was cemented to the dentin slab using luting resin cement. The adhesive interface was evaluated with a high-resolution ultrasonic imaging system. Clear internal faults were evident from the ultrasonic tomogram. The findings of this study suggest that the ultrasonic pulse-reflection technique may be useful for inspecting and imaging structural defects of adhesive interfaces.     

Dynamic viscoelastic behavior of resin cements measured by torsional resonance.

OBJECTIVE: The purpose of the study was to measure the viscoelastic properties of four dental resin composite cements using a dynamic mechanical analysis technique. METHODS: Dynamic torsional loading was conducted in the frequency range from 1 to 80 Hz. Cement specimens were tested after storage in 37 degrees C water for 24 h. One group was thermal cycled prior to testing. Measurements were taken at 21, 37, and 50 degrees C. Storage modulus, loss tangent and other viscoelastic parameters were determined from the amplitude/frequency curves. RESULTS: Storage moduli of the cements ranged from 2.9 to 4.1 GPa at 37 degrees C. Loss tangents ranged from 0.054 to 0.084. Storage moduli decreased in a regular way with increasing temperature, whereas, loss tangents increased. Thermal cycling caused small decreases in storage moduli. SIGNIFICANCE: Resin cements with higher filler loading were found to have higher storage moduli and lower loss tangents. Since these properties have been associated with better clinical performance in the areas of retention and prevention of fracture of porcelain and resin restorations, the more highly filled cements may be recommended. Temperature variations influenced viscoelastic behavior of the cements. However, within the temperature range studied no sharp drop in modulus was seen, so the materials should function satisfactorily in the oral cavity.     

Marginal and flexural integrity of three classes of luting cement, with early finishing and water storage.

OBJECTIVES: The aims of this investigation were to clarify the effects of finishing-time and 24 h water-storage on mechanical properties and marginal adaptation to dentin of seven modern luting cements, representing three chemical types. METHODS: Bistite II, Chemiace II, Compolute, XenoCem, PermaCem, Fuji Cem and Fuji Plus were investigated with specimen sub-groups (N=10) for each property measured. The principal series of experiments was conducted in dentin cavities with interfacial polishing either immediately (3 min) after setting or after 24 h water-storage. After the finishing procedure, the maximum marginal gap width and the opposing width (if any) per cavity were measured microscopically, and summed. Then the overall sum of gap-widths (per group; N=10) was calculated. Marginal gaps were similarly measured in Teflon cavities, together with shear-bond-strengths to dentin and early flexural strengths, moduli and swelling data. RESULTS: For specimen-sets polished immediately after setting, summed marginal gaps of 23-121 microm were observed, for all luting cements except Compolute. A significantly different (p<0.05) result of either no gap or 6-28 microm summed gap-widths occurred in specimens polished after 24 h. For all materials, their shear-bond-strengths, flexural strength and moduli significantly increased after 24 h storage. SIGNIFICANCE: The marginal behavior can be interpreted in terms of the contributions of bonding, shrinkage, swelling and compliance of components, along with compositional features of the cements. With these types of cement it is generally inadvisable to polish the interfacial luting surface immediately after cementing. The polishing procedures should be carried out not less than 24 h later. One resin-cement was able to withstand immediate finishing.     

Adhesive post-endodontic restorations with fiber posts: push-out tests and SEM observations.

OBJECTIVES: Nowadays, the restoration of endodontically treated teeth is based on the use of materials with a modulus of elasticity similar to that of dentin (18.6 GPa). Fiber posts, resin cements and some composite resins all have this characteristic. This study evaluated the bond strength between luting materials, root dentin and fiber posts through push-out tests and examined the integration among these three components through scanning electron microscopy. METHODS: Endodontically treated extracted teeth and plastic plates were used to test the interface between luting agent and dentin and luting agent and post. RESULTS: Chemical affinity between different components (luting materials and fiber posts) is extremely important in achieving high bond strength. The bond strength tests and SEM observations showed that in vitro, composite resins perform better than resin cements. SIGNIFICANCE: The in vivo use of these materials may significantly reinforce residual tooth structure therefore reducing the risk for fracture and debonding.     

A micromechanics model of the elastic properties of human dentine.

A generalized, self-consistent model of cylindrical inclusions in a homogeneous and isotropic matrix phase was used to study the effects of tubule orientation on the elastic properties of dentine. Closed-form expressions for the five independent elastic constants of dentine were derived in terms of tubule concentration, and the Young's moduli and Poisson ratios of peri- and intertubular dentine. An atomic-force microscope indentation technique determined the Young's moduli of the peri- and intertubular dentine as approx. 30 and 15 GPa, respectively. Over the natural variation in tubule density found in dentine, there was only a slight variation in the axial and transverse shear moduli with position in the tooth, and there was no measurable effect of tubule orientation. It was concluded that tubule orientation has no appreciable effect on the elastic behaviour of normal dentine, and that the elastic properties of healthy dentine can be modelled as an isotropic continuum with a Young's modulus of approx. 16 GPa and a shear modulus of 6.2 GPa.     

Correlation of filler content and elastic properties of resin-composites.

OBJECTIVES: The aim was to determine the Young's modulus (E), bulk modulus (B), shear modulus (G) and Poisson's ratio (nu) of a series of composite restorative materials and to correlate them with their filler volume-fractions. METHODS: Twelve model resin-composite formulations, with systematically varied volume-fraction (Tokuyama), a flowable resin-composite (Point 4 flowable, Kerr) and two hybrid resin-composites (Filtek Supreme XT, 3M-Espe & X-tra Fil, Voco) were investigated. Twelve cylindrical specimens (5 mm x 6 mm) were prepared from each material. Six were free to expand radially under axial compressive loading, and were used to calculate the Young's modulus (E). The other six were radially constricted in a rigid stainless steel ring during loading, from which the bulk modulus (B) was calculated. Compression loading was performed at 1mm/min. The Young's and bulk moduli were determined using equations of elasticity. Poisson's ratio from nu=0.5-(E/6B) and shear modulus from G=E/2(1+nu). RESULTS: Young's moduli ranged from 2.19 to 7.15GPa, bulk moduli from 12.79 to 22.43GPa and shear moduli from 0.74 to 2.47GPa. Poisson's ratio ranged from 0.45 for the stiffer to 0.47 for the more compliant composites. Statistically significant differences (ANOVA and Bonferroni at p=0.05) were found depending on filler volume-fraction. SIGNIFICANCE: Elastic moduli varied significantly and a positive correlation existed between elastic moduli and filler volume-fraction (r2: 0.905-0.992 and 0.940-1.000 for Young's and bulk moduli, respectively).     

Resin elasticity and the strengthening of all-ceramic restorations

Resin luting of all-ceramic restorations results in increased performance; however, the strengthening mechanism and the role of the mechanical properties of the resin are not fully understood. The hypothesis tested is that ceramic strength enhancement is dependent on the elastic modulus of the resin. Three-point flexural moduli of a flowable, luting, and hybrid composite resin were characterized. Two hundred forty porcelain discs were air-abraded. One group acted as a control, and 3 additional groups were coated with 120 +/- 20 microm of each resin prior to bi-axial flexure testing. All resins significantly increased in mean strength, and the associated strength increase was related to the elastic modulus of the resin (R(2) = 0.9885), so the hypothesis was accepted. The combination of Poisson constraint and the creation of a resin-inter-penetrating layer sensitive to the elastic modulus of the resin may provide an explanation of the strengthening mechanism.     

Finite element analysis model to simulate the behavior of luting cements during setting.

OBJECTIVES: Besides the fixation of the restoration, an important function of dental luting cements is to seal the gap between tooth and restoration. However, as a result of adhesion, curing contraction is hindered, creating stresses. To maintain the seal these stresses neither exceed the bond nor the cohesive strength of the cement. The aim of this study was to evaluate a rather simple model, which mimics the setting behavior of luting cements based on the division of the setting process into a liquid, visco-elastic and elastic phase, for its suitability to predict in Finite Element Analysis (FEA) the magnitude of the setting stresses occurring clinically. METHODS: Commercial luting cement, RelyX ARC, was used in this study. In a dynamic test set-up the stresses, the elastic strain, and the shrinkage were determined. Two layers with different thicknesses and different ratios between bonded and free surface (C-factor) were examined. The parameters were used in three-dimensional FEA models. The experimental contraction stresses were compared with the results of the FEA. RESULTS: In cement layers with uniform layer thickness, it is possible to predict the contraction stresses with the found parameters. The smallest plastic deformations and contraction stresses were found in the thinnest layer. The studied model was reliable in predicting the experimental stresses. SIGNIFICANCE: The results of this study may be used for the prediction using FEA of the actual stresses occurring in dental restorations.     

Antibacterial potential of contemporary dental luting cements

The aims of this investigation were to evaluate the antibacterial activities of different types of dental luting cements and to compare antibacterial action during and after setting. Agar diffusion testing was used to evaluate the antibacterial properties of seven types of dental luting cements (glass ionomer cements (GICs), resin modified GICs, resin composite, zinc oxide eugenol, zinc oxide non-eugenol, zinc phosphate, zinc polycarboxylate cements) on Streptococcus mutans bacteria. Instantly mixed zinc phosphate cements showed the strongest antibacterial activity in contrast to the non-eugenol, eugenol and resin cements that did not show any antibacterial effects. Non-hardened glass ionomer, resin modified and zinc polycarboxylate cements exhibited moderate antibacterial action. Hardened cements showed weaker antibacterial activities, than those ones applied right after mixing.     

Mechanical and physical properties of contemporary dental luting agents

STATEMENT OF PROBLEM: New luting agents, particularly with adhesive capability, are being introduced in an attempt to improve clinical success. Independent studies of basic comparative data are necessary to characterize these materials in relation to mechanical and physical properties. PURPOSE: The purpose of this study was to compare the flexural strength, modulus of elasticity, and radiopacity and pH of representatives of 5 types (categories) of luting agents. MATERIAL AND METHODS: The luting agents included a zinc phosphate, a conventional and a resin-modified glass ionomer, 2 dual-polymerizing resins ("photopolymerized" after mixing and "unphotopolymerized" conditions), and an auto-polymerizing resin. The specimens were prepared and the testing was conducted by 1 person to maximize standardization. Flexural strength (MPa) and modulus of elasticity (GPa) were determined on bar-shaped specimens (2 x 2 x 20 mm) at 24 hours and 3 months (n = 8). Radiopacity (mm Al) was measured by exposing 1 mm thick specimens along with an aluminum step wedge (n = 4). pH was measured using a pH electrode immediately after mixing; at 1, 5, 15, 30 minutes; and at 1, 2, 4, 6, and 24 hours (n = 4). The data were subjected to statistical analyses with analysis of variance and Duncan's multiple range test (P<.05). RESULTS: The resin luting agents (64 to 97 MPa) showed higher flexural strength than all other materials tested (7 to 27 MPa), with the "photopolymerized" (83 to 97 MPa) conditions higher than "unphotopolymerized" (64 to 81 MPa) (P<.0005). Zinc phosphate was the most radiopaque (6.4 mm Al) (P<.0001) and provided the highest rigidity (9.2 GPa) (P<.05). The autopolymerization resin cement was the most radiolucent (1.1 mm Al) (P<.0001). Zinc phosphate and conventional glass ionomer cements were the most acidic immediately after mixing (pH 1.5 to 2.2) but were the least acidic after 24 hours (pH 6.4 to 6.8) (P<.0001). CONCLUSIONS: Within the limitations of this study the data showed a wide variation of material properties. The dual-polymerization resin luting agents tested showed the best combination of mechanical and physical properties combined with the highest setting pH. Photopolymerization of these resin-based materials was necessary to maximize strength and rigidity.