Slow crack growth and reliability of dental ceramics

Objective. To determine the slow crack growth (SCG) and Weibull parameters of five dental ceramics: a vitreous porcelain (V), a leucite-based porcelain (D), a leucite-based glass-ceramic (E1), a lithium disilicate glass-ceramic (E2) and a glass-infiltrated alumina composite (IC). Methods. Eighty disks (empty set 12mm x 1.1mm thick) of each material were constructed according to manufacturers` recommendations and polished. The stress corrosion susceptibility coefficient (n) was obtained by dynamic fatigue test, and specimens were tested in biaxial flexure at five stress rates immersed in artificial saliva at 37 degrees C. Weibull parameters were calculated for the 30 specimens tested at 1MPa/s in artificial saliva at 37 degrees C. The 80 specimens were distributed as follows: 10 for each stress rate (10(-2), 10(-1), 10(1), 10(2) MPa/s), 10 for inert strength (10(2) MPa/s, silicon oil) and 30 for 10(0) MPa/s. Fractographic analysis was also performed to investigate the fracture origin. Results. E2 showed the lowest slow crack growth susceptibility coefficient (17.2), followed by D (20.4) and V (26.3). E1 and IC presented the highest n values (30.1 and 31.1, respectively). Porcelain V presented the lowest Weibull modulus (5.2). All other materials showed similar Weibull modulus values, ranging from 9.4 to 11.7. Fractographic analysis indicated that for porcelain D, glass-ceramics E1 and E2, and composite IC crack deflection was the main toughening mechanism. Significance. This study provides a detailed microstructural and slow crack growth characterization of widely used dental ceramics. This is important from a clinical standpoint to assist the clinician in choosing the best ceramic material for each situation as well as predicting its clinical longevity. It also can be helpful in developing new materials for dental prostheses. (c) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of ion exchange on R-curve behavior of a dental porcelain

The objective of this study was to evaluate the effect of the ion exchange treatment on the R-curve behavior of a leucite-reinforced dental porcelain, testing the hypothesis that the ion exchange is able to improve the R-curve behavior of the porcelain studied. Porcelain disks were sintered, finely polished, and submitted to an ion exchange treatment with a KNO(3) paste. The R-curve behavior was assessed by fracturing the specimens in a biaxial flexure design after making Vickers indentations in the center of the polished surface with loads of 1.8, 3.1, 4.9, 9.8, 31.4, and 49.0 N. The results showed that the ion exchange process resulted in significant improvements in terms of fracture toughness and flexural strength as compared to the untreated material. Nevertheless, the rising R-curve behavior previously observed in the control group disappeared after the ion exchange treatment, i.e., fracture toughness did not increase with the increase in crack size for the treated group.

Mechanical characterization of proanthocyanidindentin matrix interaction

Objectives To characterize the properties of dentin matrix treated with two proanthocyanidin rich cross-linking agents and their effect on dentin bonded interfaces. Methods Sound human molars were cut into 0.5mm thick dentin slabs, demineralized and either treated with one of two cross-linking agents (grape seedGSE and cocoa seedCOE extracts) or left untreated. The modulus of elasticity of demineralized dentin was assessed after 10 or 60min and the swelling ratio after 60min treatment. Bacterial collagenase was also used to assess resistance to enzymatic degradation of samples subjected to ultimate tensile strength. The effect of GSE or COE on the resindentin bond strength was evaluated after 10 or 60min of exposure time. Data were statistically analyzed at a 95% confidence interval. Results Both cross-linkers increased the elastic modulus of demineralized dentin as exposure time increased. Swelling ratio was lower for treated samples when compared to control groups. No statistically significant changes to the UTS indicate that collagenase had no effect on dentin matrix treated with either GSE or COE. Resindentin bonds significantly increased following treatment with GSE regardless of the application time or adhesive system used. Significance Increased mechanical properties and stability of dentin matrix can be achieved by the use of PA-rich collagen cross-linkers most likely due to the formation of a PAcollagen complex. The short term resindentin bonds can be improved after 10min dentin treatment.(C) 2010 Academy of Denta lMaterials. Published by Elsevier Ltd. All rights reserved.

Composite pre-heating: Effects on marginal adaptation, degree of conversion and mechanical properties

Objectives. This study evaluated the effect of composite pre-polymerization temperature and energy density on the marginal adaptation (MA), degree of conversion (DC), flexural strength (FS), and polymer cross-linking (PCL) of a resin composite (Filtek Z350, 3M/ESPE). Methods. For MA, class V cavities (4mmx2mmx2mm) were prepared in 40 bovine incisors. The adhesive system Adper Single Bond 2 (3M/ESPE) was applied. Before being placed in the cavities, the resin composite was either kept at room-temperature (25 degrees C) or previously pre-heated to 68 degrees C in the Calset (TM) device (AdDent Inc., Danbury, CT, USA). The composite was then light polymerized for 20 or 40s at 600mW/cm(2) (12 or 24 J/cm(2), respectively). The percentage of gaps was analyzed by scanning electron microscopy, after sectioning the restorations and preparing epoxy resin replicas. DC (n = 3) was obtained by FT-Raman spectroscopy on irradiated and non-irradiated composite surfaces. FS (n = 10) was measured by the three-point-bending test. KHN (n = 6) was measured after 24h dry storage and again after immersion in 100% ethanol solution for 24 h, to calculate PCL density. Data were analyzed by appropriate statistical analyses. Results. The pre-heated composite showed better MA than the room-temperature groups. A higher number of gaps were observed in the room-temperature groups, irrespective of the energy density, mainly in the axial wall (p < 0.05). Composite pre-heating and energy density did not affect the DC, FS and PCL (p > 0.05). Significance. Pre-heating the composite prior to light polymerization similar in a clinical situation did not alter the mechanical properties and monomer conversion of the composite, but provided enhanced composite adaptation to cavity walls. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of ion-exchange temperature on mechanical properties of a dental porcelain

The objective of this study was to determine the influence of different ion-exchange temperatures on the biaxial flexural strength (sigma(f)), hardness (HV) and indentation fracture resistance (K(IF)) of a dental porcelain. Disk-shaped specimens were divided into five groups (n = 10) and submitted to an ion-exchange procedure using KNO(3) paste for 15 min in the following temperatures (degrees C); (I) 430; (II) 450; (III) 470; (IV) 490; (V) 510; and control (no ion exchange). The value of sigma(f) was determined in artificial saliva at 37 degrees C. The values of HV and K(IF) were obtained using 3 Vickers indentations in each specimen (19.6 N). Results showed that ion exchange increases significantly the properties of the material as compared to the control and no significant differences were found among the temperatures tested for any of the properties studied. (C) 2010 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Long-term effect of carbodiimide on dentin matrix and resin-dentin bonds

Objectives: To characterize the interaction of 1-Ethyl-3-[3-dimethylaminopropyl] carbodiimide Hydrochloride (EDC) with dentin matrix and its effect on the resin-dentin bond. Methods: Changes to the stiffness of demineralized dentin fragments treated with EDC/N-hydroxysuccinimide (NHS) in different solutions were evaluated at different time points. The resistance against enzymatic degradation was indirectly evaluated by ultimate tensile strength (UTS) test of demineralized dentin treated or not with EDC/NHS and subjected to collagenase digestion. Short- and long-term evaluations of the strength of resin-dentin interfaces treated with EDC/NHS for 1 h were performed using microtensile bond strength (mu TBS) test. All data (MPa) were individually analyzed using ANOVA and Tukey HSD tests (alpha = 0.05). Results: The different exposure times significantly increased the stiffness of dentin (p < 0.0001, control-5.15 and EDC/NHS-29.50), while no differences were observed among the different solutions of EDC/NHS (p = 0.063). Collagenase challenge did not affect the UTS values of EDC/NHS group (6.08) (p > 0.05), while complete degradation was observed for the control group (p = 0.0008, control-20.84 and EDC/NHS-43.15). EDC/NHS treatment did not significantly increase resin-dentin mu TBS, but the values remained stable after 12 months water storage (p < 0.05). Conclusions: Biomimetic use of EDC/NHS to induce exogenous collagen cross-links resulted in increased mechanical properties and stability of dentin matrix and dentin-resin interfaces. (C) 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 94B: 250-255, 2010.

One-year stability of resin-dentin bonds created with a hydrophobic ethanol-wet bonding technique

Dentin bonding performed with hydrophobic resins using ethanol-wet bonding should be less susceptible to degradation but this hypothesis has never been validated. Objectives. This in vitro study evaluated stability of resin-dentin bonds created with an experimental three-step BisGMA/TEGDMA hydrophobic adhesive or a three-step hydrophilic adhesive after one year of accelerated aging in artificial saliva. Methods. Flat surfaces in mid-coronal dentin were obtained from 45 sound human molars and randomly divided into three groups (n = 15): an experimental three-step BisGMA/TEGDMA hydrophobic adhesive applied to ethanol (ethanol-wet bonding-GI) or water-saturated dentin (water-wet bonding-GII) and Adper Scotchbond Multi-Purpose [MP-GIII] applied, according to manufacturer instructions, to water-saturated dentin. Resin composite crowns were incrementally formed and light-cured to approximately 5 mm in height. Bonded specimens were stored in artificial saliva at 37 degrees C for 24h and sectioned into sticks. They were subjected to microtensile bond test and TEM analysis immediately and after one year. Data were analyzed with two-way ANOVA and Tukey tests. Results. MP exhibited significant reduction in microtensile bond strength after aging (24 h: 40.6 +/- 2.5(a); one year: 27.5 +/- 3.3(b); in MPa). Hybrid layer degradation was evident in all specimens examined by TEM. The hydrophobic adhesive with ethanol-wet bonding preserved bond strength (24 h: 43.7 +/- 7.4(a); one year: 39.8 +/- 2.7(a)) and hybrid layer integrity, with the latter demonstrating intact collagen fibrils and wide interfibrillar spaces. Significance. Coaxing hydrophobic resins into acid-etched dentin using ethanol-wet bonding preserves resin-dentin bond integrity without the adjunctive use of MMPs inhibitors and warrants further biocompatibility and patient safety`s studies and clinical testing. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Direct comparison of the bond strength results of the different test methods: A critical literature review

Objective. The goal of this paper is to undertake a literature search collecting all dentin bond strength data obtained for six adhesives with four tests ( shear, microshear, tensile and microtensile) and to critically analyze the results with respect to average bond strength, coefficient of variation, mode of failure and product ranking. Method. A PubMed search was carried out for the years between 1998 and 2009 identifying publications on bond strength measurements of resin composite to dentin using four tests: shear, tensile, microshear and microtensile. The six adhesive resins were selected covering three step systems ( OptiBond FL, Scotch Bond Multi-Purpose Plus), two-step (Prime & Bond NT, Single Bond, Clear. l SE Bond) and one step (Adper Prompt L Pop). Results. Pooling results from 147 references showed an ongoing high scatter in the bond strength data regardless which adhesive and which bond test was used. Coefficients of variation remained high (20-50%) even with the microbond test. The reported modes of failure for all tests still included high number of cohesive failures. The ranking seemed to be dependant on the test used. Significance. The scatter in dentin bond strength data remains regardless which test is used confirming Finite Element Analysis predicting non-uniform stress distributions due to a number of geometrical, loading, material properties and specimens preparation variables. This reopens the question whether, an interfacial fracture mechanics approach to analyze the dentin - adhesive bond is not more appropriate for obtaining better agreement among dentin bond related papers. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of argon purity on mechanical properties, microstructure and fracture mode of commercially pure (cp) Ti and Ti-6Al-4V alloys for ceramometal dental prostheses

Provision of an inert gas atmosphere with high-purity argon gas is recommended for preventing titanium castings from contamination although the effects of the level of argon purity on the mechanical properties and the clinical performance of Ti castings have not yet been investigated. The purpose of this study was to evaluate the effect of argon purity on the mechanical properties and microstructure of commercially pure (cp) Ti and Ti-6Al-4V alloys. The castings were made using either high-purity and/or industrial argon gas. The ultimate tensile strength (UTS), proportional limit (PL), elongation (EL) and microhardness (VHN) at different depths were evaluated. The microstructure of the alloys was also revealed and the fracture mode was analyzed by scanning electron microscopy. The data from the mechanical tests and hardness were subjected to a two-and three-way ANOVA and Tukey`s test (alpha = 0.05). The mean values of mechanical properties were not affected by the argon gas purity. Higher UTS, PL and VHN, and lower EL were observed for Ti-6Al-4V. The microhardness was not influenced by the argon gas purity. The industrial argon gas can be used to cast cp Ti and Ti-6Al-4V.

Effect of processing induced particle alignment on the fracture toughness and fracture behavior of multiphase dental ceramics

Objective. To investigate the processing induced particle alignment on fracture behavior of four multiphase dental ceramics (one porcelain, two glass-ceramics and a glass-infiltrated-alumina composite). Methods. Disks (empty set12mm x 1.1 mm-thick) and bars (3 mm x 4 mm x 20 mm) of each material were processed according to manufacturer instructions, machined and polished. Fracture toughness (K(IC)) was determined by the indentation strength method using 3-point bending and biaxial flexure fixtures for the fracture of bars and disks, respectively. Microstructural and fractographic analyses were performed with scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction. Results. The isotropic microstructure of the porcelain and the leucite-based glass-ceramic resulted in similar fracture toughness values regardless of the specimen geometry. On the other hand, materials containing second-phase particles with high aspect ratio (lithium disilicate glass-ceramic and glass-infiltrated-alumina composite) showed lower fracture toughness for disk specimens compared to bars. For the lithium disilicate glass-ceramic disks, it was demonstrated that the occurrence of particle alignment during the heat-pressing procedure resulted in an unfavorable pattern that created weak microstructural paths during the biaxial test. For the glass-infiltrated-alumina composite, the microstructural analysis showed that the large alumina platelets tended to align their large surfaces perpendicularly to the direction of particle deposition during slip casting of green preforms. Significance. The fracture toughness of dental ceramics with anisotropic microstructure should be determined by means of biaxial testing, since it results in lower values. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of ion exchange on strength and slow crack growth of a dental porcelain

Objectives. To determine the effect of ion exchange on slow crack growth (SCG) parameters (n, stress corrosion susceptibility coefficient, and sigma(f0), scaling parameter) and Weibull parameters (m, Weibull modulus, and sigma(0), characteristic strength) of a dental porcelain. Methods. 160 porcelain discs were fabricated according to manufacturer`s instructions, polished through 1 mu m and divided into two groups: GC (control) and GI (submitted to an ion exchange procedure using a KNO(3) paste at 470 degrees C for 15 min). SCG parameters were determined by biaxial flexural strength test in artificial saliva at 37 degrees C using five constant stress rates (n =10). 20 specimens of each group were tested at 1 MPa/s to determine Weibull parameters. The SPT diagram was constructed using the least-squares fit of the strength data versus probability of failure. Results. Mean values of m and sigma(0) (95% confidence interval), n and sigma(f0) (standard deviation) were, respectively: 13.8 (10.1-18.8) and 60.4 (58.5 - 62.2), 24.1 (2.5) and 58.1 (0.01) for GC and 7.4 (5.3 -10.0) and 136.8 (129.1-144.7), 36.7 (7.3) and 127.9 (0.01) for GI. Fracture stresses (MPa) calculated using the SPT diagram for lifetimes of 1 day, 1 year and 10 years (at a 5% failure probability) were, respectively, 31.8, 24.9 and 22.7 for GC and 71.2, 60.6 and 56.9 for GI. Significance. For the porcelain tested, the ion exchange process improved strength and resistance to SCG, however, the material`s reliability decreased. The predicted fracture stress at 5% failure probability for a lifetime of 10 years was also higher for the ion treated group. (C) 009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Subcritical crack growth in porcelains, glass-ceramics, and glass-infiltrated alumina composite for dental restorations

The objective was to compare fracture toughness (K(Ic)), stress corrosion susceptibility coefficient (n), and stress intensity factor threshold for crack propagation (K(I0)) of two porcelains [VM7/Vita (V) and d.Sign/Ivoclar (D)], two glass-ceramics [Empress/Ivolcar (E1) and Empress2/Ivlocar (E2)] and a glass-infiltrated alumina composite [In-Ceram Alumina/Vita (IC)]. Disks were constructed according to each manufacturer`s processing method, and polished before induction of cracks by a Vickers indenter. Crack lengths were measured under optical microscopy at times between 0.1 and 100 h. Specimens were stored in artificial saliva at 37A degrees C during the whole experiment. K(Ic) and n were determined using indentation fracture method. K(I0) was determined by plotting log crack velocity versus log K(I). Microstructure characterization was carried out under SEM, EDS, X-ray diffraction and X-ray fluorescence. IC and E2 presented higher K(Ic) and K(I0) compared to E1, V, and D. IC presented the highest n value, followed by E2, D, E1, and V in a decreasing order. V and D presented similar K(Ic), but porcelain V showed higher K(I0) and lower n compared to D. Microstructure features (volume fraction, size, aspect ratio of crystalline phases and chemical composition of glassy matrix) determined K(Ic). The increase of K(Ic) value favored the increases of n and K(I0).

Effect of the microstructure on the lifetime of dental ceramics

Objectives. To evaluate the effect of the microstructure on the Weibull and slow crack growth (SCG) parameters and on the lifetime of three ceramics used as framework materials for fixed partial dentures (FPDs) (YZ - Vita In-Ceram YZ; IZ - Vita In-Ceram Zirconia; AL - Vita In-Ceram AL) and of two veneering porcelains (VM7 and VM9). Methods. Bar-shaped specimens were fabricated according to the manufacturer`s instructions. Specimens were tested in three-point flexure in 37 degrees C artificial saliva. Weibull analysis (n = 30) and a constant stress-rate test (n = 10) were used to determine the Weibull modulus (m) and SCG coefficient (n), respectively. Microstructural and fractographic analyzes were performed using SEM. ANOVA and Tukey`s test (alpha = 0.05) were used to statistically analyze data obtained with both microstructural and fractographic analyzes. Results. YZ and AL presented high crystalline content and low porosity (0.1-0.2%). YZ had the highest characteristic strength (sigma(0)) value (911 MPa) followed by AL (488 MPa) and IZ (423 MPa). Lower sigma(0) values were observed for the porcelains (68-75 MPa). Except for IZ and VM7, m values were similar among the ceramic materials. Higher n values were found for YZ (76) and AL (72), followed by IZ (54) and the veneering materials (36-44). Lifetime predictions showed that YZ was the material with the best mechanical performance. The size of the critical flaw was similar among the framework materials (34-48 mu m) and among the porcelains (75-86 mu m). Significance. The microstructure influenced the mechanical and SCG behavior of the studied materials and, consequently, the lifetime predictions. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of leucite content on slow crack growth of dental porcelains

Objectives. To determine the stress corrosion susceptibility coefficient, n, of seven dental porcelains (A: Ceramco I; B: Ceramco-II; C: Ceramco-III; D: d.Sign; E: Cerabien; F: Vitadur-Alpha; and G: Ultropaline) after aging in air or artificial saliva, and correlate results with leucite content (LC). Methods. Bars were fired according to manufacturers` instructions and polished before induction of cracks by a Vickers indenter (19.6 N, 20 s). Four specimens were stored in air/room temperature, and three in saliva/37 degrees C. Five indentations were made per specimen and crack lengths measured at the following times: similar to 0; 1; 3; 10; 30; 100; 300; 1000 and 3000 h. The stress corrosion coefficient n was calculated by linear regression analysis after plotting crack length as a function of time, considering that the slope of the curve was (2/(3n + 2)]. Microstructural analysis was performed to determine LC. Results. LC of the porcelains were 22% (A and B); 6% (C); 15% (D); 0% (E and F); and 13% (G). Except for porcelains A and D, all materials showed a decrease in their n values when stored in artificial saliva. However, the decrease was more pronounced for porcelains B, F, and G. Ranking of materials varied according to storage media (in air, porcelain G showed higher n compared to A, while in saliva both showed similar coefficients). No correlation was found between n values and LC in air or saliva. Significance. Storage media influenced the n value obtained for most of the materials. LC did not affect resistance to slow crack growth regardless of the test environment. (c) 2008 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of pH on slow crack growth of dental porcelains

Objectives. To evaluate the effect of pH of storage medium on slow crack growth (SCG) parameters of dental porcelains. Methods. Two porcelains were selected: with (UD) and without (VM7) leucite particles, in order to assess if the microstructure would affect the response of the material to the pH variation. Disc specimens were produced following manufacturers` instructions. Specimens were stored in artificial saliva in pHs 3.5, 7.0 or 10.0 for 10 days and after that the fatigue parameters (n: SCG susceptibility coefficient and sigma(0): scaling parameter) were obtained by the dynamic fatigue test using the same pH of storage. Microstructural analysis of the materials was also performed. Results. For VM7, the values of n obtained in the different pHs were similar and varied from 29.9 to 31.2. The sigma(0) value obtained in pH 7.0 for VM7 was higher than that obtained in the other pHs, which were similar. For porcelain UD, n values obtained in pHs 7.0 and 10.0 were similar (40.8 and 39.6, respectively), and higher than that obtained in pH 3.5 (26.5). With respect to sigma(0), the value obtained for porcelain UD in pH 10.0 was lower than those obtained in pHs 3.5 and 7.0, which were similar. Significance. The effect of pH on the stress corrosion susceptibility (n) depended on the porcelain studied. While the n value of VM7 was not affected by the pH, UD presented lower n value in acid pH. For both porcelains, storage in acid or basic pH resulted in strength degradation. (C) 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.