The significance of brittle reaction layers in fusing of dental ceramics to titanium

This thesis comprises four intercomplementary parts that introduce new approaches to brittle reaction layers and mechanical compatibility of metalloceramic joints created when fusing dental ceramics to titanium. Several different methods including atomic layer deposition (ALD), sessile drop contact angle measurements, scanning acoustic microscopy (SAM), three-point bending (TPB, DIN 13 927 / ISO 9693), cross-section microscopy, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS) were employed. The first part investigates the effects of TiO2 layer structure and thickness on the joint strength of the titanium-metalloceramic system. Samples with all tested TiO2 thicknesses displayed good ceramics adhesion to Ti, and uniform TPB results. The fracture mode was independent of oxide layer thickness and structure. Cracking occurred deeper inside titanium, in the oxygen-rich Ti[O]x solid solution surface layer. During dental ceramics firing TiO2 layers dissociate and joints become brittle with increased dissolution of oxygen into metallic Ti and consequent reduction in the metal plasticity. To accomplish an ideal metalloceramic joint this needs to be resolved. The second part introduces photoinduced superhydrophilicity of TiO2. Test samples with ALD deposited anatase TiO2 films were produced. Samples were irradiated with UV light to induce superhydrophilicity of the surfaces through a cascade leading to increased amount of surface hydroxyl groups. Superhydrophilicity (contact angle ~0˚) was achieved within 2 minutes of UV radiation. Partial recovery of the contact angle was observed during the first 10 minutes after UV exposure. Total recovery was not observed within 24h storage. Photoinduced ultrahydrophilicity can be used to enhance wettability of titanium surfaces, an important factor in dental ceramics veneering processes. The third part addresses interlayers designed to restrain oxygen dissolution into Ti during dental ceramics fusing. The main requirements for an ideal interlayer material are proposed. Based on these criteria and systematic exclusion of possible interlayer materials silver (Ag) interlayers were chosen. TPB results were significantly better in when 5 μm Ag interlayers were used compared to only Al2O3-blasted samples. In samples with these Ag interlayers multiple cracks occurred inside dental ceramics, none inside Ti structure. Ag interlayers of 5 μm on Al2O3-blasted samples can be efficiently used to retard formation of the brittle oxygen-rich Ti[O]x layer, thus enhancing metalloceramic joint integrity. The most brittle component in metalloceramic joints with 5 μm Ag interlayers was bulk dental ceramics instead of Ti[O]x. The fourth part investigates the importance of mechanical interlocking. According to the results, the significance of mechanical interlocking achieved by conventional surface treatments can be questioned as long as the formation of the brittle layers (mainly oxygen-rich Ti[O]x) cannot be sufficiently controlled. In summary in contrast to former impressions of thick titanium oxide layers this thesis clearly demonstrates diffusion of oxygen from sintering atmosphere and SiO2 to Ti structures during dental ceramics firing and the following formation of brittle Ti[O]x solid solution as the most important factors predisposing joints between Ti and SiO2-based dental ceramics to low strength. This among other predisposing factors such as residual stresses created by the coefficient of thermal expansion mismatch between dental ceramics and Ti frameworks can be avoided with Ag interlayers.

COLOR STABILITY OF DENTAL CERAMICS SUBMITTED TO ARTIFICIAL ACCELERATED AGING AFTER REPEATED FIRINGS

Statement of problem. Color stability is an important factor to ensure the long-term clinical success of ceramic restorations. There is a lack of information on how color is affected by fabrication procedures, such as the number of firings. Purpose. The purpose of this study was to evaluate the effects that the number of firings and type of substrate have on the color stability of dental ceramic submitted to artificial accelerated aging. Material and methods. Sixty specimens were fabricated: 30 metal ceramic (Verabond II + IPS d.SIGN) and 30 all-ceramic (IPS d.SIGN). Specimens were divided into 3 groups (n=10), and submitted to 2, 3, or 4 firings (+/- 900 degrees C), respectively, according to the manufacturer`s instructions. Color readings were obtained with a spectro photometer before and after artificial accelerated aging, and L*, a*, and b* coordinates and total color variation (Delta E) were analyzed (2-way ANOVA, Bonferroni, (alpha=05). Results. For metal ceramic specimens, differences for the L* coordinates were significant (P<.05) only for the group submitted to 3 firings. With respect to the all-ceramic specimens, smaller L* coordinates were obtained for greater a* and b* coordinates, indicating that the greater the number of firings, the darker and more reddish/yellowish the specimen. All Delta E values, for all groups, were below 1.0. All-ceramic specimens submitted to 3 and 4 firings presented Delta E means differing statistically (P<.05) from those of the metal ceramic group. Conclusions. The type of substrate and number of firings affected the color stability of the ceramic material tested. Artificial accelerated aging did not produce perceptible color stability changes (Delta E<1.0). (J Prosthet Dent 2009-101:13-18)

Evaluation of thermal compatibility between core and veneer dental ceramics using shear bond strength test and contact angle measurement

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Y-TZP ceramic processing from coprecipitated powders: A comparative study with three commercial dental ceramics

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Mechanical strength and subcritical crack growth under wet cyclic loading of glass-infiltrated dental ceramics

Objectives. Evaluate the flexural strength (sigma) and subcritical crack growth (SCG) under cyclic loading of glass-infiltrated alumina-based (IA, In-Ceram Alumina) and zirconia-reinforced (IZ, In-Ceram Zirconia) ceramics, testing the hypothesis that wet environment influences the SCG of both ceramics when submitted to cyclic loading.Methods. Bar-shaped specimens of IA (n = 45) and IZ ( n = 45) were fabricated and loaded in three-point bending (3P) in 37 degrees C artificial saliva (IA(3P) and IZ(3P)) and cyclic fatigued (F) in dry (D) and wet (W) conditions (IA(FD), IA(FW), IZ(FD), IZ(FW)). The initial sigma and the number of cycles to fracture were obtained from 3P and F tests, respectively. Data was examined using Weibull statistics. The SCG behavior was described in terms of crack velocity as a function of maximum stress intensity factor (K(Imax)).Results. The Weibull moduli (m = 8) were similar for both ceramics. The characteristic strength (sigma(0)) of IA and IZ was and 466 MPa 550 MPa, respectively. The wet environment significantly increased the SCG of IZ, whereas a less evident effect was observed for IA. In general, both ceramics were prone to SCG, with crack propagation occurring at K(I) as low as 43-48% of their critical K(I). The highest sigma of IZ should lead to longer lifetimes for similar loading conditions.Significance. Water combined with cyclic loading causes pronounced SCG in IZ and IA materials. The lifetime of dental restorations based on these ceramics is expected to increase by reducing their direct exposure to wet conditions and/or by using high content zirconia ceramics with higher strength. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The effect of carbamide peroxide bleaching agents on the microhardness of dental ceramics.

This study examined the effect of 10% and 16% carbamide peroxide bleaching agents on the surface microhardness of micro-particulate feldspathic ceramics (VM7 and VM13, Vita Zahnfabrik). Forty specimens (8-mm diameter, 2-mm thickness) were divided into four groups (n=10): GI-VM7 + 10% Whiteness, G2-VM7 + 16% Whiteness, G3-VM13 + 10% and G4-VM13 + 16% Whiteness. The home-use bleaching agents were applied for 8 hours on 15 days, and the specimens were stored in distilled water at 37 degrees C. The Vickers hardness number (HV) was determined for each specimen. Data were analyzed by the Wilcoxon and Mann-Whitney tests (p < 0.05). The microhardness values before exposure were: g1-433 (57); g2-486 (22); g3-509 (28); g4-518 (24), and after exposure: G1-349 (32); G2-496 (95); G3-519 (38); G4-502 (81). G2 exhibited a higher and significant difference than GI in VM7 groups, and the effect of bleaching concentration was shown to be significant by the Mann-Whitney test. And for VM13, both the Wilcoxon and Mann-Whitney tests showed no significant differences. When using 10% carbamide peroxide, the microhardness of VM7 ceramic was affected, and there were no effect on the microhardness between VM7 and VM13 ceramics when 16% carbamide peroxide was used.

Effect of bleaching agent on dental ceramics roughness.

The aim of this study was to assess the effect of bleaching agents (10% and 16% carbamide peroxide) on the roughness of two dental ceramics in vitro, and to analyze the surface by scanning electronic microscopy (SEM). Two bleaching agents (10% and 16%/Whiteness, FGM Gel) and two microparticle feldspathic ceramics (Vita VM7 and Vita VM13) were used. Forty disks of Vita VM7 and Vita VM13 ceramic were manufactured, measuring 4 mm in diameter and 4 mm high, in accordance with the manufacturers' recommendations, and were divided into 4 groups (n = 10): (1) VM7 + Whiteness 10%; (2) VM7 + Whiteness 16%; (3) VM13 + Whiteness 10%; (4) VM13 + Whiteness 16%. The bleaching agent was applied for 8 hours a day for 15 days and during the intervals the test specimens were stored in distilled water at 37 degrees C. The roughness (Ra) of the test specimens was evaluated before and after exposure to the bleaching agents using a laser roughness meter and the topographic description was analyzed by SEM. The statistical analysis of roughness data showed significant differences in the VM7 groups, using paired t-test, p = 0.05 (VM7 + Whiteness 10%: p = 0.002; VM7 + Whiteness 16%: p = 0.001) and two-sample t-test (VM7 p = 0.047), and no significant difference was found among VM13 groups. The qualitative SEM analysis showed different degrees of surface changes. The results suggest that the roughness of the tested ceramic surfaces increased after exposure to the bleaching agents.

Effect of brushing with conventional versus whitening dentifrices on surface roughness and biofilm formation of dental ceramics

The aim of this study was to evaluate the effect of conventional and whitening dentifrices on the weight loss, surface roughness, and early in situ biofilm formation on the surface of dental ceramics. Standardized feldspar ceramic specimens (Vita VM7 and Vita VM13) were submitted to the following experimental conditions: no brushing; brushing without a dentifrice; brushing with a conventional dentifrice; and brushing with a whitening dentifrice. A brushing machine was used to simulate brushing. The mass and surface roughness of all specimens from the test groups were evaluated prior to and after brushing. Ten participants used an oral device for eight hours to evaluate the biofilm formed in situ on the specimens. Scanning electron microscopy was used for qualitative and quantitative analysis of the biofilm. ANOVA and Tukey tests were used to analyze the results of weight loss, surface roughness, and presence of bacteria. A one-way Kruskal-Wallis test was used for bacterial colonization results. For both ceramics, brushing with a whitening dentifrice resulted in weight loss that was significantly greater when compared to brushing without a dentifrice or with a conventional dentifrice. Increased surface roughness was noticed on VM13 ceramic samples with both dentifrices, whereas only conventional dentifrice had a significant effect on the surface roughness of VM7 samples. For both VM7 and VM13, no difference was found between the experimental conditions with regard to the presence or number of bacteria. Cocci and short rods were the predominant microbial morphotypes. Granular or fibrillar acellular material partially covered the specimens. Brushing with a whitening dentifrice resulted in significant weight loss of ceramic restorations, while brushing with both conventional and whitening dentifrices can roughen ceramic surfaces. The increase in roughness was not clinically significant to contribute to increased biofilm formation.

Influence of polishing procedures on the surface roughness of dental ceramics made by different techniques

The aim of this study was to evaluate the influence of 2 different surface polishing procedures - glazing (GZ) and manual polishing (MP) - on the roughness of ceramics processed by computer-aided design/computer-aided manufacturing (CAD/CAM) and conventional systems (stratification technique). Eighty ceramic discs (diameter: 8 mm, thickness: 1 mm) were prepared and divided among 8 groups (n = 10) according to the type of ceramic disc and polishing method: 4 GZ and 4 MP. Specimens were glazed according to each manufacturer's recommendations. Two silicone polishing points were used on the ceramic surface for manual polishing. Roughness was measured using a surface roughness tester. The roughness measurements were made along a distance of 2 mm on the sample surface and the speed of reading was 0.1 mm/s. Three measurements were taken for each sample. The data (μm) were statistically analyzed using analysis of variance (ANOVA) and Tukey's test (α = 0.05). Qualitative analysis was performed using scanning electron microscopy (SEM). The mean (± SD) roughness values obtained for GZ were: 1.1 ± 0.40 μm; 1.0 ± 0.31 μm; 1.6 ± 0.31 μm; and 2.2 ± 0.73 μm. For MP, the mean values were: 0.66 ± 0.13 μm; 0.43 ± 0.14 μm; 1.6 ± 0.55 μm; and 2.0 ± 0.63 μm. The mean roughness values were significantly affected by the ceramic type (P = 0.0001) and polishing technique (P = 0.0047). The SEM images confirmed the roughness data. The manually polished glass CAD/CAM ceramics promoted lower surface roughness than did the glazed feldspathic dental ceramics.

Quantitative phase analysis from X-ray diffraction in Y-TZP dental ceramics: A critical evaluation

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Surface roughness analysis of dental ceramics treated with hydrofl uoric acid and aluminum oxide jet

The aim of this study was to evaluate the surface roughness of 5 indirect restorative materials treated with hydrofluoric acid to 10%, with aluminum oxide jet and a combination of both. The specimens was prepared with 10 mm in diameter and 2 mm thickness, divided into fi ve groups: (1) Ceromer (CeseadII-Kuraray), (2) Leucite crystals ceramics (IPS EmpressIIIvoclarforcasket), (3) glass ceramic with fluorapatite (IPS D. Sign-Ivoclar), (4) lithium disilicate ceramic (IPS Empress II-Ivoclar restorations), (5) ceramics (Cergogold-Degussa). For all groups were performed the controls, and the surfaces with the 3 types of treatment. For testing roughness used the rugosimeter Taylor/Hobson-Precision, model form tracerSV-C525 high sensitivity. After confi rmation of variance analysis with a signifi cance level of 1% (p < 0.01), there was equality between the average roughness of materials from groups 1, 3 and 5, and the group 2 was different from the others. It was also found that the ceramics of the group 5 behaved similar to group 4. However the lowest average roughness was observed in group 2 ceramic. In the evaluation between the types of treatment, the aluminum oxide jet and associations and blasting with hydrofl uoric acid were similar, and different isolated hydrofl uoric acid, and 3 types of treatment signifi cantly higher than the control group. All treatments promoted superfi cial alterations in all tested materials.

Relationship between elastic and mechanical properties of dental ceramics and their index of brittleness

The purpose of the study was to verify the effects of a number of materials' parameters (crystalline content; Young's modulus, E; biaxial flexure strength, sigma(i); Vickers hardness, VH; fracture toughness, K-Ic; fracture surface energy, gamma(f); and index of brittleness, B) on the brittleness of dental ceramics. Five commercial dental ceramics with different contents of glass phase and crystalline particles were studied: a vitreous porcelain (VM7/V), a porcelain with 16 vol% leucite particles (d.Sign/D), a glass-ceramic with 29 vol% leucite particles (Empress/E1), a glass-ceramic with 58 vol% lithium-disilicate needle-like particles (Empress 2/E2), and a glass-infiltrated alumina composite with 65 vol% crystals (In-Ceram Alumina/IC). Discs were constructed according to manufacturers' instructions, ground and polished to final dimensions (12 mm x 1.1 mm). Elastic constants were determined by ultrasonic pulse-echo method. sigma(i) was determined by piston-on-3-balls method in inert condition. VH was determined using 19.6 N load and K-Ic was determined by indentation strength method. gamma(f) was calculated from the Griffith-Irwin relation and B by the ratio of HV to K-Ic. IC and E2 showed higher values of sigma(i), E, K-Ic and gamma(f), and lower values of B compared to leucite-based glass-ceramic and porcelains. Positive correlations were observed for sigma(i) versus K-Ic, and K-Ic versus E-1/2, however, E did not show relationship with HV and B. The increase of crystalline phase content is beneficial to decrease the brittleness of dental ceramics by means of both an increase in fracture surface energy and a lowering in index of brittleness. (C) 2012 Elsevier Ltd and Techna Group Sri. All rights reserved.

Evaluation of interface characterization and adhesion of glass ceramics to commercially pure titanium and gold alloy after thermal- and mechanical-loading

Objectives. This study evaluated the effect of thermal- and mechanical-cycling on the shear bond strength of three low-fusing glassy matrix dental ceramics to commercial pure titanium (cpTi) when compared to conventional feldspathic ceramic fused to gold alloy.Methods. Metallic frameworks (diameter: 5 min, thickness: 4 mm) (N = 96, n = 12 per group) were cast in cpTi and gold alloy, airborne particle abraded with 150 mu m aluminum oxide. Low-fusing glassy matrix ceramics and a conventional feldspathic ceramic were fired onto the alloys (thickness: 4mm). Four experimental groups were formed; Gr1 (control group): Vita Omega 900-Au-Pd alloy; Gr2: Ticeram-cpTi; Gr3: Super Porcelain Ti-22-cpTi and G4: Vita Titankeramik-cpTi. While half of the specimens from each ceramic-metal combination were randomly tested without aging (water storage at 37 C for 24h only), the other half were first thermocycled (6000 cycles, between 5 and 55 C, dwell time: 13 s) and then mechanically loaded (20,000 cycles under SON load, immersion in distilled water at 37 C). The ceramic-alloy interfaces were loaded under shear in a universal test machine (cross-head speed: 0.5 mm/min) until failure occur-red. Failure types were noted and the interfaces of the representative fractured specimens from each group were examined with stereo microscope and scanning electron microscope (SEM). in an additional study (N = 16, n = 2 per group), energy dispersive X-ray spectroscopy (EDS) analysis was performed from ceramic-alloy interfaces. Data were analyzed using ANOVA and Tukey's test.Results. Both ceramic-metal combinations (p < 0.001) and aging conditions (p < 0,001) significantly affected the mean bond strength values. Thermal- and mechanical-cycling decreased the bond strength (MPa) results significantly for Gr3 (33.4 +/- 4.2) and Gr4 (32.1 +/- 4.8) when compared to the non-aged groups (42.9 +/- 8.9, 42.4 +/- 5.2, respectively). Gr1 was not affected significantly from aging conditions (61.3 +/- 8.4 for control, 60.7 +/- 13.7 after aging) (p > 0.05). Stereomicroscope images showed exclusively adhesive failure types at the opaque ceramic-cpTi interfacial zone with no presence of ceramic on the substrate surface but with a visible dark titanium oxide layer in Groups 2-4 except Gr1 where remnants of bonder ceramic was visible. EDS analysis from the interfacial zone for cpTi-ceramic groups showed predominantly 34.5-85.1% O(2) followed by 1.1-36.7% Aland 0-36.3% Si except for Super Porcelain Ti-22 where a small quantity of Ba (1.4-8.3%), S (0.7%) and Sn (35.3%) was found. In the Au-Pd alloy-ceramic interface, 56.4-69.9% O(2) followed by 15.6-26.2% Si, 3.9-10.9% K, 2.8-6% Na, 4.4-9.6% Al and 0-0.04% Mg was observed.Significance. After thermal-cycling for 6000 times and mechanical-cycling for 20,000 times, Triceram-cpTi combination presented the least decrease among other ceramic-alloy combinations when compared to the mean bond strength results with Au-Pd alloy-Vita Omega 900 combination. (c) 2008 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.