Effect of calcination on minimally processed recycled zirconia powder derived from milling waste.

OBJECTIVE: To assess the influence of calcination process on the properties of minimally processed recycled 3Y-TZP, and to compare it with its commercial counterpart. METHODS: Non-milled 3Y-TZP waste was collected, fragmented and ball-milled to a granulometric < 5 µm. Half of the recycled powder was calcined at 900 °C. Recycled 3Y-TZP disks were uniaxially pressed and sintered to create two recycled groups: 1) Calcined and 2) Non-calcined to be compared with a commercial CAD/CAM milled 3Y-TZP. The microstructure of experimental groups was assessed through density (n = 6), scanning electron microscopy (n = 3) and energy-dispersive X-ray spectroscopy (n = 3); and the crystalline content was evaluated through X-ray diffraction (XRD) (n = 3). Optical and mechanical properties were investigated through reflectance tests (n = 10), and Vickers hardness, fracture toughness (n = 5), and biaxial flexural strength tests (n = 16), respectively. Fractographic analysis was performed to identify fracture origin and crack propagation. Statistical analyses were performed through ANOVA followed by Tukey´s test, and by Weibull statistics. RESULTS: Particle size distribution of recycled powder revealed an average diameter of ∼1.60 µm. The relative density of all experimental groups was > 98.15 % and XRD analysis exhibited a predominance of tetragonal-phase in both recycled groups, which were similar to the crystallographic pattern of the control group. Cross-section micrographs presented flaws on the non-calcined group, and a more homogeneous microstructure for the calcined and commercial groups. Commercial samples showed lower contrast-ratio and higher translucency-parameter than the recycled groups, where non-calcined presented higher translucency-parameter and lower contrast-ratio than its calcined counterpart. The commercial group presented higher fracture toughness and characteristic strength than the recycled groups. Moreover, the calcined group exhibited higher hardness, characteristic strength, and probability of survival at higher loads than the non-calcined group. Fractographic analysis depicted the presence of microstructural flaws in the non-calcined group, which may have acted as stress-raisers and led to failures at lower flexural strengths values. SIGNIFICANCE: The calcination process improved the microstructure, optical, and mechanical properties of the recycled 3Y-TZP.

Influence of straight versus angulated screw channel titanium bases on failure loads of two-piece ceramic and titanium implants restored with screw-retained monolithic crowns: An in-vitro study.

OBJECTIVE: To analyze the influence of titanium-base (straight [SSC]/angulated-screw-channel [ASC]) on failure-loads and bending-moments of two-piece ceramic and titanium-zirconium implants restored with monolithic-zirconia crowns after fatigue. MATERIALS AND METHODS: Thirty-two anterior monolithic-screw-retained zirconia crowns were divided into four groups (n = 8/group) according to the factors: (1) type of implant material: two-piece titanium-zirconium implant (Ti-Zr; control-group) versus two-piece ceramic implant (CI; test-group) and (2) type of titanium-base: SSC (0° angle) versus ASC (25°). An intact implant was used for field emission gun-scanning electronic microscopy (FEG-SEM) characterization and Raman spectroscopy for phase analyses and residual stress quantification. All samples were exposed to fatigue with thermodynamic loading (1.2-million-cycles, 49 N, 1.6 Hz, 5-55°C) at a 30° angle. Surviving specimens were loaded until failure (SLF) and bending moments were recorded. Failed samples were examined using light microscope and SEM. Statistical analyses included ANOVA and Mann-Whitney U-test. RESULTS: Raman-spectroscopy revealed the presence of residual compressive stresses. FEG-SEM revealed a roughened surface between threads and polished surface at the cervical-collar of the ceramic implant. All samples survived fatigue and were free of complications. Mean bending-moments (±SD) were: Ti-Zr-0: 241 ± 45 N cm, Ti-Zr-25: 303 ± 86 N cm, CI-0: 326 ± 58 N cm, CI-25: 434 ± 71 N cm. Titanium-base and implant-material had significant effects in favor of ASC titanium bases (p = .001) and ceramic-implants (p < .001). Failure analysis after SLF revealed severe fractures in ceramic implants, whereas titanium implants were restricted to plastic deformation. CONCLUSIONS: Ceramic and titanium implants exhibited high reliability after fatigue, with no failures. From a mechanical perspective, titanium bases with ASC can be recommended for both ceramic and titanium implants and are safe for clinical application.

Infiltration OF 5Y-PSZ with thermally compatible glass: Strength, microstructure and failure mode analyses.

This study set out to develop a thermally compatible glass to be infiltrated into zirconia partially stabilized by yttrium oxide (5Y-PSZ), to characterize it, and to evaluate its structural reliability and mechanical behavior. 5Y-PSZ zirconia discs (N = 90), dimensions 1.5 mm × 15 mm were produced, polished with #600 alumina oxide and #1200 silicon carbide sandpaper in a polisher. Three groups of 5Y-PSZ discs were assigned (n = 30): Zctrl: as sintered zirconia, Zinf-comp: glass-infiltrated zirconia on the occlusal surface, and sintered, and Zinf-tens: glass-infiltrated zirconia on the cementing surface and sintered; for biaxial flexural strength testing (ISO 6872:2015). A gel was synthesized via the sol-gel method and applied to the ceramic surface. Mechanical assay data (MPa) were evaluated via Weibull analysis (α = 5%) and specimens via X-Ray Diffractometry (XRD), Scanning Electron Microscopy (SEM), and fractographic analysis. The Zinf-tens group showed a characteristic strength of 824 MPa and m = 9.9; Zinf-comp 613 MPa and m = 10.2; Zctrl 534 MPa and m = 8; all groups differed statistically (σ0). However, they were similar in structural homogeneity (m). XRD showed 20-50 µm of infiltration, which means dissolution of part of the yttrium and reduction in the size of the cubic grains. In addition, the Zinf-tens group presented a failure origin from inside the material. The developed glass infiltrated into zirconia partially stabilized by yttrium oxide, increasing its characteristic strength and structural homogeneity by reducing surface defects and changing the failure mode.

Water as Veneering Modeling Liquid Affects Microhardness of Glassy Matrix Veneering Ceramic.

PURPOSE/AIM: To evaluate the effect of different veneering liquids used for modeling on microhardness, fracture toughness and biaxial flexural strength of a glass-veneering ceramic. MATERIAL AND METHODS: The manufacturer recommended modeling liquid (ML), distilled water (DW), isopropyl alcohol (IA), 0.5% (P05), 1% (P1), and 2% (P2) polyethylene glycol solutions were mixed with feldspathic ceramic powder to form disc-shaped samples (n=20, 15 mm × 1.2 mm). After sintering, samples were mirror-polished and subjected to Vickers indentation (n=5) for measurement of microhardness and fracture toughness. The remaining 15 samples from each group were subjected to biaxial flexural strength. Data were subjected to one-way ANOVA and Weibull analysis. RESULTS: The microhardness was affected by veneering liquid (p=0.002): DW promoted higher microhardness values than ML and IA. Fracture toughness (p=0.301) and flexural strength (p=0.930) were not affected by the veneering liquid but Weibull parameters were affected. All groups presented surface pores under high magnification. CONCLUSION: Even though the use of DW led to higher values of surface microhardness than the ML, all obtained values are inside the range of enamel microhardness values reported in the literature. Such parameters may affect antagonist wear and should be reported in clinical trials.

Incorporation of 45S5 bioglass via sol-gel in ß-TCP scaffolds: Bioactivity and antimicrobial activity evaluation.

In this work, ß-TCP (ß-tricalcium phosphate) bioresorbable scaffolds were prepared by the gel casting method. Then, they were impregnated with a 45S5 bioglass sol gel solution to improve biocompatibility and promote bioactivity and antimicrobial activity. The ß-TCP scaffolds had an apparent porosity of 72%, and after the incorporation of the bioglass, this porosity was maintained. The elements of the bioglass were incorporated into ß-TCP matrix and there was a partial transformation from the ß-TCP phase to the α-TCP (α-tricalcium phosphate) phase, besides the formation of bioactive calcium and sodium­calcium silicates. The scaffolds ß-TCP with 45S5 bioglass incorporated (ß-TCP/45S5) did not show a reduction in their values of mechanical strength and Weibull modulus, despite the partial transformation to the α-TCP phase. Bioactivity, cell viability, and antimicrobial activity improved significantly for the ß-TCP/45S5 scaffold comparing to the scaffold without the bioglass. The mineralization of carbonated hydroxyapatite was verified in Simulated Body Fluid (SBF). The cell viability, evaluated by the reduction of 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazolium bromide - MTT in MG63 cells, increased by 178%, and ß-TCP/45S5 scaffold also enhanced cell activity and osteoblast differentiation observed by means of total protein contend and alkaline phosphatase activity, respectively. The formation of growth inhibition zones was also observed in the disk diffusion assay for three tested microorganisms: Staphylococcus aureus, Escherichia coli and Candida albicans. To conclude, the vacuum impregnation method in 45S5 bioglass sol gel solution was effective in penetrating all the interconnected macroporosity of the scaffolds and covering the surface of the struts, which improved their biological properties in vitro, bioactivity and antibacterial activity, without reducing mechanical strength and porosity values. Thus, the ß-TCP/45S5 scaffolds are shown as potential candidates for use in tissue engineering, mainly in bone tissue regeneration and recovery.

Nanoscale physico-mechanical properties of an aging resistant ZTA composite.

OBJECTIVE: To characterize the effects of aging on the nanomechanical properties and 3D surface topographical parameters of an experimental Zirconia Toughened Alumina (ZTA) composite compared to its respective individual counterpart materials. METHODS: Disk-shaped specimens comprised of three material groups were processed: 1) ZTA 70/30 (70% alumina reinforced with 30% second-generation 3Y-TZP); 2) Zpex (Second-generation 3Y-TZP), and; 3) Al2O3 (High purity Alumina) (n = 10/material, 12 × 1 mm). After synthesis, ceramic powders were pressed, the green-body samples were sintered and polished. Nanoindentation testing was performed to record elastic modulus (E) and hardness (H). Interferometry was utilized to assess 3D surface roughness parameters (Sa, Sq), while X-ray diffraction (XRD) and scanning electron microscope (SEM) assessed the crystalline content and microstructure. All tests were performed before and after simulated aging (134°C, 2.2 bar, 20 h). Statistical analyses were performed using linear mixed-model and least square difference pos-hoc tests (α = 5%). RESULTS: XRD spectra indicated increase of monoclinic peaks for Zpex (~18%) relative to ZTA 70/30 (~2.5%) after aging. Additionally, aging did not affect the surface roughness parameters of ZTA 70/30 and Al2O3, although a significant increase in Sa was recorded for Zpex following aging (~90 nm) (p < 0.001). Al2O3 yielded the highest H and E values (H:21 GPa, E: 254 GPa), followed by ZTA 70/30 (H: 13 GPa, E: 214 GPa) and Zpex (H:11 GPa, E: 167 GPa), all significantly different (p < 0.03). CONCLUSION: ZTA 70/30 and Al2O3 presented high hydrothermal stability with respect to all evaluated variables, where artificial aging significantly increased the monoclinic content and surface roughness of Zpex.

Failure probability and stress distribution of milled porcelain-zirconia crowns with bioinspired/traditional design and graded interface.

OBJECTIVE: To evaluate the failure probability and stress distribution of traditional and bioinspired porcelain-zirconia milled crowns, with and without silica infiltration (graded zirconia). METHODS: Traditional crown design had a zirconia infrastructure veneered with porcelain; Bioinspired, had a porcelain infrastructure with translucent-zirconia veneer; Graded and Graded Bioinspired crowns had their zirconia layer infiltrated by silica (n = 25). The cameo surface of each crown (porcelain or zirconia) was glazed. The restoration layers were fused by a vitreous connector and the crowns were adhesively cemented to dies. The specimens were then mechanically cycled in a sliding machine using 100 N load at 4 Hz. The specimens were tested until 2 × 106 cycles, and every 0.5 × 106 cycles the crowns were evaluated under stereomicroscopy for the presence of failures. The stress distribution was inspected with Finite Element Analyses. RESULTS: The predominant failure modes for the Traditional and Graded crowns were delamination and cracking, respectively. The Weibull parameters beta and eta were, respectively: Traditional 1.30 and 2.3 × 106 cycles, and Graded 1.95 and 2.3 × 106 cycles. Thus, the Traditional and Graded crowns presented greater susceptibility to failure due to fatigue, while the Bioinspired and Graded Bioinspired crowns showed no fatigue effect using 100N load, showing beta = 1 and eta of approximately 17 × 106 cycles. Also, through finite element analyses, it was verified that the Bioinspired and Graded Bioinspired crowns presented the best stress distribution on both crowns and dental structures. SIGNIFICANCE: Bioinspired and Graded Bioinspired crowns had the lowest failure probability and better stress distribution and may be considered robust long lasting restorations.

Microstructural, mechanical, and optical characterization of an experimental aging-resistant zirconia-toughened alumina (ZTA) composite.

OBJECTIVE: To evaluate the effect of aging on the microstructural, mechanical, and optical properties of an experimental zirconia-toughened alumina composite with 80%Al2O3 and 20%ZrO2 (ZTA Zpex) compared to a translucent zirconia (Zpex) and Alumina. METHODS: Disc-shaped specimens were obtained by uniaxial and isostatic pressing the synthesized powders (n = 70/material). After sintering and polishing, half of the specimens underwent aging (20 h, 134 °C, 2.2 bar). Crystalline content and microstructure were evaluated using X-ray diffraction and scanning electron microscopy, respectively. Specimens underwent biaxial flexural strength testing to determine the characteristic stress, Weibull modulus, and reliability. Translucency parameter (TP) and Contrast ratio (CR) were calculated to characterize optical properties. RESULTS: ZTA Zpex demonstrated a compact surface with a uniform dispersion of zirconia particles within the alumina matrix, and typical alumina and zirconia crystalline content. ZTA Zpex and alumina exhibited higher CR and lower TP than Zpex. ZTA Zpex and Zpex showed significantly higher characteristic stress relative to alumina. While aging did not affect optical and mechanical properties of ZTA Zpex and alumina, Zpex demonstrated a significant increase in translucency, as well as a in characteristic stress. Alumina reliability was significantly lower than others at 300 MPa, ZTA Zpex and Zpex reliability decreased at 800 MPa, except for aged Zpex. SIGNIFICANCE: While aging did not affect the mechanical nor the optical properties of ZTA Zpex and alumina, it did alter both properties of Zpex. The results encourage further investigations to engineer ZTA as a framework material for long span fixed dental prostheses specially where darkened substrates, such as titanium implant abutments or endodontically treated teeth, demand masking.

Silica infiltration in partially stabilized zirconia: Effect of hydrothermal aging on mechanical properties.

It aimed to evaluate if silica infiltration might influence the hydrothermal degradation of zirconia by determining: the phases formed, hardness, microstructure, and flexural strength of a 3Y-TZP. Yttria partially stabilized zirconia discs (1.2 mm thickness x 13 mm diameter) (InCeram YZ, Vita Zanhfabrik) were produced and assigned into 6 groups, considering 2 factors: silica infiltration in 2 levels (as-sintered or infiltration) and hydrothermal aging (LTD-Low Temperature Degradation) in 3 levels (baseline, aging at 132 °C for 35 h or 140 h). All the groups were subjected to the biaxial flexural test (n = 30), and Vickers hardness (n = 42). Weibull analysis was performed to determine the Weibull moduli (m) and characteristic strenghts (σ0). The specimens were characterized by scanning electron microscopy (SEM) to evaluate microstructure and X-ray diffraction (XRD) for phases percentages determination. For as-sintered condition: there was saturation of the amount of monoclinic zirconia after 35 h of hydrothermal aging, with 66% of monoclinic zirconia formed on the surface. LTD generated a progressive reduction in hardness over time; flexural strength was increased by the 35-h treatment (baseline: 974 MPa; 35 h: 1161.5 MPa), but, the 140 °C treatment was deleterious (698.5 MPa). On the other hand, the infiltrated specimens had an increase in the amount of cubic zirconia on the surface and showed 26% (35h) and 31% (140h) of monoclinic zirconia after the hydrothermal aging ; the strength was kept unaltered after LTD-35 h (935.9 MPa) and an increase was observed after LTD-140 h (1033.6 MPa); the hardness values had no statistically significant changes during the process. Thus, one can concludes that the silica infiltration can prevent the decrease in the mechanical properties due to the LTD on partially stabilized zirconia materials.

Silica-Based Infiltrations for Enhanced Zirconia-Resin Interface Toughness.

Novel silica-based infiltrations on the surface of zirconia have the potential to improve their bondability, allowing for the etching/silane adhesive bonding technique. Nonetheless, adhesively bonded joints are subject to mixed tensile and shear stresses when the restoration is in occlusal service. Thus, we aimed to investigate the effect of 2 novel silica-based infiltrations on the interfacial toughness of adhesively bonded zirconia using the Brazil nut method, which allows for controlled types of stresses to be applied at the interfaces. In total, 150 3Y-TZP (In-Ceram YZ; Vita) Brazil nuts were machined and randomly assigned to 3 groups: C, control (air abraded); SG, sol-gel silica infiltration; and GI, glass infiltration. SG specimens were immersed twice in silicic acid for 20 min and dried (100°C, 1 h). GI specimens were presintered (1,400°C, 1 h) before a glass powder slurry was applied to the intaglio surface. All specimens were then sintered (1,530°C, 2 h). Following adhesive bonding (Panavia F 2.0, Kuraray) and water storage (37°C) for 10 d, the Brazil nuts were subdivided into groups baseline and aged (40,000 thermal cycles between 5°C and 55°C, with a dwell time of 30 s). The Brazil nuts were subjected to axial-loading tests using various inclinations (precrack angle with load direction): Θ = 0°, 5°, 10°, 15°, or 25°, which define the stress type at the interface, from pure tension (0°) to increasing levels of shear. Under pure tension (0°), GI yielded superior interfacial fracture energy, SG and C were similar, and aging had no effect. Under predominantly shear stresses (25°), aging significantly decreased interfacial fracture energy of C and SG, while GI remained stable and was superior. The glass infiltration of the zirconia intaglio surface increases its adhesive bonding interfacial toughness. The sol-gel silica infiltration method requires improvement to obtain a homogeneous surface infiltration and an enhanced bond strength.

A new silica-infiltrated Y-TZP obtained by the sol-gel method.

OBJECTIVE: The aim of this study was to evaluate silica infiltration into dental zirconia (VITA In-Ceram 2000 YZ, Vita Zahnfabrik) and its effects on zirconia's surface characteristics, structural homogeneity and bonding to a resin cement. METHODS: Infiltration was performed by immersion of the pre-sintered zirconia specimens in silica sols for five days (ZIn). Negative (pure zirconia specimens, ZCon-) and positive controls (specimens kept in water for 5 days, ZCon+) were also performed. After sintering, the groups were evaluated by X-ray diffraction (XRD), grazing angle X-ray diffraction (DRXR), scanning electron microscopy (SEM), contact angle measurements, optical profilometry, biaxial flexural test and shear bonding test. Weibull analysis was used to determine the Weibull modulus (m) and characteristic strength (σ0) of all groups. RESULTS: There were no major changes in strength for the infiltrated group, and homogeneity (m) was also increased. A layer of ZrSiO4 was formed on the surface. The bond strength to resin cement was improved after zirconia infiltration, acid conditioning and the use of an MDP primer. CONCLUSION: The sol-gel method is an efficient and simple method to increase the homogeneity of zirconia. Infiltration also improved bonding to resin cement. CLINICAL SIGNIFICANCE: The performance of a zirconia infiltrated by silica gel improved in at least two ways: structural homogeneity and bonding to resin cement. The infiltration is simple to perform and can be easily managed in a prosthesis laboratory.

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

UNLABELLED: The dentistry literature shows consensus to use the Garvie and Nicholson equation modified by Toraya to quantify the Y-TZP phase transformation. However, this method does not include the possibility of cubic phase transformation and crystallographic texture after artificial ageing, and in this case, it is possible to observe errors of quantification. OBJECTIVES: The aim of this study was to evaluate a dental Y-TZP ageing kinetic of phase transformation under pressure and hydrothermal conditions (130°C, 2bar) and to compare the methods of quantification by the equation of Garvie and Nicholson modified by Toraya and the Rietveld refinement method. METHODS: Discs of Y-TZP (12mm Ø×1.2mm in height) were divided into groups (n=4) according to the ageing times (in the range of 6 and 138h). The superficial characterisation was made using SEM and the XDR for crystallographic analysis. RESULTS: An aggressive superficial degradation process at the beginning of phase transformation in 6-10h of ageing was observed by SEM. The phase transformation quantification showed differences between the methods. It was observed the increase and stabilisation of monoclinic phase until 80% at 40h of ageing by the Garvie and Nicholson modified by Toraya equation, compared to 60% of monoclinic phase and approximately 30% of cubic phase observed by the Rietveld method. CONCLUSION: The Toraya equation showed an overestimated result of monoclinic quantification compared to the Rietveld method. CLINICAL SIGNIFICANCE: The overestimated result of monoclinic phase could lead to different interpretation about the dental Y-TZP ageing process.