Characterization of a hydrothermally aged experimental alumina-toughened zirconia composite.

OBJECTIVES: To assess the effects of different aging protocols on chemical, physical, and mechanical properties of an experimental ATZ composite compared to a zirconia. METHODS: Disc-shaped specimens were obtained through uniaxial pressing of commercial powders (Tosoh), ATZ comprised of 80%ZrO2/20%Al2O3 (TZ-3YS20AB) and 3Y-TZP (3Y-SBE). The specimens of each material were divided into different groups according to the aging protocol: immediate, autoclave aging and hydrothermal reactor aging. The aging protocols were performed at 134 ºC for 20 h at 2.2 bar. Crystalline evaluations were performed using X-Ray Diffraction. The nanoindentation tests measured the elastic modulus (Em) and hardness (H). Biaxial flexural strength was performed, and Weibull statistics were used to determine the characteristic strength and Weibull modulus. The probability of survival was also determined. The Em and H data were analyzed by one-way ANOVA and Tukey test. RESULTS: Diffractograms revealed the presence of monoclinic phase in both materials after aging. The hydrothermal reactor decreased the Em for ATZ compared to its immediate condition; and the H for both ATZ and 3Y-TZP regarding their immediate and autoclave aging conditions, respectively. The aging protocols significantly increased the characteristic strength for ATZ, while decreased for 3Y-TZP. No difference regarding Weibull modulus was observed, except for 3Y-TZP aged in reactor. For missions of up to 500 MPa, both materials presented a high probability of survival (>99 %) irrespective of aging condition. SIGNIFICANCE: The synthesized ATZ composite exhibited greater physical and microstructural stability compared to 3Y-TZP, supporting potential application of the experimental material for long-span reconstructive applications.

Development of ZTA (80% Al2O3/20% ZrO2) pre-sintered blocks for milling in CAD/CAM systems.

The present work aims to develop a production method of pre-sintered zirconia-toughened-alumina (ZTA) composite blocks for machining in a computer-aided design and computer-aided manufacturing (CAD-CAM) system. The ZTA composite comprised of 80% Al2O3 and 20% ZrO2 was synthesized, uniaxially and isostatically pressed to generate machinable CAD-CAM blocks. Fourteen green-body blocks were prepared and pre-sintered at 1000 °C. After cooling and holder gluing, a stereolithography (STL) file was designed and uploaded to manufacture disk-shaped specimens projected to comply with ISO 6872:2015. Seventy specimens were produced through machining of the blocks, samples were sintered at 1600 °C and two-sided polished. Half of the samples were subjected to accelerated autoclave hydrothermal aging (20h at 134 °C and 2.2 bar). Immediate and aged samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Optical and mechanical properties were assessed by reflectance tests and by biaxial flexural strength test, Vickers indentation and fracture toughness, respectively. Samples produced by machining presented high density and smooth surfaces at SEM evaluation with few microstructural defects. XRD evaluation depicted characteristic peaks of alpha alumina and tetragonal zirconia and autoclave aging had no effect on the crystalline spectra of the composite. Optical and mechanical evaluations demonstrated a high masking ability for the composite and a characteristic strength of 464 MPa and Weibull modulus of 17, with no significant alterations after aging. The milled composite exhibited a hardness of 17.61 GPa and fracture toughness of 5.63 MPa m1/2, which remained unaltered after aging. The synthesis of ZTA blocks for CAD-CAM was successful and allowed for the milling of disk-shaped specimens using the grinding method of the CAD-CAM system. ZTA composite properties were unaffected by hydrothermal autoclave aging and present a promising alternative for the manufacture of infrastructures of fixed dental prostheses.

Reliability and Failure Mode of Ti-Base Abutments Supported by Narrow/Wide Implant Systems.

To assess the reliability and failure modes of Ti-base abutments supported by narrow and wide-diameter implant systems. Narrow (Ø3.5 × 10 mm) and wide (Ø5 × 10 mm) implant systems of two different manufacturers with internal conical connections (16°) and their respective Ti-base abutments (3.5 and 4.5 mm) were evaluated. Ti-base abutments were torqued to the implants, standardized metallic maxillary incisor crowns were cemented, and step stress accelerated life testing of eighteen assemblies per group was performed in three loading profiles: mild, moderate, and aggressive until fracture or suspension. Reliability for missions of 100,000 cycles at 100 and 150 N was calculated, and fractographic analysis was performed. For missions at 100 N for 100,000 cycles, both narrow and wide implant systems exhibited a high probability of survival (≥99%, CI: 94-100%) without significant differences. At 150 N, wide-diameter implants presented higher reliability (≥99%, CI: 99-100%) compared to narrow implants (86%, CI: 61-95%), with no significant differences among manufacturers. Failure mode predominantly involved Ti-base abutment fractures at the abutment platform. Ti-base abutments supported by narrow and wide implant systems presented high reliability for physiologic masticatory forces, whereas for high load-bearing applications, wide-diameter implants presented increased reliability. Failures were confined to abutment fractures.

Alumina-toughened zirconia nanocomposite: Aging effect on microstructural, optical, and mechanical properties.

OBJECTIVES: To process an alumina-toughened zirconia (ATZ) nanocomposite and to characterize its crystalline phases, microstructure, residual stress, mechanical and optical properties before and after two different artificial aging methodologies. METHODS: Disc-shaped specimens were obtained through uniaxial pressing of a commercial ATZ powder comprised of 80%ZrO2 / 20%Al2O3, with a particle size of 50 nm and 150 nm, respectively. Sintering was performed at 1500ºC for 2 h. Groups were established according to the aging protocol as immediate (ATZ-I) and aged either in autoclave (ATZ-A) or hydrothermal reactor (ATZ-R) at 134 ºC for 20 h at 2.2 bar. Crystalline phases and microstructure were assessed by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. Residual stress was evaluated by Raman spectroscopy. Contrast Ratio (CR) and Translucency Parameter (TP) were calculated to characterize optical properties. Mechanical properties were analyzed through Vickers microhardness, fracture toughness, and biaxial flexural strength test. RESULTS: XRD spectra of both aging protocols revealed the presence of monoclinic zirconia (20-31%), where higher phase transformation was observed after aging in hydrothermal reactor. Optical properties evaluation demonstrated high opacity (CR: 0.99) and masking ability (TP: 0.26), with no significant differences after aging. Raman spectroscopy evidenced the presence of residual compressive stresses in the aged groups, being significantly higher for ATZ-R (-215.2 MPa). As-sintered specimens revealed hardness of ∼12.3 GPa and fracture toughness of ∼1.9 MPa.m1/2. Characteristic strength was 740 MPa for ATZ-I, 804 MPa for ATZ-A, and 879 MPa for ATZ-R, with significant differences between groups. Weibull modulus ranged from 16.5 to 18.8. All groups demonstrated high reliability up to 500 MPa stress missions (99-100%), with no significant differences after aging. SIGNIFICANCE: The experimental ATZ nanocomposite presented high opacity and a high Weibull modulus. While aging created internal compressive stress responsible for an increase in characteristic strength, the nanocomposite was susceptible to hydrothermal degradation. Further studies are required to evaluate its degradation kinetics at low temperatures.

Probability of survival and failure mode of endodontically treated incisors without ferrule restored with CAD/CAM fiber-reinforced composite (FRC) post-cores.

PURPOSE: This study evaluated the probability of survival and failure mode of endodontically treated incisors without ferrule restored with CAD/CAM FRC post-cores. METHODS: Root canals of bovine incisors were treated, leaving post preparations of ∼10 mm. Teeth were allocated into three groups: (i) cast metal post-core, (ii) FRC prefabricated post with a direct resin core build-up, and (iii) CAD/CAM FRC post-core. Posts and zirconia crowns were cemented using resin cement. Specimens were subjected to step-stress accelerated-life fatigue testing in water. Use level probability Weibull curves, probability of survival for a mission of 100,000 cycles at 25, 50, and 100 N, Weibull modulus, and characteristic strength were calculated and plotted. Failure mode was examined under a stereomicroscope. RESULTS: Restored incisors demonstrated high probability of survival (93-100%) for missions estimated at 25 and 50 N, irrespective of post-core foundation. At 100 N, incisors restored with metal posts presented significantly higher probability of survival (99%) relative to CAD/CAM posts (79%), whereas FRC groups demonstrated no significant difference. Weibull analysis indicated no significant difference on the Weibull modulus (m = 3.38-5.92). Incisors reconstructed with metal post-cores (431 N) presented significantly higher characteristic strength relative to prefabricated (200 N) and CAD/CAM (202 N) FRC post-cores. While post fracture was the chief failure mode for prefabricated and CAD/CAM FRC post-cores, post and/or root fracture were the main event for metal post-cores. CONCLUSION: Endodontically treated incisors without ferrule restored with CAD/CAM FRC post-cores presented promising probability of survival for loads compatible with anterior masticatory forces and favorable failure modes.

Temporary materials used in prosthodontics: The effect of composition, fabrication mode, and aging on mechanical properties.

PURPOSE: To evaluate the effect of composition, fabrication mode, and thermal cycling on the mechanical properties of different polymeric systems used for temporary dental prostheses. MATERIALS AND METHODS: Standard bar-shaped specimens (25 × 2 × 2 mm) were fabricated of six polymeric systems of varying compositions and fabrication modes (n = 10/group): conventional PMMA (Alike, GC) - group CGC; conventional PMMA (Dêncor, Clássico) - group CD; bis-acryl (Tempsmart, GC) - group BGC; bis-acryl (Yprov, Yller) - group BY; milled PMMA (TelioCAD, Ivoclar) - group MI; 3D printed bis-acryl - (Cosmos Temp, Yller) group PY. Half of the specimens were subjected to 5000 thermal cycles (5 °C to 55 °C). Three-point bending tests were performed using a universal testing machine with a crosshead speed set to 0.5 mm/min. Flexural strength and elastic modulus were calculated from the collected data. FTIR spectra were recorded pre and post curing and after thermal cycling to evaluate material composition and degree of conversion. Energy-dispersive spectroscopy (EDS) and scanning electron microscope (SEM) were utilized to examine the composition and micromorphology of the systems, respectively. Data were analyzed using two-analysis of variance and Tukey tests (α = 0.05). RESULTS: FTIR spectra indicated that BGC, BY and PY groups corresponded to urethane dimethacrylate systems (bis-acryl), while CGC, CD, and MI groups corresponded to monomethacrylate systems, polymethyl methacrylate (PMMA). Bis-acryl BGC system yeilded the highest flexural strength (80 MPa), followed by the milled PMMA MI system (71 MPa), both statistically significant different relative to other groups. Bis-acryl BY exhibited the lowest flexural strength (27 MPa). Thermocycling significantly increased the flexural strength of all polymeric systems (∼10-15 MPa), except for the 3D-printed PY group. Bis-acryl BGC (1.89 GPa) and conventional PMMA CGC (1.66 GPa) groups exhibited the highest elastic modulus, followed by milled PMMA MI group (1.51 GPa) and conventional PMMA CD (1.45 GPa) systems, with significant difference detected between BGC group and MI and CD groups. The 3D printed PY (0.78 GPa) and bis-acryl BY (0.47 GPa) systems presented the lowest elastic modulus. Thermocycling did not have a significant influence on the elastic modulus. FTIR spectra indicate water sorption and release of unreacted monomers as well as increased degree of conversion (∼5-12%) after thermal cycling. CONCLUSION: Composition and fabrication mode and thermal cycling significantly affected the mechanical properties of polymeric systems used for temporary dental prostheses.

Hydrothermal aging affects the three-dimensional fit and fatigue lifetime of zirconia abutments.

OBJECTIVE: Evaluate the effect of aging using two different methods on the three-dimensional fit of zirconia abutments at the implant-abutment connection and estimate the probability of survival of anterior crowns supported by straight and 17-degree angled abutments. MATERIALS AND METHODS: Two different zirconia abutment designs, straight and 17-degree angled abutments (n = 63/group), were evaluated in the current study. The abutments were randomly allocated into three experimental groups according to laboratory aging condition (134°C, 2.2 bar, 20 h): (i) control, (ii) autoclave aging, and (iii) hydrothermal reactor aging. Crystalline content was determined by X-Ray diffraction (XRD) and Raman spectroscopy, and microstructure was analyzed using field-emission gun scanning electron microscope (FEG-SEM). Implant-abutment volume misfit was determined in the straight abutments by micro-computed tomography using the silicone replica technique. For fatigue testing, abutments were torqued to the implants and connected to standardized maxillary incisor zirconia crowns. The assemblies were subjected to step-stress accelerated life testing (SSALT) in water until fracture or suspension. The use level probability Weibull curves and probability of survival for a mission of 50,000 cycles at 50, 100, 150 and 200 N were calculated and plotted. Fractured samples were analyzed using a stereomicroscope and scanning electron microscope. RESULTS: The crystalline spectra depicted a zirconia system primarily composed of the tetragonal phase. Laboratory aging yielded a 20%- and 37%-increase in the monoclinic content for abutments aged in autoclave and hydrothermal reactor relative to control, respectively. A fully crystalline matrix with a regular grain size was observed in the FEG-SEM for control abutments, with a considerable presence of intergranular defects. While autoclave aging triggered no significant alteration to the microstructure, defect population was reduced after hydrothermal reactor aging. Control abutments presented a significantly higher volume misfit (2.128 ± 0.54 mm3) relative to aged abutments using autoclave (1.244 ± 0.48 mm3) or hydrothermal reactor (1.441 ± 0.41 mm3). The beta (ß) values indicated that failures were predominantly controlled by material strength rather than fatigue damage accumulation for all groups, except for straight control abutments. Irrespective of aging, the probability of survival of straight and angled zirconia abutments was up to 95% (95-100%) at 50 and 100 N. A 50N-increase in the load resulted in wider range of survival estimate, with straight autoclave abutments percentage significantly lower probability of survival (77%) than angled hydrothermal reactor abutments (99%). At 200N, angled hydrothermal reactor (97%) or autoclave (82%) aged abutments demonstrated the highest probability of survival, angled control (71%) and straight hydrothermal reactor (69%) abutments intermediate values, and straight autoclave (23%) and control (7%) abutments the lowest estimate. The failure mode predominantly involved abutment and/or abutment screw fracture for both straight and angled abutments. CONCLUSIONS: Hydrothermal aging significantly influenced volume misfit, as well as the probability of survival of zirconia abutments at higher loads for both angled and straight abutments.