Sintering Of Zirconia Research Articles

Flash sintering of zirconia: Effect of field strength on the incubation stage before densification

The effect of field strength on the incubation time of flash treating dense ZrO2 ceramics was studied at various temperatures. The results showed that the incubation time was related to k/((E-Ec)2E), where E is the applied field strength, Ec is the critical field strength below which flash cannot occur, and k is a constant reversely related to the conductivity of ZrO2. Curve-fitting the experimental data showed that the activation energy related to Ec was ∼24 kJ/mol, similar to that for the formation of oxygen vacancy; meanwhile the activation energy related to k was ∼89 kJ/mol, close to that for the migration of oxygen vacancies. These results suggest that by applying an electric field with the strength above the critical value, the extra oxygen vacancies were injected into the sample by overcome the electrochemical potential and accumulated within the sample with time. The incubation time is the time required to accumulate sufficient oxygen vacancies for the power density reaching a critical value.

Simultaneous effect of microwave sintering and TiO2 addition on sinterability, mechanical properties, and scratch resistance of zirconia toughened alumina ceramics

This paper delves into the transformative impact of varying titanium dioxide (TiO2) content on the sinterability, physical, and mechanical properties, as well as scratch behavior, of zirconia-toughened alumina (ZTA) ceramic composites. By adjusting TiO2 content from 0 wt% to 5 wt% and employing advanced microwave sintering at 1150 °C, the study aims to lower the sintering temperature of ZTA. Microwave sintering, known for its efficiency and rapid processing, enables significant enhancements in material properties at reduced temperatures. Notably, incorporating TiO2 into ZTA yields remarkable improvements in physical and mechanical attributes, with the optimal TiO2 content determined to be 3 wt%. At this concentration, the composite achieves exceptional properties: a relative density of ∼99 %, microhardness of ∼2002 HV, and an indentation fracture toughness of ∼6.13 MPa m0.5. These enhancements represent increases of over 120 % in hardness and 61 % in toughness compared to TiO2-free ZTA. Additionally, the highest scratch resistance is observed at 3 wt% TiO2, evidenced by a minimal scratch depth of ∼7.53 μm. However, exceeding the 3 wt% solubility limit results in the formation of secondary phases, such as tialite (Al2TiO5) and zirconium titanate (ZrTiO4), which degrade the composite's properties. This research underscores the potential of TiO2 doping and microwave sintering to elevate the performance of ZTA ceramics, offering a pathway to superior materials for advanced applications.

Effect of rapid cooling on residual stress and surface fracture toughness of dental zirconia

Short-time sintering of dental zirconia not only improves manufacturing efficiency of zirconia prosthetics, but also enables an attractive situation in which prosthetic treatment can be completed within a single visit. Although many studies have clarified the effects of heating rate and dwell time on the properties of dental zirconia during short-time sintering, there are only a few studies on rapid cooling. In this study, we investigated the effect of cooling rate on dental zirconia. It was found that the cooling rate had no effect on the three-point flexural strength, but a fast cooling rate improved fracture toughness at the material surface. Raman piezo-spectroscopy showed that a compressive stress layer formed in the neighborhood of the zirconia surface and that its thickness increased with increasing cooling rate. From the above results, it was concluded that the compressive stress layer formed on the surface by rapid cooling improved the apparent fracture toughness at the material surface.

Evaluation of Surface Roughness of Translucent Zirconia After Applying Nd:YAG and CO2 Lasers: An In Vitro Study.

Surface roughness is one of the most important factors that play an important role in increasing the connection between the surface of the tooth and the applied restoration. Due to the increased interest in zirconia and the improvement of its mechanical and aesthetic properties, studies have increased that work to improve and increase its surface roughness so that it can be used as a veneer in the future. This study aims to compare the effect of two types of lasers on the surface of highly transparent zirconia to evaluate the surface roughness resulting from the two techniques. The study sample consisted of 20 ceramic cubes made of translucent zirconia (DD cubeX2, Dental Direct, Germany). It was made using a CAD-CAM Zircodenta device (Imes-Icore, Germany) and a zirconia sintering furnace (Imes-Icore, Germany). The study sample was divided into two groups; the first group consisted of 10 cubes exposed to Nd:YAG laser and the second group consisted of 10 discs exposed to continuous wave CO2 laser. The surface roughness test was conducted for the study samplesin each of the groups using a surface roughness tester. Data were collected and analyzed using SPSS v25 software. The surface roughness was measured and its mean was 1.208±0.22in the Nd:YAG laser group and 0.809±0.21in the CO2laser group. There was a significant difference between the study groups according to the independent sample T-test. This study concluded that the Nd:YAG laser surface roughensof zirconia isgreaterthan the continuous wave CO2 laser, with a substantially significant difference.

Abnormal grain growth inhibition of extrusion-based 3D-Printed 3Y-TZP ceramics sintered by flash sintering

This study investigated the combination of Direct Ink Writing (DIW) and Flash Sintering of zirconia stabilized with 3 mol. % Y2O3 (3Y-TZP). The samples were printed in two stacking configurations, and flash sintering was performed without current ramp control (FS) and using current ramp (CRFS) for comparison purposes. In both conditions, an electric field of 80 V cm−1 and a current density of 150 mA mm−2 were applied. The physical, microstructural, and mechanical properties of the printed samples were evaluated. The stacking configuration influenced both the grain size gradients and mechanical properties. Furthermore, controlling the current density ramp resulted in a slight homogenization of the grains’ size across different regions of the sample (core, edge, and flat surfaces). The presence of zirconia polymorphs, such as ZrO2-t and ZrO2-c, as well as a distorted form of the tetragonal phase (ZrO2-t'), was observed in the samples. These phases were affected by both the printing strategy and the current ramp control during the flash sintering step. In addition, the samples demonstrated typical values of Vickers hardness for 3Y-TZP (ranging from 10.5 to 11.8 GPa) and fracture toughness (ranging from 3.6 to 4.7 MPa m1/2), with a minor current density ramp control influence. Therefore, both FS and CRFS techniques represent viable pathways for producing dense 3D printed ceramic materials.

The Effect of Colloidal Silica and Glaze Coatings on the Adhesion of Zirconia with Various Ytrria Concentration.

This study evaluated the effect of coating traditional and translucent Y-TZP with an industrial nanometric colloidal silica or glaze before or after sintering on the adhesion of zirconia with various ytrria concentration. Specimens of Y-TZP with 3% and 5% yttria were subdivided into 5 groups (n=10), according to the coating applied and moment of application (before or after Y-TZP sintering): Control (no coating), Colloidal Silica/Sintering, Sintering/Colloidal Silica, Glaze/Sintering, Sintering/ Glaze. Lithium disilicate (LD) was used as positive control. Except for Y-TZP controls, groups were conditioned with silane before cementation with a self-adhesive resin cement. After 24 hours, the shear bond strength and failure analysis were performed. Also, analysis of specimens' surface was accomplished with SEM-EDX. Kruskal-Wallis and Dunn tests were applied to analyze differences between groups (p⟨0.05). Overall, the worst and best values of shear bond strength test were control and glaze after sintering groups. Different morphological and chemical aspects were observed in SEM-EDX analysis. Coating Y-TZP with colloidal silica showed unsatisfactory results. In 3Y-TZP, the surface treatment associated with the best adhesion values was the application of glaze after zirconia sintering. However, in 5Y-TZP, glaze application can be performed before or after the zirconia sintering to optimize clinical steps.

Influence of an internal firing of feldspathic porcelain before or after sintering on adaptation of high-translucent zirconia laminate veneers

The aim of the present study was to evaluate the influence of two different internal surface treatments, namely, the firing of feldspathic porcelain before or after zirconia sintering, on the marginal and internal adaptation of laminate veneers (LVs) made of high-translucent zirconia. A total of 33 zirconia LVs were fabricated using a CAD/CAM system and divided into three groups based on the internal surface treatment method: the pre-firing (PRE) group involved firing feldspathic porcelain before zirconia sintering, the post-firing (POS) group involved firing feldspathic porcelain after zirconia sintering, and the no treatment (NT) group involved no application of feldspathic porcelain. The adaptation of the LVs was measured using a silicone replica technique. Data were analyzed using the Kruskal–Wallis and Steel–Dwass tests (α = .05). The POS group showed significantly higher marginal discrepancy values than the PRE group across all sites. The internal space values of the PRE groups were significantly lower than those of the NT group at all sites. The internal firing of feldspathic porcelain before zirconia sintering resulted in better marginal adaptation of the high-translucent zirconia LVs than the internal firing of feldspathic porcelain after zirconia sintering. The internal firing of feldspathic porcelain before zirconia sintering can achieve uniform internal adaptation of high-translucent zirconia LVs.

Effect of TiO2 reinforcement on low temperature (1300 °C) sinterability of zirconia toughened alumina ceramics by correlating its structural and physico-mechanical properties

The primary goal of this research is to investigate the sinterability of zirconia toughened alumina (ZTA) at low temperature (1300 °C) utilizing two different sintering techniques: hot press and cold press. The effect of titanium oxide (TiO2) content variation (0–5 wt%) in ZTA is compared for each sintering method. The solubility limits of TiO2 in ZTA are identified to be 2 wt% and 3 wt% for hot press and cold press sintering respectively which have served exceptional physical and mechanical properties. In the case of hot press, outstanding relative density (99%) is achieved due to excellent compaction, including high microhardness of ∼2092 HV0.5, nanohardness of ∼25.05 GPa, elastic modulus of ∼371.59 GPa and indentation fracture toughness of ∼5.43 MPa·√m for 2 wt% TiO2 inclusion. Whereas in the case of cold press, 3 wt% TiO2 addition has revealed a considerable relative density (96%), alongside microhardness of ∼1975 HV0.5, nanohardness of ∼20.92 GPa, elastic modulus of ∼280.39 GPa and an indentation fracture toughness of ∼4.84 MPa·√m. However, further addition of TiO2 leads to the formation of secondary phases i.e., tialite and zirconium titanate which deteriorate the mechanical and physical properties due to the abnormal grain growth. Therefore, it has been postulated that the small additions of TiO2 have enormous capability of lowering the sintering temperature of ZTA-MgO ceramic without compromising the physical and mechanical characteristics.

Flash microwave sintering of zirconia by multiple susceptors cascade strategy

Flash microwave sintering of zirconia by multiple susceptors cascade strategy

Microwave sintering of zirconia toughened alumina - Influence of the type and content of doping in zirconia

This study focuses on the influence of zirconia on microwave (MW) sintering of zirconia-toughened alumina (ZTA). ZTA samples containing various zirconia powders (unstabilized and stabilized with yttria or ceria) were sintered in a MW cavity, in a sintering cell with or without susceptor. 8 mol% yttria-stabilized zirconia was denser when it was sintered without susceptor. The densification curves also showed different behaviours in the intermediate stage of sintering, between the four samples. The samples with 3 and 8 mol% yttria-stabilized zirconia were easier to densify than the samples with unstabilized and 10 mol% ceria-stabilized zirconia samples. This was confirmed when the samples were heated in a single-mode cavity. These differences of behaviour under MW can be linked to the chemical composition of zirconia. The substitution of zirconium cation by yttrium in the lattice generates an excess of oxygen vacancies and of dipoles. The latter are involved in the MW/material interactions.

Influence of bismuth oxide as a sintering aid on the densification of cold sintering of zirconia

In the past decades, Zirconia (ZrO2) has emerged as a promising technical ceramic, both as high temperature structural material and electrolyte for fuel cells, etc. The traditional synthesis of ZrO2 with spark plasma sintering (SPS) usually requires a sintering temperature as high as 1200 °C. General interest in lowering the sintering temperature to reduce energy consumption and thermal stresses has led to research on two promising routes – cold sintering via temperature-dependent chemical reactivity and sintering aids, which facilitates mass transport and improves densification. Here we combine both by developing a single-step sintering process benefitting from both water vapor through the in-situ conversion of Zr(OH)4 to ZrO2 and liquid phase Bi2O3 as a sintering aid. The resultant ZrO2 has a relative density above 80% with a sintering temperature as low as 900 °C, significantly higher than that of ZrO2 without sintering aids, which had a relative density of 54%, both sintered at 50 MPa. The dependence of porosity of sintered samples as a function of sintering pressure (range: 50 MPa–300 MPa) and temperature (range 400 °C–1200 °C) is mapped out as guidance for further material property design. A linear relationship between hardness and relative density was found, with a maximal hardness of 6.6 GPa achieved in samples with 30% porosity. In addition to sintered density, phase stabilization of tetragonal ZrO2 is enhanced at sintering temperature of 900 °C with water vapor and Bi2O3, respectively.

Effect of superspeed sintering on translucency, opalescence, microstructure, and phase fraction of multilayered 4 mol% yttria-stabilized tetragonal zirconia polycrystal and 6 mol% yttria-stabilized partially stabilized zirconia ceramics

Statement of problemThe optical properties of recently developed multilayer zirconia have mainly been studied for the effects of conventional sintering and speed sintering but not as much for the effect of superspeed sintering. As superspeed sintering protocols typically require a higher sintering temperature and higher heating and cooling rates than speed- and conventional sintering protocols, the optical properties of superspeed sintered zirconia may be affected differently. PurposeThe purpose of this in vitro study was to investigate the effect of superspeed sintering on the optical properties, microstructure, and phase fraction of multilayered 4 mol% yttria-stabilized (4Y-) and 6 mol% yttria-stabilized (6Y-) zirconia. Material and methodsMultilayered 4Y- and 6Y-zirconia were sectioned. After conventional and superspeed sintering, the translucency parameter (TP), and opalescence parameter (OP) were measured with a spectrophotometer (n=10). To obtain the grain sizes from the field emission scanning electron microscopy (FE-SEM) images for each layer (n=2), more than 500 (6Y-zirconia) and 800 grains (4Y-zirconia) were measured by linear intercept methods. The phase fractions were obtained through X-ray diffraction (XRD) analysis by using the Rietveld method (n=1). The results were analyzed by 3-way ANOVA and post hoc Tukey honest significant difference tests (TP and OP) and by 3-way ANOVA and post hoc Scheffé tests (grain size) (α=.05). ResultsNo layers exhibited a significant difference in TP after superspeed sintering, except the dentin layer (DL) and transition layer 2 (T2) of 4Y- and 6Y-zirconia, respectively. The TP increased (P<.05) in DL for superspeed sintered 4Y-zirconia and decreased (P<.05) in T2 for the superspeed sintered 6Y-zirconia. However, the difference in TP by superspeed sintering was lower than the perceptibility thresholds of 50:50%. The OP decreased (P<.05) in the DL and T2 of 4Y-zirconia after superspeed sintering. For 6Y-zirconia, the OP decreased (P<.05) in all layers except for the transition layer 1 (T1) after superspeed sintering. However, the difference in OP values was minimal, with only a 1.1 difference observed for Zolid Gen-X (4Y) and a range of 1.22 to 1.62 for Katana UTML (6Y) when using superspeed sintering. No significant change was found in the grain size after superspeed sintering of either zirconia. Regardless of the sintering speed, the average grain size of the 6Y-zirconia (conventional: 2.09 to 2.21 μm; superspeed: 2.11 to 2.20 μm) was larger than that of the 4Y-zirconia (conventional: 0.50 to 0.52 μm; superspeed: 0.52 to 0.54 μm). Owing to superspeed sintering, the metastable tetragonal (T′) phase content increased while the tetragonal (T) phase decreased in 4Y-zirconia; in 6Y-zirconia, the cubic (C) phase content increased, while the T′-phase content decreased. ConclusionsSuperspeed sintering did not result in any clinically significant changes in the translucency and opalescence of 4Y- or 6Y-zirconia.

Modeling spark plasma sintering of zirconia with prediction of final stage high densification rate

In this study, the SPS of 0.1 µm zirconia has been performed and shows high densification rate behavior in the final stage. This work consists of modeling the densification behavior of this powder especially at the intermediate/final stage transition. To model this, a Master Sintering Curve (MSC) is combined with an analytic model to identify the activation energy and the sintering moduli. The modeling of the behavior of the powder during the sintering tests is done via the Skorohod-Olevsky model. It appears from this study that the modeling of final stage sintering requires a regime transition to model the exceptionally high densification rate of the powder. The final stage grain growth seems not to decrease the final stage sintering kinetics.

Effect of Ga2O3 Dopant on High Speed Sintered 5 mol% Y2O3 Stabilized Dental Zirconia.

The high-speed sintering of zirconia has become essential for ceramic dental prosthesis treatment in a single visit. Previous studies have shown that 5 mol% yttria-stabilized zirconia (5Y zirconia), with the exception of some types, loses strength and translucency with high-speed sintering. In this study, 0.15-0.92 wt% Ga2O3, which is expected to promote the sintering of zirconia, was added to improve the properties of 5Y zirconia high-speed sintered bodies, and the effect of its addition was evaluated. The specimens were characterized by density and translucency measurements, a three-point bending test, X-ray diffraction (XRD), scanning electron microscopy (SEM), and shrinkage measurement. The addition of Ga2O3 improved both translucency and flexural strength of 5Y zirconia high-speed sintered bodies. XRD and SEM observations revealed that this improvement in properties was due to the change in the crystal phase composition and the decrease in the amount and size of pores due to the addition of Ga2O3. Shrinkage measurements also revealed that the addition of Ga2O3 changed the sintering behavior of 5Y zirconia, suggesting that this change led to a reduction in porosity. From the above results, it was concluded that Ga2O3 addition is effective in improving the properties of 5Y zirconia high-speed sintered bodies.

Effect of speed sintering of monolithic zirconia with different yttria contents on color and crystal phase.

This study evaluated the color and microstructure of monolithic zirconia crowns with different yttrium oxide (Y2 O3 ) contents treated by conventional or speed sintering. Four types of zirconia ceramics were assessed: two monolayer zirconia, and two multilayer zirconia. The monolithic zirconia crowns were fabricated using a dental computer-aided design/computer-aided manufacturing (CAD/CAM) system and in two shades (A2 and BL). After milling, the zirconia crowns were sintered using either speed sintering or conventional sintering. For each combination of zirconia (4), shade (2), and sintering condition (2), the color parameters were determined at three positions of each of nine crowns using a non-contact dental spectrophotometer. In addition, the zirconia phases in the specimens were quantified using X-ray diffractometry. Significant differences in the ΔE00 values at different measurement positions were observed for the Multi2 crown of the BL shade group. The color difference resulting from conventional and speed sintering programs was not affected by the difference in yttria content of Mono1, Mono2, and Multi1. However, in Multi2, containing 3Y-TZP and 5Y-PSZ, a color change was caused by the use of speed sintering. Therefore, when performing speed sintering with Multi2, it is necessary to select the color in consideration of these results or take measures for staining.

Conventional, Speed Sintering and High-Speed Sintering of Zirconia: A Systematic Review of the Current Status of Applications in Dentistry with a Focus on Precision, Mechanical and Optical Parameters.

The aim of this systematic review was to provide an overview of the technical and clinical outcomes of conventional, speed sintering and high-speed sintering protocols of zirconia in the dental field. Data on precision, mechanical and optical parameters were evaluated and related to the clinical performance of zirconia ceramic. The PICOS search strategy was applied using MEDLINE to search for in vitro and in vivo studies using MeSH Terms by two reviewers. Of 66 potentially relevant studies, 5 full text articles were selected and 10 were further retrieved through a manual search. All 15 studies included in the systematic review were in vitro studies. Mechanical, precision and optical properties (marginal and internal fit, fracture strength and modulus, wear, translucency and opalescence, aging resistance/hydrothermal aging) were evaluated regarding 3-, 4- and 5-YTZP zirconia material and conventional, high- and high-speed sintering protocols. Mechanical and precision results were similar or better when speed or high-speed sintering methods were used for 3-, 4- and 5-YTZP zirconia. Translucency is usually reduced when 3 Y-TZP is used with speed sintering methods. All types of zirconia using the sintering procedures performed mechanically better compared to lithium disilicate glass ceramics but glass ceramics showed better results regarding translucency.

Evaluation of the Effect of High-Speed Sintering and Specimen Thickness on the Properties of 5 mol% Yttria-Stabilized Dental Zirconia Sintered Bodies

High-speed sintering of zirconia has become essential to single-visit dental prosthetic treatments. This important prosthetic dentistry technique demands a translucent material tougher than porcelain. Previous studies on high-speed sintered zirconia did not take heat and material thickness into consideration. We evaluated pre-sintered specimen thickness and the effect of high-speed sintering on the properties of 5 mol% Y2O3-stabilized zirconia (5Y zirconia). High-speed sintered bodies of 5Y zirconia were evaluated by density measurements, translucency measurements, three-point flexural and fracture toughness tests, X-ray diffraction (XRD), and scanning electron microscopy (SEM). High-speed sintering reduced the translucency and mechanical properties of 5Y zirconia. XRD and SEM observation results clarified that these reductions were due to the change in crystal phase composition and to the increase in residual pores, respectively, both resulting from high-speed sintering. Moreover, in high-speed sintering, as the thickness of the specimen increased, the number and size of internal pores increased, and the translucency and strength decreased. The threshold value for avoiding a reduction in translucency and mechanical properties was found to lie at ~4.4 mm. From the above results, it was concluded that 5Y zirconia is not suitable for high-speed sintering applications.

Editorial: Is Zirconia the Holy Grail of All-Ceramic Restorations?

Editorial: Is Zirconia the Holy Grail of All-Ceramic Restorations?

Editorial: Dental Ceramics: From Science and Technology to Clinical Application

Editorial: Dental Ceramics: From Science and Technology to Clinical Application

Effect of sintering condition and low-temperature degradation on the flexural strength and phase transformation of zirconia

Statement of problemThe traditional sintering of zirconia takes an extended time, and accelerated treatments have been developed to reduce treatment time and manufacturing costs. Studies evaluating the effect of sintering time on the mechanical properties of zirconia are lacking. PurposeThe purpose of this in vitro study was to evaluate the effect of the sintering condition and the low-temperature degradation (LTD) of zirconia on the flexural strength of monolithic zirconia. Material and methodsZirconia specimens (LUXEN Enamel) were sintered at 1500 °C, 1530 °C, and 1560 °C for 4, 5, 6, 7, and 12 hours and subjected to LTD (n=10). Control specimens were assessed in the nontreated condition. The 3-point flexural strength was measured by using a universal testing machine. The crystal phases of the specimens were compared and quantitatively analyzed through X-ray diffraction (XRD) analysis, and the crystal grain size was measured by using a field emission scanning electron microscope (FE-SEM). Two-way ANOVA and the independent sample t test were used to analyze the experimental results (α=.05). ResultsIn the group not subjected to LTD, there was no difference in flexural strength according to the change in sintering temperature and sintering time (P>.05). The group subjected to LTD showed a difference in flexural strength according to sintering time difference (P<.001). The flexural strength of the zirconia with LTD exposure increased compared with that of the zirconia specimen not subjected to LTD (P<.001). With LTD exposure, cubic and monoclinic crystals increased, tetragonal crystals decreased, and the particle size increased. As the sintering temperature increased, the particle size increased, but not according to the sintering time. ConclusionsAt all sintering times, the flexural strength of zirconia was over 800 MPa, which is the minimum flexural strength of a 4-unit or longer prosthesis as specified in the International Organization for Standardization (ISO) 6872. With LTD exposure, the increase in the flexural strength of zirconia was associated with the phase change from tetragonal to monoclinic.