• Restorative Dentistry and Endodontics
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• v.45 no.1
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• pp.6.1-6.8
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• 2020

Objectives: This study investigated the effects of a hydrofluoric acid (HA; solution of hydrogen fluoride [HF] in water)-based smart etching (SE) solution at an elevated temperature on yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics in terms of bond strength and morphological changes. Materials and Methods: Eighty sintered Y-TZP specimens were prepared for shear bond strength (SBS) testing. The bonding surface of the Y-TZP specimens was treated with 37% phosphoric acid etching at 20℃-25℃, 4% HA etching at 20℃-25℃, or HA-based SE at 70℃-80℃. In all groups, zirconia primers were applied to the bonding surface of Y-TZP. For each group, 2 types of resin cement (with or without methacryloyloxydecyl dihydrogen phosphate [MDP]) were used. SBS testing was performed. Topographic changes of the etched Y-TZP surface were analyzed using scanning electron microscopy and atomic force microscopy. The results were analyzed and compared using 2-way analysis of variance. Results: Regardless of the type of resin cement, the highest bond strength was measured in the SE group, with significant differences compared to the other groups (p < 0.05). In all groups, MDP-containing resin cement yielded significantly higher bond strength values than MDP-free resin cement (p < 0.05). It was also shown that the Y-TZP surface was etched by the SE solution, causing a large change in the surface topography. Conclusions: Bond strength significantly improved when a heated HA-based SE solution was applied to the Y-TZP surface, and the etched Y-TZP surface was more irregular and had higher surface roughness.

• Journal of the Korean Ceramic Society
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• v.26 no.5
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• pp.719-727
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• 1989

By using commercial zirconia powder CeO2-ZrO2 ceramics containing 8~16mol% CeO2 was made by heat treatment at 1350~155$0^{\circ}C$ for 1~10hr. The minimum amount of CeO2 for obtaining complete tetragonal phase was 12mol%, and in the tetragonal phase region fracture toughness of Ce-TZP was decreased with increasing CeO2 content and the maximum value was obtained when 12mol% CeO2 was added. The bending strength goes through maximum at 14mol% CeO2. Fracture mode of Ce-TZP transformed from intergranular to transgranular fracture with increasing CeO2 content, so the morphology of fracture surface of 16mol% Ce-TZP was wholly transgranular and this tendency was independent on grain size. The crystal structure of the 12mol% Ce-TZP was monoclinic with fringes along the grain boundaries which are lying in the particular plane from the TEM observation. The chemical composition of the sintered body was homogeneous as a whole and some amorphism or air pocket was observed at the triple junction.

• The Korean Journal of Ceramics
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• v.5 no.1
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• pp.1-11
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• 1999

The effect of aliovalent dopents, $Nb_3O_5$ and MnO, on the grain growth kinetics of 12 mol% ceria stabilized tetragonal zirconia polycrystals (Ce-TZP) was studied. All specimens were sintered at $1550^{\circ}C$ for 20 minutes prior to annealing at different temperatures to study grain growth kinetics. Grain growth kinetics of Ce-TZP and 1 mol% $Nb_2O_5$ doped Ce-TZP (Ce-TZP/$Nb_3O_5$) during annealing at 1475, 1550, and $1600^{\circ}C$ adequately matched with square law $(D^2-D_\;o^2=k_at)$. However, grain growth in 1 mol% MnO suppressed grain growth in Ce-TZP by drag force exerted by $Mn^{+2}$ ions which segregated strongly to the positively-charged grain boundaries of Ce-TZP, $Nb_2O_5$ enhanced grain growth by increasing the concentration of vacancies of $Zr^{+4}$ ion and $Ce^{+4}$ ions. Surface analysis with X-ray photoelectron spectroscopy (XPS) showed the segregation of Mn+2 ions to grain boundaries. The kinetics of grain growth obtained in the base Ce-TZP and the Ce-TZPs with the aliovalent dopants were examined in the context of impurity drag effect and space charge effect.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 2000.06a
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• pp.243-248
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• 2000

Effect of NiO addition on microstructure, stability of tetragonal phase and mechanical properties was investigated. (Y, Ni)-TZP solid solution was obtained by pressureless sintering. The fracture toughness was increased by solid solution of NiO. Neither reaction phase nor glassy phase was observed at the grain boundaries. From these results, it was determined that solid solution of NiO was destabilized tetragonal phase of Y-TZP. Y-TZP/Ni nanocomposite that contained nano-sized Ni particles was also fabricated by internal reduction method. Some evaluations and discussions were carried out for both (Y, Ni)-TZP solid solution and Y-TZP/Ni nanocomposite.

• The Korean Journal of Ceramics
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• v.5 no.4
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• pp.331-335
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• 1999

Mechanical propeties of $Y_2O_3$-containing tetragonal $ZrO_2$ polycrystals(Y-TZP) were investigated. Several additives were used to modify the hardness fracture toughness of Y-TZP. The effects of these individual additives were discussed and their interactions were also analyzed. Each additive, such as CoO, $Fe2O3, MnO_2$ was found to deteriorate the mechanical propeties of Y-TZP when it was used singly. But the fracture toughness of Y-TZP was singnificantly improved when these additives and $Al_2O_3$ were added in combination at a certain ratio.

• Journal of the Korean Ceramic Society
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• v.29 no.11
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• pp.877-887
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• 1992

Tetragonal zirconia powder with 3 mol% Y2O3 mas mixed with up to 30 vol% of ${\beta}$-SiC powders, and the mixtures were hot-pressed at 1500$^{\circ}C$ for 60 min under a pressure of 30 MPa in Ar atmosphere. Flexural strength and fracture toughness were measured at room-and high-temperature (1000$^{\circ}C$). Evolution of microstructure was also conducted to investigate the effects of SiC addition on the properties of 3Y-TZP ceramics. Average grain size of the composites was about 0.5 $\mu\textrm{m}$, and decreased with SiC addition. Both room- and high-temperature mechanical properties of the composites were improved with SiC content. Particularly, high-temperature strength and fracture toughness of 3Y-TZP/30v/o SiC composite were twice as high as those of 3Y-TZP. The hardness of the composites also increased with SiC content and reached maximum value at 3Y-TZP/30v/o SiC composite.

• Journal of the Korean Ceramic Society
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• v.27 no.4
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• pp.465-472
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• 1990

The effects of Al2O3 and Cr2O3 addition on the mechanical properties and microstructures of Y-TZP ceramics obtained by co-precipitation method of ZrO2＋3m/o Y2O3, following pressureless sintering at 150$0^{\circ}C$ for 2h were investigated. The addition of Al2O3 and Cr2O3 improved the Y-TZP sinterability and the Al2O3 addition showed the better effect on Y-TZP sintering than that of the Cr2O3 addition. The density and microstructure had the better effect on the bending strength of specimen more than stressinduced phase transformation (SIPT) of ZrO2 from tetragonal to monoclinic phase. The hardness of the specimens was found to be depend on the relative density and the fracture toughness of Y-TZP was found to rely on the amount of SIPT. The grian size of Cr2O3-doped Y-TZP was observed to be relatively smaller and had a narrower distribution than that of Al2O3-doped Y-TZP. If decomposition reaction of Cr2O3 can be controlled at high temperatures, it is anticipated that the mechanical properties of Y-TZP can be much improved by the Cr2O3 addition.

• Restorative Dentistry and Endodontics
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• v.46 no.4
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• pp.54.1-54.10
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• 2021

Objectives: The purpose of this study was to quantify phase transformation after hydrofluoric acid (HF) etching at various concentrations on the surface of yttria-stabilized tetragonal zirconia polycrystal (Y-TZP), and to evaluate changes in bonding strength before and after thermal cycling. Materials and Methods: A group whose Y-TZP surface was treated with tribochemical silica abrasion (TS) was used as the control. Y-TZP specimens from each experimental group were etched with 5%, 10%, 20%, and 40% HF solutions at room temperature for 10 minutes. First, to quantify the phase transformation, Y-TZP specimens (n = 5) treated with TS, 5%, 10%, 20% and 40% HF solutions were subjected to X-ray diffraction. Second, to evaluate the change in bond strength before and after thermal cycling, zirconia primer and MDP-containing resin cement were sequentially applied to the Y-TZP specimen. After 5,000 thermal cycles for half of the Y-TZP specimens, shear bond strength was measured for all experimental groups (n = 10). Results: The monoclinic phase content in the 40% HF-treated group was higher than that of the 5%, 10%, and 20% HF-treated groups, but lower than that of TS-treated group (p < 0.05). The 40% HF-treated group showed significantly higher bonding strength than the TS, 5%, and 10% HF-treated groups, even after thermal cycling (p < 0.05). Conclusions: Through this experiment, the group treated with SiO₂ containing air-borne abrasion on the Y-TZP surface showed higher phase transformation and higher reduction in bonding strength after thermal cycling compared to the group treated with high concentration HF.

• Korean Journal of Materials Research
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• v.10 no.10
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• pp.677-683
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• 2000

Three- and five-layer 3Y-YZP/12Ce- TZP composites prepared by a slip casting method have been char­acterized in terms of mechanical properties. The fracture strength of mutilayer c$\alpha$nposites determined in a diametral compression test was 327~534 MPa. Although the indentation strength of the materials was generally reduced with i increasing Vickers indentation load up to 300 N, the damage resistance of multilayer composites was superior com­pared to monolithic layer TZP material. The four-point bend strength of the layered material remained at the values of 620~674 MPa after indentation with a load of 49 N, while that of the monolithic TZP material was 129~339 MPa. The microindentation toughness of the multilayer material was $7.7~13.1\;MPa{\cdot}m^{1/2}$.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.28 no.3
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• pp.170-174
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• 2015

Composite ceramics of alumina-TZP(3Y) have good mechanical and electrical properties. So, They have been used as high strength refractory materials and thick film substrates, etc. In this study, Composite ceramics of alumina-TZP(3Y) were fabricated by uniaxial pressing and sintering at 1,400, 1,500, and $1,600^{\circ}C$, and their microstructures and mechanical properties were investigated. As the TZP(3Y) content in composite ceramics increases from 20 wt.% to 80 wt.%, the fracture toughness increases monotonically, which seems to be related to the higher relative density and/or toughening mechanism by means of stabilized tetragonal zirconia phase at room temperature. In contrast to the fracture toughness, Vickers hardness of the composite ceramics shows maximum value (1,938 Hv) at a 40 wt.% of TZP(3Y). The result of Vickers hardness is likely to be due to more dense sintered microstructure of composite ceramics than pure alumina and reinforcement of composite ceramics with TZP(3Y), considering that Vickers hardness of pure $Al_2O_3$ is greater than that of TZP(3Y). It is also shown that the $ZrO_2$ particles are $l^{\circ}Cated$ between $Al_2O_3$ grains and suppress grain growth each other.