• 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.

• Journal of the Korean Ceramic Society
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• v.40 no.6
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• pp.525-529
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• 2003

Biotribological properties, such as wear rate and friction coefficient, of 3Y-TZP and Low Temperature Degradation (LTD) free materials were investigated via a ball(SiC)-on-plate sliding wear test to evaluate the relationship between wear mechanism and phase transformation. Wear test was conducted with a sliding speed of 0.035 m/s at room temperature and at 25$0^{\circ}C$ in air under a normal load of 49 N, respectively. Although friction coefficient of 3Y-TZP was the lowest due to the fine grain size, the highest wear loss and rate were observed due to the debris of monoclinic grains introduced during sliding and their values increased drastically with raising temperature. However, the biotribological properties of LTD-free materials were insensitive to temperature due to the inertness of the phase transformation, suggesting that they may be applicable to the biomechanical parts.

• Journal of the Korean Ceramic Society
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• v.42 no.2 s.273
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• pp.140-144
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• 2005

The microstructures and mechanical properties of Tetragonal Zirconia Polycrystals (TZP) sintered bodies, which made by pressureless and spark plasma sintering techniques, were investigated using XRD, SEM, and TEM techniques. In the spark plasma sintered samples, the TZP grains were equiaxed type including many sub-grain boundaries regardless of sintering conditions. The biaxial strength of TZP having an average of 80 nm grains in diameter was high in value with 1025 MPa, but fracture toughness showed a low value due to the absence of a fracture toughening mechanism such as transformation toughening. In the Pressureless Sintered (PLSed) samples, the grain size of TZP was strongly dependent on the sintering temperature; i.e., it gradually increased as the sintering temperature increased. The value of fracture toughness increased as the grain size increased by the stress-induced phase transformation and Borne crack deflection.

• Journal of the Korean Ceramic Society
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• v.32 no.10
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• pp.1147-1161
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• 1995

When ceramic membrance was made from metal salt solution in place of metal akoxide solution, crack free and good adhesion to supporter was optimized for sol stability and good adhesion force. A starting sol was prepared from aluminum oxychloride aqueous solutjion in order to inhibit the grain growthof Al2O3 during heat treatment. The crack free dip coating can't be achieved in 1mol/ι zirconium oxychloride solution because of the high viscosity which interferes with the hydration copolymerization between Al3+ ion and Zr4+ ion. Thus Al2O3-ZrO2 sol stability and viscosity for dip coating was effective when 0.01 mol/ι zirconium oxychloride was added. The minimizing of crack and achieving better adhesion to the supporter wa obtained by microwave drying, surfactant addition and ultrasonic dip coating in wet atmosphere. The result seems to minimize the capillary force and improve the adhesive ability to supporter during the process. Where the average pore size of Al2O3-ZrO2 ultrafilter ceramic membrane measured 17 Å by the BET method and observed γ-Al2O3 phase with tetragonal zirconia after firing at 700℃.

• Korean Journal of Materials Research
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• v.24 no.7
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• pp.357-362
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• 2014

Thermal barrier coatings(TBCs) are being applied in many industrial fields such as thermal power generation, aviation and seasonal fields. $ZrO_2-Y_2O_3$(8%) thermal spray coating powders are commercially used as thermal-barrier coating materials to protect against oxidation and corrosion of heat-resistant alloys at elevated temperatures. Currently, $ZrO_2-Y_2O_3$(8%) thermal-spray powder is made using the industrial co-precipitation process, which is very complex and requires a lot of time. In this study, orthorhombic $ZrO_2$ and $Y_2O_3$ powders were fabricated by mechanical mixing, which is more economical than the co-precipitation process. A tetragonal, yttria-stabilized zirconia(YSZ) coating-layer was produced by plasma spraying, using orthorhombic $ZrO_2-Y_2O_3$(8%) powder. Our experimental results indicate that $ZrO_2-Y_2O_3$(8%) mixed powder can be used economically in industry because it is no longer necessary to make this powder by liquid and gas-phase methods.

• Korean Journal of Materials Research
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• v.26 no.2
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• pp.95-99
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• 2016

In this study, 5 um sized $ZrSiO_4$ was ground to 1.9 um, 0.3 um, and 0.1 um sized powders by wet high energy milling process, and the sintering characteristics were observed. Pure $ZrSiO_4$ itself can-not be sintered to these levels of theoretical density, but it was possible to sinter $ZrSiO_4$ powder of nano-scale size of, -0.1 um to the theoretical density and to lower the sintering temperature for full density. Also, the decomposition of $ZrSiO_4$ with a size in the micron range resulted in the formation of monoclinic $ZrO_2$; however, in the nano sized range, the decomposition resulted in the tetragonal phase of $ZrO_2$. So, it was possible to improve the sintering characteristics of nano-sized $ZrSiO_4$ powders.

• Journal of dental hygiene science
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• v.12 no.2
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• pp.123-129
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• 2012

The aim of study was to compare the color parameters and mean color difference of porcelain specimens by different veneering technique in order to examine the effect of veneering technique on esthetics of yttria-stabilized tetragonal zirconia polycrystalline(Y-TZP) all ceramic restoration. Three groups of square-shaped core ceramic specimens(14mm in diameter and 0.3, 0.5, 0.7 mm) and two groups of veneering ceramic specimen were prepared for analysis. Color parameter($L^*,a^*,b^*$) and color difference of zirconia core squares and core-veneer specimens were measured with ShadeEye $NCC^{(R)}$ spectrophotometer, respectively. Mean color difference(${\Delta}E^*$)were calculated using color difference formula. Two-way analysis of variance(ANOVA) combined with a Tukey multiple-range test were used to analysis the data(${\alpha}=0.05$). ${\Delta}E^*$ values were not significantly affected by core thickness and veneering porcelain(p=0.083). The color differences(${\Delta}E^*$) of core-veneer specimens with 0.5, 0.7 mm-A1,A2,A3.5 shade were mostly below 3.7 which was within the clinically acceptable range, while color differences between 0.3 mm-A1,A2 showed more than 3.7. All-ceramic system has color characteristics that clinicians have to consider when selecting materials. Also, manufacturers of different porcelain systems must make every effort to achieve color reproducibility.

• Journal of the Mineralogical Society of Korea
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• v.13 no.3
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• pp.164-170
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• 2000

Neutron single crystal and powder diffraction techniques have been applied to the structure analysis of yttria-stabilized zirconium, Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$., prepared by the skull-melting method. The crystal structure has been determined to be cubic symmetry, space group Fm/equation omitted/ with a=5.155(2)$\AA$, V=136.99(5)$\AA$, Z=4, and R(F)=5.65%, $\omega$R(I)=10.57% for 70 integrated intensities of Bragg Peaks observed from single crystal of Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$. The stabilizer atoms randomly occupy the zirconium sites and there are displacements of oxygen atoms with amplitudes of $\Delta$/a~0.033 and 0.11 along <110> and <100> directions from the ideal positions of the fluorite structure, respectively. There are no significant differences in crystallographic data between the single crystal and powder studies. Diffraction pattern after Rietveld refinement, using neutron powder data, has shown the evidence of a tetragonal impurity phase, or a slight tetragonal distortion.

• Korean Chemical Engineering Research
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• v.51 no.2
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• pp.208-213
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• 2013

Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

• Journal of the Korean Ceramic Society
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• v.24 no.3
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• pp.243-250
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• 1987

The effects aging on some properties and thermal-shock behavior of zirconia partially stabilized with 9 mol% MgO (9MZ) were studied. 9MZ specimens were aged over $1200^{\circ}$-$1400^{\circ}C$ for 12hours subsequently, after sintering at $1650^{\circ}C$ for 4 hours. Fracture strength(both before and after thermal-shock test), linear thermal expansion, monoclinic fraction and phase transition by XRD, density, galvanic potential and microstructure were measured. Quantitative chemical analysis around the grain-boundary of the specimen aged at $1350^{\circ}C$ was also conducted by EDX. The aging of 9MZ specimen causes a thermal decomposition of cubic-$ZrO^{2}$ into the formation metastable tetragonal-$ZrO^{2}$ and MgO. The former increases the residual strength after thermal-shock test and the latter improves the thermal-shock resistance due to thermal conduction through the continuous magnesia phase and the formation of monoclinic phase content in matrix were increased with decreasing the aging temperature from $1400^{\circ}C$ to $1200^{\circ}C$. Galvanic potential of the aged specimen exhibited a proper emf characteristic.