• Journal of the Korean Ceramic Society
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• v.41 no.2
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• pp.111-117
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• 2004

3Y-TZP containing 0.3∼1.2 wt% of $Al_2$O$_3$ was prepared by slip-casting after attrition milling. The specimen was sintered at 1390∼151$0^{\circ}C$ and mechanical characterization and microstructure analysis were conducted. Monoclinic content of the specimen was calculated by XRD. The apparent density of specimen increased with increasing sintering temperature. While above 1470%, the formation of m-ZrO$_2$ degraded the density. The microhardness of specimen decreased with temperature because monoclinic phase increased wit the grain growth. The specimen containing $Al_2$O$_3$ below 0.9 wt% sintered at 143$0^{\circ}C$ showed the highest microhardness of 1360 Hv.

• Journal of the Korean Ceramic Society
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• v.38 no.7
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• pp.602-607
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• 2001

Zirconia powder containing 3 mol% yttria (3Y-PSZ) was casted on the cast iron substrate by plasma spraying method. Coated specimens were then heat treated at 500$\^{C}$ in nitrogen plasma. Wear tests were performed on nitrogen heat treated and non heat treated samples at temperatures from 25$\^{C}$ to 600$\^{C}$. Wear results showed that the friction coefficient and the wear loss of both the treated and the non-treated samples showed maximum value at 400$\^{C}$. These results were explained by low temperature thermal degradation due to the monoclinic transformation. Nitrogen plasma treatment significantly improved the tribological performance. The effect of nitrogen heat treatment on tribological behavior was explained by the increased micro-hardness and decreased monoclinic faction.

• Journal of the Korean Ceramic Society
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• v.47 no.4
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• pp.343-352
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• 2010

A zirconia gel/polymer hybrid nanofiber was produced in a nonwoven fabric mode by electrospinning a sol derived from hydrolysis of zirconium butoxide with a polyvinyl butyral. Results indicated that the hydroxyl groups on the vinyl alcohol units in the backbone of the polymer were involved in the hydrolysis as well as grafting the hydrolyzed zirconium butoxide. In addition, use of acetic acid as a catalyst resulted in further hydrolysis and condensation in the sol, which led to the growth of -Zr-O-Zr- networks among the polymer chains. These networks gradually transformed into a crystalline zirconia structure upon heating. The as-spun fiber was smooth but partially wrinkled on the surface. The average fiber diameter was $690{\pm}110\;nm$. The fiber exhibited a strong but broad blue photoluminescence with its maximum intensity at a wavelength of ~410 nm at room temperature. When the fiber was heat-treated at $400^{\circ}C$, the fiber diameter shrunk to $250{\pm}60\;nm$. Nanocrystals which belonged to a tetragonal zirconia phase and were ~5 nm in size appeared. A strong white photoluminescence was observed in this fiber. This suggests that oxygen or carbon defects associated with the formation of the nanocrystals play a role in generating the photoluminescence. Further heating to $800^{\circ}C$ resulted in a monoclinic phase beginning to form In the heat-treated fibers, coloring occurred but varied depending on the heating temperature. Crystallization, coloring, and phase transition to the monoclinic structure influenced the photoluminescence. At $600^{\circ}C$, the fiber appeared to be fully crystallized to a tetragonal zirconia phase.

• Applied Chemistry for Engineering
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• v.25 no.6
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• pp.564-569
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• 2014

Zirconia nanoparticles were synthesized by hydrothermal process, and experimental parameters such as reaction temperature, reaction time, kind and concentration of precipitator, kind of precursor were varied. Particle sizes and crystalline phases of each synthesized nanoparticles were analyzed with X-ray diffraction and FE-scanning electron microscope (SEM). The particle size and crystallization of zirconia increased with increasing concentration of precipitator. The growth rate of particle sizes when NaOH as a precipitator was used also increased more than that of KOH. Therefore, the use of KOH rather than NaOH was more effective in the control of particle sizes. An amorphous zirconia nanoparticle was found in 4 h of hydrothermal reaction, but the monoclinic zirconia nanoparticle was found in 8 h and over of hydrothermal reaction, and the width of nanoparticles was slightly slimmed and the length of nanoparticles was slightly extended with increasing reaction time. The smallest particle size was produced at the same synthesis condition when zirconium chloride among the precursors such as zirconium (IV) acetate, zirconium nitrate and zirconium chloride was used.

• The Journal of the Korean dental association
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• v.49 no.5
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• pp.260-264
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• 2011

Zirconia ($ZrO_2$) is a crystalline dioxide of zirconium. Dental zirconia blocks for CAD/CAM are usually fabricated with powders of tetragonal zirconia polycrystals (TZP) stabilized with 3mol% yttria. Because of its mechanical properties similar to those of metals and color similar to tooth, it is evaluated to attain the two purposes at a time, strength and aesthetic in prosthetic dentistry. The ability of transformation of Y-TZP from tetragonal to monoclinic helps to prevent crack propagation and contributes the increase of strength and fracture toughness. Two different types of blocks, soft and hard, are used to prepare the zirconia frameworks. The fuzzy-sintered block is difficult in machining, so pre-sintered soft 3Y-TZP block is usually used to mill by computer aided machining.

• Journal of the Korean Ceramic Society
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• v.45 no.2
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• pp.126-131
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• 2008

In this study, we prepared zirconia gel by the sol-gel method and investigated its photoluminescence properties by varying pyrolysis temperature. The addition of acetic acid into a Zr-alkoxide solution resulted in forming the bidentate ligands with Zr ions and producing a stable gel. At the pyrolysis temperature of $350^{\circ}C$, the zirconia nanocrystals with tetragonal structure gradually appeared in the gel. The PL intensity of the zirconia gel increased with increasing the pyrolysis temperature up to $350^{\circ}C$, but decreased above the temperature. Concurrently, its PL peak wavelength continuously shifted from ${\sim}440\;nm$ to ${\sim}550\;nm$ with the temperature. The PL characteristics of the zirconia gels were closely associated with decomposition of residual organic groups, the formation of the zirconia nanocrystals, and the tetragonal to monoclinic phase transformation.

• Journal of the Korean Ceramic Society
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• v.20 no.4
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• pp.347-355
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• 1983

A batch mixture was prepared as 16mol% CaO-84mol% $ZrO_2$ of regeant-grade powder. The monoclinic Zirconia powder had an average particle size of $9.24 \mu\textrm{m}$ and calcium carbonate powder had a reported purity of 99.7 weight percent and mean particle size of TEX>$24, 37<\mu\textrm{m}$. The specimens were fired at 1400, 1500, 1650 and $1750^{\circ}C$ for 0. 3, 5 and 7 hours respectively. After fired the specimens were investigated using Scaning electron microscopy. Density Porosity Compressive strength Modulus of rupture and Thermal expansion were measured X-ray diffration analysis was also carried out. The results are as follows ; 1) As the firing temperature or soaking time was increased firing linear shrinkage apparent density compressive strength and modulus of rupture increased but apparent porosity decreased, 2) Cubic and monoclinic Zirconia was found at $1400^{\circ}C$ and cubic Ziconia found above $1500^{\circ}C$ 3) The specimens fired at 140$0^{\circ}C$ without soaking display thermal expansion curves by monoclinic〓tetragonal transformation and no tranformation was found at $1400^{\circ}C$ for 5hrs and above $1500^{\circ}C$. 4) The lattice parameter had constant value of 5.1345 $\AA$ through all the ranges of firing temperature 5) The higher the firing temperature was or the longer the soaking time was the larger the grain size was.

• Journal of the Korean Ceramic Society
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• v.20 no.3
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• pp.217-226
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• 1983

Adquate amount of calcia was added to the regent-grade Zirconia body. Here the amount and the form of calcia were 7-21 mol% and regent-grade calcium cabonate respectively. The specimens were fired at 175$0^{\circ}C$ for 0, 3, 5 and 7 hours respectively. The phase Strength X-ray diffraction analysis and Scaning electron microscopy. The results were as follows (1) As the additive amount of calcia was increased the firing linear shrinkage apparent density compressive strength and modulus of rupture decreased but the apparent porosity increased. (2) The specimens soaked and containing calcia displayed the grain growth. (3) Monoclinic and cubic zirconia were seen in the sepcimens containing 7 mol% calcia. When without soaking the specimens containing 7-10 mol% calcia had the volume change by monoclinic$\rightleftharpoons$tetragonal transformation. (4) The lattice parameter increased according as the calcia additive was increased. The specimens containing above 19mol% calcia had the costant lattice parameter. The value of that was from 5.1264 to 5.1396 $\AA$ in the case of 7 hours soaking.

• The Journal of Advanced Prosthodontics
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• v.1 no.3
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• pp.113-117
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• 2009

STATEMENT OF PROBLEM. Recently Yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) has been introduced due to superior flexural strength and fracture toughness compared to other dental ceramic systems. Although zirconia has outstanding mechanical properties, the phenomenon of decrease in the life-time of zirconia resulted from degradation in flexural strength after low temperature aging has been reported. PURPOSE. The objective of this study was to investigate degradation of flexural strength of Y-TZP ceramics after various low temperature aging treatments and to evaluate the phase stability and micro-structural change after aging by using X-ray diffraction analysis and a scanning electron microscope (SEM). MATERIAL AND METHODS. Y-TZP blocks of Vita In-Ceram YZ (Vita Zahnfabrik, Bad $S\ddot{a}ckingen$, Germany) were prepared in 40 mm (length) $\times$ 4 mm (width) $\times$ 3 mm (height) samples. Specimens were artificially aged in distilled water by heat-treatment at a temperature of 75, 100, 125, 150, 175, 200, and $225^{\circ}C$ for 10 hours, in order to induce the phase transformation at the surface. To measure the mechanical property, the specimens were subjected to a four-point bending test using a universal testing machine (Instron model 3365; Instron, Canton, Mass, USA). In addition, X-ray diffraction analysis (DMAX 2500; Rigaku, Tokyo, Japan) and SEM (Hitachi s4700; Jeol Ltd, Tokyo, Japan) were performed to estimate the phase transformation. The statistical analysis was done using SAS 9.1.3 (SAS institute, USA). The flexural strength data of the experimental groups were analyzed by one-way analysis of variance and to detect statistically significant differences ($\alpha$= .05). RESULTS. The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below $125^{\circ}C$ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above $150^{\circ}C$, the flexural strength started to decrease. Although low temperature aging caused the tetragonal-to-monoclinic phase transformation related to temperature, the minimum flexural strength was above 700 MPa. CONCLUSION. The monoclinic phase started to appear after aging treatment above $100^{\circ}C$. With the higher aging temperature, the fraction of monoclinic phase increased. The ratio of monoclinic/tetragonal + monoclinic phase reached a plateau value, circa 75% above $175^{\circ}C$. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.

• Journal of Powder Materials
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• v.14 no.5
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• pp.309-314
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• 2007

Zirconia powders with nano size pores and high specific surface areas were synthesized via aqueous precipitation and hydrothermal synthetic method using $ZrOCl_28H_2O$ and $NH_4OH$ under pH=11 and ambient condition. By this reaction. zirconia hydrate $(ZrO_x(OH)_{4-2x})$ was primarily synthesized and the obtained zirconia hydrate was heat treated hydrothermally using an autoclave at various temperatures under pH=11. X-ray diffraction, Scanning electron microscopy, Energy dispersive X-ray spectroscopy, FT-IR, Raman, Particle size analysis, DTA-TG, and BET techniques were used for the characterization of the powder. The synthesized zirconia showed an amorphous phase, however, the phase was transformed to the crystalline state during the hydrothermal process. The observed crystalline phase above $160^{\circ}C$ was a mixed phase of monoclinic and tetragonal zirconia. By the BET analysis, it was found that the specific surface area was ranged in $126{\sim}276m^2/g$ and the zirconia had the cylindrical shaped pores with average diameter of $2{\sim}7nm$.