• 한국세라믹학회지
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• 제41권2호
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• pp.111-117
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• 2004

고순도 3Y-TZP에 알루미나를 0.3∼l.2wt%까지 첨가하여 attrition milling을 하고 slip-casting하여 시료를 제조하였다. 1390∼151$0^{\circ}C$까지 열처리하여 소결체의 소결특성을 기제적 물성과 미세구조 분석을 통하여 확인하였다. XRD를 이용하여 monoclinic-ZrO$_2$의 생성량을 정량적으로 확인하였으며, 147$0^{\circ}C$ 이장에서 열처리한 시료의 경우 m-ZrO$_2$의 생성으로 밀도의 저하를 보였으며, 비정상 입자성장을 유발하여 경도가 저하되었다. 알루미나의 첨가량이 0.9wt% 미만, 열처리 온도143$0^{\circ}C$에서 microhardness가 1360Hv 이상의 소결체를 제조할 수 있었다.

• 한국세라믹학회지
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• 제38권7호
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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.

• 한국세라믹학회지
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• 제47권4호
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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.

• 공업화학
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• 제25권6호
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• pp.564-569
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• 2014

지르코니아 나노분말을 수열합성법으로 제조하였으며, 반응온도, 반응시간, 침전제의 종류 및 농도, 전구체의 종류를 실험 변수로 하였고, 각각의 제조된 분말을 X-선 회절(XRD)과 주사전자현미경(FE-SEM)을 통해 입자크기 및 결정상을 측정하였다. 침전제의 농도 증가에 따라 지르코니아 입자크기가 증가하였으며, 입자의 결정화도도 높아졌고, KOH 보다 NaOH 침전제를 사용하였을 경우, 입자 성장 속도가 증가하였다. 이는 입자의 크기 컨트롤에 있어 NaOH를 사용하는 경우보다 KOH를 사용하는 것이 더 효과적이었다. 4 h의 수열반응시간에서는 4 h의 수열반응시간에서는 비정질의 지르코니아 입자가 발견되었지만, 8 h 이상 합성 시, 단사정상의 지르코니아 입자가 생성됨을 확인하였고, 반응시간이 길어짐에 따라 지르코니아 입자의 폭이 소폭으로 줄어들고, 길이는 소폭 늘어남을 확인하였다. 동일한 합성 조건에서 전구체로서 zirconium (IV) acetate, zirconium nitrate, zirconium chloride 중에서 zirconium chloride를 사용하여 합성하였을 경우, 입자의 크기가 가장 작게 형성되었다.

• 대한치과의사협회지
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• 제49권5호
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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.

• 한국세라믹학회지
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• 제45권2호
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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.

• 한국세라믹학회지
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• 제20권4호
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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.

• 한국세라믹학회지
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• 제20권3호
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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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• 제1권3호
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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%.

• 한국분말재료학회지
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• 제14권5호
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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 $2{\sim}7nm$.