• Journal of the Korean Ceramic Society
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• v.33 no.6
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• pp.637-644
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• 1996

Phase stability and isothermal phase transformation during gaging at 25$0^{\circ}C$ were investigated in yttria stabilized zirconia powders prepared from hydrolysis of zirconium isopropoxide. The stability of tetragonal phase at room temperature in zirconia powder was decreased with calcination temperature but increased with the addition of yttria content. During aging at 25$0^{\circ}C$ in humid atmosphere isothermal phase transformation occurred in tetragonal zirconia powder stabilized by constraint effect not by alloying effect and grain size effect. Many twins and microcrackings were found in transformed monomlinic zirconia particles.

• Korean Journal of Materials Research
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• v.20 no.7
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• pp.379-384
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• 2010

The usual ceramic process of mixing and milling in state of oxides $ZrO_2$ and $CeO_2$ was adopted in this study in a wet process to manufacture Ce-TZP. $CeO_2$-$ZrO_2$ ceramics containing 8~20 mol% $CeO_2$ were made by heat treatment at $1250\sim1500^{\circ}C$ for 5hr. The maximum dispersion point of every slurry manufactured with a mixture of $ZrO_2$ and $CeO_2$ was neat at pH10. A stable slurry with average particle size of 90 nm can be manufactured when it is dispersed with the use of ammonia water and polycarboxylic acid ammonium. The sintered Ce-TZP ceramics manufactured with the addition of $CeO_2$ in a concentration of less than 10 mol% progressed to the fracture of the specimen due to the existence of a monoclinic phase of more than 30% at room temperature. More than 99% of the tetragonal phase was created for the sintered body with the addition of $CeO_2$ beyond 18 mol%, but the degradation of the mechanical properties on the entire specimen was brought about due to the $CeO_2$ existing in a percentage above 3%. Consequently, the optimal Ce-TZP level combined in the oxide state was identified to be 16 mol% of $CeO_2$ contents.

• Journal of the Korean Ceramic Society
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• v.39 no.11
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• pp.1055-1062
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• 2002

The phase stability and the Low Temperature Degradation(LTD) mechanism of Tetragonal Zirconia Polycrystals(TZP), sintered specimens of $Y_2O_3$-Stabilized Zirconia(2Y-TZP), doped with trivalent cations, were evaluated by investigating meachnical properties, Raman spectra, lattice parameter variation and the oxygen vacancy behavior under applied electric field. XRD observation was put forward on 2Y-TZP doped with trivalent cation whose ionic radii were larger than $Zr^{4+}(Sc^{3+},\;Yb^{3+},\;Y^{3+},\;Sm^{3+},\;Nd^{3+},\;La^{3+})$ up to 2 mol% and sintered at 1500 h for 1h. For $La^{3+}$ doping, the stability of tetragonal phase was degraded due to the formation of the pyrochlore phase $(La_2Zr_2O_7)$ as the dopant content increased above exceeded 0.5 mol%. As the dosage increased, tetragonal phase maintained for the case of $Sc^{3+}$, whose radius was similar to $Zr^{4+}$, on the other hand, the cubic phase was formed for the cases of $Yb^{3+},\;Y^{3+},\;Sm^{3+},\;Nd^{3+}$. As the radii of dopant cation increased, c/a ratio increased and it was experimentally observed that the amount of monoclinic phase decreased when the specimens were annealed at $220{\circ}C$ for 500 h.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.55-85
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• 1996

지르코니아 분말은 ZrO2 결정상이 온도변화에 따라 부피변화를 수반하는 상전이변태를 나타낸다. 단사정 ZrO2가 110$0^{\circ}C$에서는 정방정으로, 2$700^{\circ}C$ 내외에서는 입방정으로 결정구조가 가역적으로 변한다. 이 ZrO2에 금속산화물을 고용시키면 형석 (CaF2:Florite)형의 입방정 결정구조가 실온에서도 안정하게 존재하게 된다. 안정화제 산화물은 caO, MgO등 2가 산화물외에 3가 또는 4가의 금속산화물로서 Sc2O3, Y2O3, Sm2O3, Nd2O3, Gd2O3, Y2O3, CeO2 등이며 이들은 금속이온의 원자가가 변하기 쉬운 희토류 산화물이다. 안정화 지르코니아는 형석형 결정구조이며 결정화학적으로 보면 금속양이온이 산소이온에 대해서 정육면체형의 8배위를 하고 있다. 이때 이온반경비(양이온/음이온)에 따라 Zr+4자리와 O-2자리의 격자위치와 모양이 형성되므로 비틀어진 정육면체구조이건 이상적인 정육면체 형석구조를 이룬다. 이는 지르코니아의 결정상의 2상-3상인 부분안정화 지르코니아다결정체(PSZ : partially stabilized zirconia)이거나 단일상-2상인 정방정 지르코니아다결정체(TZP : tetragonal zirconia polycrystal)의 결정구조를 가지는데 기인한다. PSZ는 주로 MgO, CaO를 안정화제로 고용시켜 입방정 영역에서 소결하고 이를 다시 입방정과 정방정의 상 영역에서 열처리하여 입방정 입자내부에 정방정을 석출 형성시킨 것이며 TZP는 Y2O3 및 CeO2를 고용시켜 PSZ와 다르게 일반적인 상압소결한 정방정 결정상의 미립자이다. 산화지르코늄 분말은 지르콘사에서 열분해시킨 지르코늄소결.융해괴(caustic fusion clinker)를 산처리하여얻어진 지르코늄산용액(zirconyl acid solution : cloride, sulfide, nitride 등)으로부터 제조된다. 고순도 산화지르코늄은 용액 결정석출법에 의해 ZrOCl2.8H2O, 5ZrO2.3SO3.15H2O, ZrO(NO3)2.xH2O 등의 지르코늄 수화물만을 재결정화시킨 것으로부터 얻을 수 있으며 이 지르코늄염 수용액으로부터 입자미세구조를 효과적으로 제어하여 산화지르코늄 및 안정화 지르코니아 분말제조가 가능하다. 안정화 지르코니아 분말은 ZrO2와 안정화산화물의 고용을위하여 가열처리를 필요로 하며 일정온도에서 최적상태로 숙성하므로서 2가지 상(phase) 이상의 고용체를 가지게 된다. 안정화 지르코니아 분말은 고용처리온도를 낮추고 효과적으로 생성시키기 위해서는 지르코늄 및 안정화제염을 혼합하고 습식 직접합성하여 저온에서 고용체의 합해진상 영역을 생성시키는 것이다. 이는 지르코니아 원료분말의 미세구조를 제어하므로서 가능하며 이때 화학성분조성과 크기형태가 균일하게 분포된 입자분말을 얻을 수 있다.

• Journal of the Korean Ceramic Society
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• v.55 no.4
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• pp.337-343
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• 2018

The influence of solid loading in the slurry composition on the morphology of 3Y-TZP granules fabricated by two-fluid spray drying was investigated for solid contents varying between 30 wt% and 50 wt%. The resulting 3Y-TZP granules showed a sphere-like shape with diameters of $40-70{\mu}m$. However, a donut-like shape and a few cracks were observed on the granule surfaces fabricated using the slurry with 50 wt% solid content. The green density after cold isostatic pressing at 200 MPa was $2.1-2.2g/cm^3$, and a homogeneous fracture surface was obtained by complete destruction of granules. After sintering at $1500^{\circ}C$ for 2 h, all specimens had relative densities of 96.2 - 98.3%. With increasing solid content, the relative density decreased from 98.3% to 96.2%, but the grain size increased from $0.3{\mu}m$ to $0.6{\mu}m$. Highly sinterable zirconia granule powder could be obtained by controlling the slurry composition.

• The Journal of Advanced Prosthodontics
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• v.13 no.6
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• pp.385-395
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• 2021

PURPOSE. To characterize the microstructure of three yttria partially stabilized zirconia ceramics and to compare their hardness, indentation fracture resistance (IFR), biaxial flexural strength (BFS), and fatigue flexural strength. MATERIALS AND METHODS. Disc-shaped specimens were obtained from 3Y-TZP (Vita YZ HT), 4Y-PSZ (Vita YZ ST) and 5Y-PSZ (Vita YZ XT), following the ISO 6872/2015 guidelines for BFS testing (final dimensions of 12 mm in diameter, 0.7 and 1.2 ± 0.1 mm in thicknesses). Energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses were performed, and mechanical properties were assessed by Vickers hardness, IFR, quasi-static BFS and fatigue tests. RESULTS. All ceramics showed similar chemical compositions, but mainly differed in the amount of yttria, which was higher as the amount of cubic phase in the diffractogram (5Y-PSZ > 4Y-PSZ > 3Y-TZP). The 4Y- and 5Y-PSZ specimens showed surface defects under SEM, while 3Y-TZP exhibited greater grain uniformity on the surface. 5Y-PSZ and 3Y-TZP presented the highest hardness values, while 3Y-TZP was higher than 4Y- and 5Y-PSZ with regard to the IFR. The 5Y-PSZ specimen (0.7 and 1.2 mm) showed the worst mechanical performance (fatigue BFS and cycles until failure), while 3Y-TZP and 4Y-PSZ presented statistically similar values, higher than 5Y-PSZ for both thicknesses (0.7 and 1.2 mm). Moreover, 3Y-TZP showed the highest (1.2 mm group) and the lowest (0.7 mm group) degradation percentage, and 5Y-PSZ had higher strength degradation than 4Y-PSZ group. CONCLUSION. Despite the microstructural differences, 4Y-PSZ and 3Y-TZP had similar fatigue behavior regardless of thickness. 5Y-PSZ had the lowest mechanical performance.

• Korean Journal of Materials Research
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• v.23 no.4
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• pp.250-254
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• 2013

In order to increase the toughness of ZTA(zirconia toughened alumina) ceramics, the present study focused on rearrangement and densification of particles according to the particle size of the parent material. When rough alumina was used for production of ZTA, densification behavior was observed in the specimen sintered at a temperature over $1550^{\circ}C$. However, it was found that the densification behavior was occurred in the specimen sintered at $1450^{\circ}C$ when fine alumina powder was used. High relative density exceeding 98% was obtained when fine alumina powder was mixed with 15 wt% of 3Y-TZP and sintered at $1600^{\circ}C$. Also, a hardness of 1820.2 Hv was obtained when a specimen containing 10 wt% of 3Y-TZP was sintered at $1600^{\circ}C$. In the case of 3Y-TZP containing rough alumina powder that had been sintered the hardness value was around 1720.3 Hv. It was predicted that an improved toughening effect in ZTA could be achieved by using finer alumina powder as the parent material.

• Journal of the Korean Ceramic Society
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• v.37 no.2
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• pp.174-180
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• 2000

Y-TZP/mullite composites were prepared by the infiltration of Y-TZP precursor into partially reaction-sintered mullite. The addition of Y-TZP(~7.2 wt%) increased the bend strength(207 MPa), fracture toughness(4.6MPa.m1/2) and Vickers microhardness(853kg/$\textrm{mm}^2$) of the uninfiltrated mullite sintered at 162$0^{\circ}C$ for 10h by more than 75, 70 and 105%, respectively. Residual alumina-rich glass was observed at a mullite/mullite junction, due to the mullitization reaction of silica melt with crystalline $\alpha$-Al2O3 during a final sintering. Although ZrO2 inclusions improved the final sintered density of mullite they did not effectively prevent its grain growth.

• Journal of the Korean Ceramic Society
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• v.56 no.1
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• pp.37-48
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• 2019

The objective of this research is to analyze the fracture toughness of pure and silica co-doped yttria-stabilized tetragonal zirconia polycrystal (3Y-TZP) bioceramics containing 0.1 and 0.2 wt.% of alumina, and sintered at a temperature of $1500^{\circ}C$. Because of the relatively easy preparation of the test specimens and the high speed of testing, the Vickers indentation fracture (VIF) technique is more frequently used to evaluate the fracture toughness of biomaterials and hard biological tissues. The Young's modulus and hardness values were obtained by means of nanoindentation and indentation methods. The fracture toughness values of 3Y-TZP bioceramics were calculated and analyzed using 15 equations related to the VIF technique, and loadings of 49.03 and 196.13 N with a Vickers diamond. For validation, the results were compared with fracture toughness values obtained by the single-edge laser-notch beam (SELNB) method with an almost atomically sharp laser-machined initial notch.

• The Journal of Advanced Prosthodontics
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• v.11 no.1
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• pp.1-6
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• 2019

PURPOSE. The purpose of this in vitro study was to evaluate the effect of surface grinding and polishing procedures using high speed zirconia diamond burs with different grit sizes on the phase transformation and flexural strength of zirconia. MATERIALS AND METHODS. Forty disc shape specimens ($15{\times}1.25mm$) with a cylindrical projection in the center of each disc ($1{\times}3mm$) were fabricated with 3Y-TZP (Prettau, Zirkonzahn, Italy). The specimens were divided into 4 groups (n=10) according to the grinding and polishing procedures: Control group - grinding (coarse-grit diamond bur), Group 1 - grinding (coarse-grit diamond bur) + polishing, Group 2 - grinding (fine-grit diamond bur) + polishing, and Group 3 - grinding (fine grit diamond bur). Each specimen was analyzed by 3D-OM, XRD analysis, and biaxial flexural strength test. RESULTS. Based on the surface morphology by 3D-OM images, polished specimens showed smoother surface and lower roughness value (Ra). In the result of XRD analysis, partial phase transformation from tetragonal to monoclinic zirconia occurred in all groups. Control group, ground with a coarse grit diamond bur, showed more $t{\rightarrow}m$ phase transformation and lower flexural strength than Groups 1 and 2 significantly. CONCLUSION. The flexural strength in all specimens after grinding and polishing showed over 500 MPa, and those were clinically acceptable. However, grinding with a coarse grit diamond bur without polishing induced the phase transformation and low strength. Therefore, surface polishing is required for the occlusal adjustment using a high speed zirconia diamond bur to reduce the phase transformation and to prevent the decrease of flexural strength of zirconia.