• Korean Chemical Engineering Research
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• 제57권1호
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• pp.133-141
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• 2019

침전법으로 환류방법 또는 수열합성법을 이용하여 산 염기점을 갖는 고비표면적 지르코니아를 합성하였다. 제조된 지르코니아는 침전제로 수산화암모늄 수용액을 사용하여 Zr 용액의 pH를 2에서 10 범위 내에서 조절하였으며 질소흡착분석, X-선 회절분석(XRD), 이소프로판올 승온탈착법(IPA-TPD), 주사전자현미경 분석, X-선 광전자분광분석, 산-염기점 분석을 통해 IPA 분해반응의 촉매활성과 연관하여 특성분석을 수행하였다. 환류방법을 사용할 시, tetragonal 상이 높은 지르코니아를 얻기 위해서는 Zr 용액의 pH가 높아야 하며, pH 9 이상에서는 순수한 tetragonal 상의 지르코니아 합성이 가능하였다. 또한, 비표면적이 큰 지르코니아를 얻기 위해서는 높은 pH가 요구되었으며, pH 10에서 합성한 경우에는 $600^{\circ}C$에서 소성 후에도 $260m^2g^{-1}$의 높은 비표면적이 얻어졌다. 하지만 같은 조건 하에서 고압이 수반되는 수열합성에는 $40m^2g^{-1}$ 이하의 매우 낮은 비표면적을 보였으며, monoclinic 상의 지르코니아가 합성되었다. 고 비표면적 tetragonal 상의 지르코니아를 얻기 위해서는 용액의 pH가 가장 큰 영향을 미쳤으며, 용액의 pH와 무관하게 높은 압력이 필요한 수열합성에서는 monoclinic 지르코니아가 생성되었으며 상대적으로 비표면적이 낮게 나타났다. 높은 비표면적과 tetragonal 상을 갖는 지르코니아는 염기점에 비해 산점이 우세하여 IPA 분해반응에서 선택적 탈수반응만 진행되는 프로필렌만 생성되었다.

• 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.

• 대한치과기공학회지
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• 제42권4호
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• pp.307-312
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• 2020

Application of ceramic materials for fabrication of dental restoration materials has been a focus of interest in the field of esthetic dentistry. The ceramic materials of choice are glass ceramics, spinel, alumina, and zirconia. The development of yttrium tetragonal zirconia polycrystal (YTZP)-based systems is a recent addition to all-ceramic systems that have high strength and are used for crowns and fixed partial dentures. Computer-aided design/computer-aided manufacturing (CAD/CAM)-produced, YTZP-based systems are popular with respect to their esthetic appeal for use in stress-bearing regions. The highly esthetic nature of zirconia and its superior physical properties and biocompatibility have enabled the development of restorative systems that meet the demands of today's patients. Many in vitro trials have been performed on the use of zirconia; however, relatively fewer long-term clinical studies have been published on this subject. The use of zirconia frameworks for long-span fixed partial dentures is currently being evaluated; in the future, more in vivo research and long-term clinical studies are required to provide scientific evidence for drawing solid guidelines. Further clinical and in vitro studies are required to obtain data regarding the long-term clinical use of zirconia-based restorations.

• 한국분말재료학회지
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• 제17권3호
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• pp.197-202
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• 2010

Low temperature degradation behavior in yttria stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics was microscopically observed from the phase contrast between monoclinic surface and tetragonal matrix. The degradation behavior was dependent on the surface treatment of sintered Y-TZP, even if the sintering history is same. In the mirror polished specimen, the monoclinic layer appeared in a uniform thickness from the surface. On the contrary, for the specimen with coarse scratch, the thickness of degraded surface was more than double especially from the coarse scratch. Since the scratch results in local deformation, the residual stress should be induced around the scratch. With the transformation from tetragonal to monoclinic, the volume expansion exerts a stress on a neighboring grains and promotes a successive phase transformation. Such a autocatalytic effect can be triggered from the part of coarse scratch.

• 한국세라믹학회지
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• 제31권9호
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• pp.1060-1068
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• 1994

Stable zirconia sol was prepared from zirconium butoxide Zr(OC4O9)4 as a precursor and ethylacetoacetate(EAcAc) or diethylene glycol(DEG) as a chelating agent under ambient agent under ambient atmosphere by Sol-Gel process. The sythesized sol was coated on 304 stainless steel substrate by dip coating, thereafter zirconia film could be obtained by heat-treatment at $600^{\circ}C$. The characteristics of coating film were determined by FT-IR, XRD, and ellipsometion peak represented Zr-O-Zr bonding of tetragonal phase was shown at 470cm-1. Crystallization of zirconia gel and film from amorphous state to tetragonal phase started at 40$0^{\circ}C$, and then transformed into monoclinic phase around $700^{\circ}C$. Zirconia film coated on 304 stainless steel substrate showed relatively low porosity of 16% when it was coated with 0.4M zirconia sol and thereafter heat-treated at 80$0^{\circ}C$ and the film was densified continuously up to 90$0^{\circ}C$. The zirconia film of 10 nm thick acted as a protective layer against oxidation up to $700^{\circ}C$.

• 센서학회지
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• 제18권6호
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• pp.441-448
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• 2009

Magnesia partially stabilized zirconia(Mg-PSZ) solid electrolytes for an improvement of thermal shock resistance, which is suitable for the measurement of oxygen activity in a molten steel, were prepared by post-thermal aging treatment. The steelmaking oxygen sensor elements were formed by an injection molding method, sintered at $1650^{\circ}C$, and then thermal aged ranged from 1250 to $1400^{\circ}C$. Sintered density and porosity were decreased as increasing the magnesia content in a zirconia-magnesia solid solution. Fractions of cubic phase to the synthesized Mg-PSZ solid electrolytes were ranged from 13.13 to 79.54.% after post-thermal aging treatment. Very dense microstructure without voids in the grains was obtained by the post-thermal aging process. Fine tetragonal phase crystallites precipitated on the cubic surface during post-thermal aging up to $1300^{\circ}C$ improve a thermal shock resistance and reappearance of electro motive force(EMF) curve.

• 대한치과기공학회지
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• 제33권1호
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• pp.15-23
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• 2011

Purpose: Thy yttria tetragonal zirconia polycrystalline(Y-TZP) is a good structural ceramic for dental restoration. But it have a problem that delamination of veneering ceramic from the Y-TZP core materials. The problem generally occur at the interface, thus this study was conducted to evaluate the interface of Y-TZP using scanning electron microscopy(SEM). Methods: To investigate this aspect, high-resolution SEM observations were made of polished and etched (HF content gel) cross-sections of the interface area. Dry and moist veneering porcelain powders were built up on the zirconia base. Results: The extent of this surface faceting is dependent upon the moisture content of the porcelain powder and the firing temperature. More moisture and higher final heating temperature accelerates the observed faceting of the Y-TZP grains at the interface to the veneering ceramic. Conclusion: These changes of the Y-TZP grains indicate that destabilization of the tetragonal phase of zirconia occurs at the interface during veneering with ceramic. It may result in a reduction of the stability of the zirconia and interface.

• The Korean Journal of Ceramics
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• 제4권4호
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• pp.297-303
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• 1998

The effect of aliovalent dopants, $ Nb_2O_5$ and MnO, on the phase stability of 12 mol% ceria partially-stabilized zirconia (Ce-TZP) polycrystals was studied. Both dopants (MnO and $ Nb_2O_5$) significantly increased the stability of the tetragonal zirconia phase (Mb temperature lower than liquid nitrogen temperature). The enhancement of the stability of the tetragonal phase in Ce-TZP doped with 1 mol% of Mno(Ce-TZP/MnO) andCe-TZP doped with 1 mol% of $ Nb_2O_5$(Ce-TZP/$ Nb_2O_5$) were explained by the significant reduction of the driving force, -${\Delta}$Gchem, for the tetragonal-to-mono-clinic phase transformation caused by the addition of MnO and $ Nb_2O_5$. The enhanced stability of the tetragonal phase in the Ce-TZP and Al2O3 composite (Ce-TZP/$Al_2O_3$) is believed to be caused by smaller grain size, moderate reduction in the chemical driving force and increase in the strain energy barrier to the transformation. Mechanical properties of the Ce-TZP and the Ce-TZP/$Al_2O_3$ with (i) the same grain size and (ii) the same Mb temperature were examined by measuring stress-strain behavior in 3 point bending. The Ce-TZP/$Al_2O_3$ composite doped with 1.3w% MnO (Ce-TZP/$Al_2O_3$/MnO), which had the same grain size as the Ce-TZP and De-TZP/$Al_2O_3$ showed more transformation plasticity than either the Ce-TZP or the Ce-TZP/$Al_2O_3$ composite. The Ce-TZP wihch had the same Mb temperature as that of the Ce-TZP/$Al_2O_3$/MnO did not show any transformation plasticity.

• 한국세라믹학회지
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• 제26권5호
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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.