• Title/Summary/Keyword: Monoclinic zirconia

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Fabrication of Crystalline $ZrO_2$ Nanotubes by ALD

  • Kim, Hyeon-Cheol;Panda, Sovan K.;Yu, Hyeon-Jun;Kim, Myeong-Jun;Yang, Yun-Jeong;Lee, Seon-Hui;Sin, Hyeon-Jeong
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.241.1-241.1
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    • 2011
  • Numerous possible applications for $ZrO_2$ nanotubes exist such as for catalyst support structures, for sensing or for applications as a solid state electrolyte. Especially, because of a large specific surface area, high efficiency for solid oxide fuel cell (SOFC) application at low temperature can be expected for nanotublar structures in even small size. A zirconium precursor, Tetrakis (ethylmethylamino) zirconium, TEMAZr and $H_2O$ oxidant were used to deposit$ZrO_2$ thin films on an anodized aluminum oxide (AAO) templates having sub-100nm cylindrical pores by atomic layer deposition (ALD) in the temperature range of 150~250$^{\circ}C$. The crystalline structures of as-prepared and post-annealed $ZrO_2$ nanotubes were characterized by x-ray diffraction and high-resolution transmission electron microscopy. The as-prepared samples at $150^{\circ}C$ and $200^{\circ}C$ were showed amorphous, whereas a mixed phase of tetragonal, monoclinic and amorphous polymorph was observed at $250^{\circ}C$. In the bulk, zirconia remains monoclinic phase up to $1,175^{\circ}C$, however, $ZrO_2$ nanotubes were showed tetragonal phase upon post thermal treatments merely at $400^{\circ}C$. This trend may be indicative of high-curvature surfaces of nanotubes and thereby the presence of intrinsic compressive strain. The amount of amorphous structures in the mixed phase as well as as-grown $ZrO_2$ nanotubes were also gradually decreased by subsequent heat treatment.

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Analysis of Monoclinic Phase Change and Microstructure According to High-temperature Heat Treatment of Oxide-doped YSZ (산화물이 Doping된 YSZ의 고온 열처리에 따른 Monoclinic 상변화 및 미세구조 분석)

  • Gye-Won, Lee;Yong-Seok, Choi;Chang-Woo, Jeon;In-Hwan, Lee;Yoon-Suk, Oh
    • Journal of Powder Materials
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    • v.29 no.6
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    • pp.468-476
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    • 2022
  • Yttria-stabilized zirconia (YSZ) has a low thermal conductivity, high thermal expansion coefficient, and excellent mechanical properties; thus, it is used as a thermal barrier coating material for gas turbines. However, during long-time exposure of YSZ to temperatures of 1200℃ or higher, a phase transformation accompanied by a volume change occurs, causing the YSZ coating layer to peel off. To solve this problem, YSZ has been doped with trivalent and tetravalent oxides to obtain coating materials with low thermal conductivity and suppressed phase transformation of zirconia. In this study, YSZ is doped with trivalent oxides, Nd2O3, Yb2O3, Al2O3, and tetravalent oxide, TiO2, and the thermal conductivity of the obtained materials is analyzed according to the composition; furthermore, the relative density change, microstructure change, and m-phase formation behavior are analyzed during long-time heat treatment at high temperatures.

Preparation and Properties of Zirconia-based Electrolytes from m-Zirconia and Yag Sol (m-지르코니아와 Yag 졸로부터 지르코니아계 전해질 제조 및 물성)

  • Kang, Keon-Taek;Han, Kyoung R.;Nam, Suk-Woo;Kim, Chang-Sam;Lee, Young-Soo;Yoo, Han-Ill
    • Journal of the Korean Ceramic Society
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    • v.38 no.9
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    • pp.834-838
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    • 2001
  • Attempts were made to improve mechanical properties of zirconia-based electrolyte by preparing yttria-stabilized cubic zirconia/alumina composite. It was performed by precipitating Yag precursor in aqueous m-zirconia slurry. The powder was separated and then followed by heat treatment with expecting yttria to react with m-$ZrO_2$ to give yttria stabilized zirconia and alumina to be dispersed homogeneously. When 17.8wt% Yag(6.3mol% $Y_2O_3$) was used, fracture toughness and strength were substantially improved from 1.44MPa${\cdot}m^{1/2}$ and 270Mpa for YZ8Y to 3.62MPa${\cdot}m^{1/2}$ and 447MPa respectively, but electrical conductivity at $^{\circ}$C in air was decreased from 0.126 to 0.057${\Omega}^{-1}cm^{-1}$. It seemed due to the presence of small amount of tetragonal zirconia. But when 21.58wt% Yag(8.0mol% $Y_2O_3$) was added, fracture toughness of 2.93MPa${\cdot}m^{1/2}$ and flexural strength of 388MPa were obtained with electrical conductivity of ${\Omega}^{-1}cm^{-1}$.

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Preparation of Zirconia Nanocrystalline Powder by the Hydrothemal Treatment at low Temperature (수열법에 의한 저온 결정형 지르코니아 나노 분말의 제조)

  • Noh, Hee-Jin;Lee, Jong-Kook;Seo, Dong-Seok;Hwang, Kyu-Hong
    • Journal of the Korean Ceramic Society
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    • v.39 no.3
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    • pp.308-314
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    • 2002
  • The nanocrystalline zirconia powder was synthesized from the zirconium hydroxide precipitate by hydrothermal process with the reaction temperature range 100∼250$^{\circ}$C, reaction time 1∼48 hours and additive concentration 1, 5 N NaOH solutions. The lower hydrothermal treatment temperature, the inner spherical tetragonal zirconia was synthesized. The fraction of monoclinic phase zirconia with rod shape increased with increasing the hydrothermal treatment temperature. As the concentration of the NaOH solution increases, the synthesized particle in breadth and length increased; breadth and length ratio decreased. In the case of the low concentration of NaOH solution, however, the particle length became relatively larger than its breadth resulting in the rod-shaped particles with bigger aspect ratio.

Analysis of Attrition Rate of Y2O3 Stabilized Zirconia Beads with Different Microstructure and Mechanical Properties (고에너지 분쇄 매체 지르코니아 Beads의 미세구조 및 기계적 특성에 따른 마모율 분석)

  • Kim, Jung-Hwan;Yoon, Sae-Jung;Hahn, Byung-Dong;Ahn, Cheol-Woo;Yoon, Woon-Ha;Choi, Jong-Jin
    • Korean Journal of Materials Research
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    • v.28 no.6
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    • pp.349-354
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    • 2018
  • Particle size reduction is an important step in many technological operations. The process itself is defined as the mechanical breakdown of solids into smaller particles to increase the surface area and induce defects in solids, which are needed for subsequent operations such as chemical reactions. To fabricate nano-sized particles, several tens to hundreds of micron size ceramic beads, formed through high energy milling process, are required. To minimize the contamination effects during high-energy milling, the mechanical properties of zirconia beads are very important. Generally, the mechanical properties of $Y_2O_3$ stabilized tetragonal zirconia beads are closely related to the mechanism of phase change from tetragonal to monoclinic phase via external mechanical forces. Therefore, $Y_2O_3$ distribution in the sintered zirconia beads must also be closely related with the mechanical properties of the beads. In this work, commercially available $100{\mu}m-size$ beads are analyzed from the point of view of microstructure, composition homogeneity (especially for $Y_2O_3$), mechanical properties, and attrition rate.

Comparison of the optical properties of pre-colored dental monolithic zirconia ceramics sintered in a conventional furnace versus a microwave oven

  • Kim, Hee-Kyung;Kim, Sung-Hun
    • The Journal of Advanced Prosthodontics
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    • v.9 no.5
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    • pp.394-401
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    • 2017
  • PURPOSE. The purpose of this study was to compare the optical properties of pre-colored dental monolithic zirconia ceramics of various thicknesses sintered in a microwave and those in a conventional furnace. MATERIALS AND METHODS. A2-shade of pre-colored monolithic zirconia ceramic specimens ($22.0mm{\times}22.0mm$) in 3 thickness groups of 0.5, 1.0, and 1.5 mm were divided into 2 subgroups according to the sintering methods (n=9): microwave and conventional sintering. A spectrophotometer was used to obtain CIELab color coordinates, and translucency parameters and CIEDE2000 color differences (${\Delta}E_{00}$) were measured. The relative amount of monoclinic phase ($X_m$) was estimated with x-ray diffraction. The surface topography was analyzed by atomic force microscope and scanning electron microscope. Statistical analyses were conducted with two-way ANOVA (${\alpha}=.05$). RESULTS. There were small interaction effects on CIE $L^*$, $a^*$, and TP between sintering method and thickness (P<.001): $L^*$ (partial eta squared ${{\eta}_p}^2=0.115$), $a^*$ (${{\eta}_p}^2=0.136$), and TP (${{\eta}_p}^2=0.206$), although higher $b^*$ values were noted for microwave sintering regardless of thickness. Color differences between two sintering methods ranged from 0.52 to 0.96 ${\Delta}E_{00}$ units. The $X_m$ values ranged from 7.03% to 9.89% for conventional sintering, and from 7.31% to 9.17% for microwave sintering. The microwave-sintered specimen demonstrated a smoother surface and a more uniform grain structure compared to the conventionally-sintered specimen. CONCLUSION. With reduced processing time, microwave-sintered pre-colored dental monolithic zirconia ceramics can exhibit similar color perception and translucency to those by conventional sintering.

A Study on the Improvement of Oxidation and Corrosion Resistance of Stainless Steel by Sol-Gel Ceramic Coating (II); Effect on Oxidation and Corrosion REsistance of $CeO_2$ Stabilized Zirconia Thin Film (졸-겔 세라믹 코팅에 의한 스테인레스강의 내산화 및 내식성 향상에 관한 연구 (II);$CeO_2$ 안정화 지르코니아 박막의 내산화 및 내식성 효과)

  • 이재호;우일기;김병호
    • Journal of the Korean Ceramic Society
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    • v.32 no.1
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    • pp.95-105
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    • 1995
  • Ceria(CeO2) stabilized zirconia(CeSZ) sol was synthesized with zirconium n-butoxide Zr(OC4H9)4 and cerium nitrate hexahydrate Ce(NO3)3.6H2O as precursors and ethylacetoacetate(EAcAc) as a chelating agent under atmosphere. CeSZ films were deposited on AISI 304 stainless steel using the prepared polymeric sol by dipcoating and the coating characteristics were investigated by XRD, ellipsometry, scratch test and SEM. The CeSZ film began to crystallize from amorphous to tetragonal phase at 40$0^{\circ}C$ and it was not converted into monoclinic phase up to 100$0^{\circ}C$ by the addition of 16mol% CeO2 as a stabilizer which could suppress phase transformation of zirconia. The CeSZ films were prepared by varying the EAcAc contents and the cncentration of CeSZ sol and measured the thickness and refractive index. From these results, it was found that the EAcAc contents and concentration of CeSZ coating sol evidently affect the densification of CeSZ film. The CeSZ film coated with 0.4M CeSZ sol and heat-treated at $600^{\circ}C$ for 10min had thickness of 50nm and 17% porosity. The CeSZ film on 304 stainless steel effectively acted as a protective layer against oxidation up to 80$0^{\circ}C$ and had superior corrosion resistance in 25% H2SO4 solution for 4.5 hrs.

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Effect of Transition Metal Oxides Addition on Yttria - stabilized Zirconia for improving Physical and Mechanical Properties

  • Park, Jaesung;Lee, Yeongshin
    • Journal of Korea Society of Digital Industry and Information Management
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    • v.12 no.3
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    • pp.25-31
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    • 2016
  • Mechanical properties of Y2O3-containing tetragonal ZrO2 polycrystals(Y-TZP) were investigated. Several additives were used to modify the hardness and fracture toughness of Y-TZP. The effects of these individual additives were discussed and their interactions were also analysed. Each additive, such as CoO, Fe2O3, MnO2 was found to deteriorate the mechanical properties of Y-TZP when it was used singly. But the fracture toughness of Y-TZP was significantly improved when these additives and Al2O3 were added in combination at a certain ratio. The addition of CoO, Fe2O3 and MnO2 into Y-TZP resulted in the more complex behavior of fracture toughness and hardness. The specimen with 1.5 wt%-Fe2O3, 3.0 wt% -Al2O3 and 1.5 wt%-CoO showed the monoclinic to tetragonal phase ratio of 18% and the highest toughness of $10.8MPa{\cdot}m1/2$ with Vickers hardness of 1201 kgf/mm2. However, the toughness decreased as the ratio increased and macrocracks developed beyond the ratio of 25%. Sample No. 16 is improved high Physical and Mechanical Properties.

Fabrication and Its Characteristics of YSZ Composite with Added Transition Metal Oxides (천이금속산화물이 첨가된 YSZ 복합체의 제조 및 그 특성)

  • 최성운;박재성
    • Journal of the Institute of Electronics Engineers of Korea TE
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    • v.39 no.4
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    • pp.341-349
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    • 2002
  • Electrical, mechanical and sinterability properties of yttria-stabilized zirconia doped with 5.35wt% $Y_2$O$_3$(Y$_2$O$_3$- containing stabilized zirconia : YSZ) were studied as a function of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ addition. The ratio of monoclinic phase to tetragonal phase was changed by the addition of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ to 8.00 wt% and sintered density decreased with increasing $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ addition. Fracture toughness increased with the increase of monoclinic to tetragonal phase ratio and was maximum at about 18%. When transition metals such as CoO, Fe$_2$O$_3$ or MnO$_2$ was added more than 1.5 wt%, the electrical conductivity of YSZ increased. But $Al_2$O$_3$ hardly affected the electrical conductivity of YSZ. The addition of $Al_2$O$_3$, CoO, Fe$_2$O$_3$ and MnO$_2$ into YSZ resulted in the more complex behavior of fracture toughness and hardness variation and the specimen with 1.5wt%-Fe$_2$O$_3$, 3.0wt%-Al$_2$O$_3$ and 1.5wt%-CoO showed the monoclinic to tetragonal phase ratio of 18% and the highest toughness of 10.8 MPa.m$^{1}$2/ and Vickers hardness of 1201 kgf/mm$^2$.

Property of Sintered Y2O3-stabilized Zirconia from Scrap Powders (폐 상안정 지르코니아 분말로 제조한 소결체의 물성 연구)

  • Song, Oh-Sung;Park, Jong-Sung;Nam, Kyung-Ju
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.10 no.8
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    • pp.1783-1788
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    • 2009
  • We newly propose that we may reuse scrap powders ($Z_rO_2$+8 mol%-$Y_2O_3$) as $Y_2O_3$-stabilized zirconia (YSZ) sintered products through sintering process at 1550$^{circ}C$ for 2hrs. We also prepared the reference specimen from fresh $Z_rO_2$+30 mol%-$Y_2O_3$ powder mixture (celluar type with 1㎛-length). The reference sample showed a dense microstructure with grains of $\sim$10㎛ in diameter, while the sintered sample from scrap powder showed irregular grains of 1$\sim$30 ㎛ in diameter. Through XRD analysis, we confirmed that the reference sample has mixed phases of $Y_2O_3$(cubic), $Z_{r0.8}O_{1.9}$(cubic), and $Z_rO_2$(monoclinic), while the sintered YSZ sample from scrap powder has only tetragonal phase. Moreover, the sintered YSZ from scrap powder showed vickers hardness and apparent density more than 70 and 4.11 g/cc, which implies that it can be suitable for structural material application.