• Journal of the Korean Ceramic Society
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• v.34 no.2
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• pp.145-156
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• 1997

ZrO2 phase transformations depending on the type and amount of dopants and the sintering temperatures were studied for the 2 components (CaO-, Y2O3-, MgO-ZrO2) and the 3 components(MgO-ZrO2-Al2O3)ZrO2 powder by X-ray diffraction and Raman spectroscopy. In the CaO- and Y2O3-ZrO2 systems, as the CaO and Y2O3 contents increased to 6~15mol% and 3~15mol% respectively, we were not able to identify between tetragonal and cubic in the X-ray diffraction patterns. On the other hand, all Raman modes shifted to lower wavenumbers, decreasing in intensity and the number of bands, markedly. These phenomena were caused by tetragonallongrightarrowcubic phase transformation and interpreted by the breakdown of the wave vector selection rule(k=0) and the structural disorder associated with the formation of oxygen sublattice which was caused by the substitution between Zr4+ ion and Ca2+ or Y3+ ion in ZrO2 matrix. The monoclinic to cubic phase transformation occurred in 10mol% MgO-ZrO2 system. As the Al2O3 content increased from 0 to 20mol% in the MgO-ZrO2-Al2O3 systems, cubic phase transformed to monoclinic phase, this is because the MgO didn't play a role in a stabilizer because of the formation of the spinel(MgAl2O4) by the reaction between MgO and Al2O3, Also, the ZrO2 phase transformation was explained by the change of it's lattice parameters depending on the type and amount of dopants. Namely, as the amount of dopant increased to 10~13mol%, the axial ra-tio c/a came close to unity with increasing the lattice parameter a and decreasing the lattice parameter c. At that time, the tetragonallongrightarrowcubic phase transformation occurred.

• Journal of the Korean Ceramic Society
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• v.45 no.3
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• pp.167-171
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• 2008

Zirconium-doped $Li_{1.1}Co_{1-x}Zr_xO_2(0{\leq}x{\leq}0.05)$ powders as cathode materials for lithium ion batteries were synthesized using an ultrasonic spray pyrolysis method. Cyclic voltammetry and cyclic stability tests were performed, and the changes of microstructure were observed. The solubility limit of zirconium into $Li_{1.1}CoO_2$ was less than 5 mol%, and monoclinic $Li_2ZrO_3$ phase was formed above the limit. The Zr-doping suppressed the grain growth and increased the lattice parameters of the hexagonal $LiCoO_2$ phase. The Zr-dopiong of 1mol% resulted in the best cyclic performance in the range of $3.0{\sim}4.3V$ at 1C rate (140 mA/g); the initial discharge capacity decreased from 158 mAh/g to 60 mAh/g in the undoped powder, while from 154 mAh/g to 135 mAh/g in the Zr-doped powder of 1 mol% after 30 cycles. The excellent cycle stability of Zr-doped powder was due to the low polarization during chargedischarge processes which resulted from the delayed collapse of the crystal structure of the active materials with Zr-doping.

• Journal of the Korean Ceramic Society
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• v.22 no.5
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• pp.17-22
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• 1985

This study was to make powder by coprecipitation method and spray dispersion precipitation method in $(1-x)ZrO_2-xMgO$ system to improve sinterability. As the result the specific surface area of powder prepared by spray dispersion precipitation method and coprecipitation method was above $110m^2/g$ and $10-20m^2/g$ respectively. Spray dispersion precipitation method was more effective than coprecipitation method in powder preparation.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2000.04a
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• pp.11-11
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• 2000

Large-size ceramic/metal bulk FGMs have been fabricated on a recently developed and the world's largest Spark Plasma Sintering(SPS) systems, As a part of the development program for practical production processes and machines for FGMs by SPS, the processes, mechanical properties, dimensional size and shape effects, and production machine systems were investigated. In the past, $ZrO_{2}$/TiAI, $ZrO_{2}$/Ni, $Al_{2}O_{3}$/Ti, WC/Co, WC/Co/Steel, A1/P, Polymide, Cu/Polymide, nano-composites, porous and other combinations of bulk FGMs have already been processed using SPS. However, most of the specimen sizes were small, in a range of 20 to 30mm in diameter. Recently disk-shape sintered compacts with diameters of 100 and 150 mm, and thickness of approximately 15 and 17 mm, $ZrO_{2}$(3Y)/ stainless steel FGMs were homogenous consolidated in a shorter sintering time, while maintaining high quality and repeatability by utilizing a temperature gradient sintering method. The SPS heating up and holding time totaled less than one hour. Therefore, the SPS process in expected to find increased use in the fabrication of large-size FGMs as a new industrial processing technology. This paper introduces SPS systems, the processing principles, features and the characteristies of ceramic/metal bulk FGM.

• Journal of Powder Materials
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• v.22 no.6
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• pp.413-419
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• 2015

Lanthanum zirconate, $La_2Zr_2O_7$, is one of the most promising candidates for next-generation thermal barrier coating (TBC) applications in high efficient gas turbines due to its low thermal conductivity and chemical stability at high temperature. In this study, bulk specimens and thermal barrier coatings are fabricated via a variety of sintering processes as well as suspension plasma spray in lanthanum zirconates with reduced rare-earth contents. The phase formation, microstructure, and thermo-physical properties of these oxide ceramics and coatings are examined. In particular, lanthanum zirconates with reduced rare-earth contents in a $La_2Zr_2O_7-4YSZ$ composite system exhibit a single phase of fluorite or pyrochlore after fabricated by suspension plasma spray or spark plasma sintering. The potential of lanthanum zirconate ceramics for TBC applications is also discussed.

• Journal of the Korean Ceramic Society
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• v.41 no.4
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• pp.334-339
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• 2004

Microstructures and mechanical properties of SPSed monolithic HAp, HAp-Ag, and HAp-ZrO$_2$sintered bodies were investigated by the XRD, SEM, and TEM techniques. The nano-sized HAp powders were successfully synthesized by precipitation of Ca(NO$_3$)$_2$4$H_2O$ and (NH$_4$)HPO$_4$solution. In the HAp-Ag composite, the shrinkage cavities were observed at the interfaces between HAp and large sized Ag particles due to the mismatch of their thermal expansion coefficients. However, no found the defect at the interfaces between HAp and fine-sized Ag particles. In the HAp-ZrO$_2$composite. nano-sized ZrO$_2$particles were almost dispersed at the grain boundaries of HAp phase. The fracture toughness of HAp-Ag and HAp-ZrO$_2$ composites were increased due to the plastic deformation and phase transformation mechanisms of the dispersed fine Ag and ZrO$_2$phase in the HAp matrix, respectively.

• Korean Journal of Materials Research
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• v.24 no.5
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• pp.255-258
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• 2014

Zirconium boride is an artificial or which is rarely found in the nature. $ZrB_2$ is popular in the hard material industry because it has a high melting point, excellent mechanical properties and chemical stability. There are two known methods to synthesize $ZrB_2$. The first involves direct reaction between Zr and B, and the second is by reduction of the metal halogen. However, these two methods are known to be unsuitable for mass production. SHS(Self-propagating High-temperature Synthesis) is an efficient and economic method for synthesizing hard materials because it uses exothermic reactions. In this study, $ZrB_2$ was successfully synthesized by subjecting $ZrO_2$, Mg and $B_2O_3$ to SHS. Because of the high combustion temperature and rapid combustion, in conjunction with the stoichiometric ratio of $ZrO_2$, Mg and $B_2O_3$; single phase $ZrB_2$ was not synthesized. In order to solve the temperature problem, Mg and NaCl additives were investigated as diluents. From the experiments it was found that both diluents effectively stabilized the reaction and combustion regime. The final product, made under optimum conditions, was single-phase $ZrB_2$ of $0.1-0.9{\mu}m$ particle size.

• Korean Journal of Materials Research
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• v.8 no.3
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• pp.256-262
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• 1998

산소이온전도체 13mol% CaO안정화 $ZrO_{2}$에 대한 $AI_{2}$$O_{3}$의 첨가효과를 살펴보기 위해 출발원료분말을 ($Zr_{0.87}$ $Ca_{0.13}$ O$1.87_{1-x}$ $AI_{2}$$O_{3}$)x,(x=0,0.01,0.02,0.03,0.05)와 같은 조성이 되도록 공침법으로 합성하고 $1400^{\circ}C$에서 소결시켜, $AI_{2}$$O_{3}$의 첨가에 따른 /grain size의 변화, $AI_{2}$$O_{3}$의 형태 및 존재위치, 소결밀도의 변화, 그리고 저항률의 변화를 살펴보았다. 그 결과, 결정립의 크기는 1mol% A $I_{2}$$O_{3}$첨가까지는 증가하였고, 2mol%첨가이상에서는 입계로 석출하기 시작한 $AI_{2}$$O_{3}$의 pinning효과에 기인되어 감소하였다. 또 1mol% $AI_{2}$$O_{3}$첨가시에 격자상수값의 급격한 감소가 보여지고, 그 이상에서는 변화가 별로 없어 13mol%CaO안정화 $ZnO_{2}$의 고용도한은 최대 1mol%임을 알 수 있었다. 전기전도도 또한 1mol% $AI_{2}$$O_{3}$첨가시에 증가됨을 나타냈다. $ZrO_{2}$에의 고용도한까지의 $AI_{2}$$O_{3}$첨가는 결정립성장을 촉진시키며 밀도값의 증대를 가져오고 전기전도도의 증가를 가져오는 긍정적인 효과를 나타냈다.

• Journal of Powder Materials
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• v.25 no.2
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• pp.151-157
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• 2018

In this study, the compound $Li_3BO_3$ (LBO) is intended to be prepared by a polymeric complex method as a sintering aid for the densification of $Li_7La_3Zr_2O_{12}$ (LLZ) solid electrolyte. A polymeric precursor containing Li and B is heat-treated in an air atmosphere at a temperature range between $600^{\circ}C$ and $800^{\circ}C$. Instead of LBO, the compound $Li_{2+x}C_{1-x}B_xO_3$ (LCBO) is unexpectedly synthesized after a heat-treatment of $700^{\circ}C$. The effect of LCBO addition on sintering behavior and ion conductivity of LLZ is studied. It is found that the LCBO compound could lead to significant improvements in the densification and ionic conductivity of LLZ compared to pure LLZ. After sintering at $1100^{\circ}C$, the density of the LLZ-12wt%LBO composite is $3.72g/cm^3$, with a high Li-ion conductivity of $1.18{\times}10^{-4}Scm^{-1}$ at $28^{\circ}C$, while the pure LLZ specimen had a densify of $2.98g/cm^3$ and Li-ion conductivity of $5.98{\times}10^{-6}Scm^{-1}$.

• Journal of the Mineralogical Society of Korea
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• v.30 no.3
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• pp.127-136
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• 2017

High pressure has been applied to check the pressure effect on the powdered $TiO_2$-complex, which was synthesized for ultra-violet rays cutoff and antimicrobial applications. $TiO_2$-complex consists of anatase, rutile and silver chloride. Grain size was determined to be ~34 nm. Both anatase and rutile begin structural phase transitions to $ZrO_2$ (baddeleyite)-type crystal structures at 14~16 GPa, then sustain their phases up to 22.7 GPa. Under decompression to 0.0001 GPa (ambient pressure), rutile transforms to another phase with ${\alpha}-PbO_2$ structure, while anatase retains its high pressure structure upon complete decompression. Silver chloride peaks disappear at the low pressures.