• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1998.11a
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• pp.311-314
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• 1998

The effects of the additions of transition metal oxides on ZrO$_2$ - Y$_2$O$_3$ (Y$_2$O$_3$ - containing tetragonal zirconia polycrystals : Y-TZP) system has been studied by investigating fracture toughness and phase stability of the sintered specimens. In the specimens sintered at 1450$^{\circ}C$ for 2hrs in air the phase transformation from tetragonal to monoclinic was observed. The ratios of monoclinic phase to tetragonal phase were changed with the additions of CoO, Fe$_2$O$_3$ and MnO$_2$, respectively, from 0.00 to 8.00wt%. The fracture toughness was increased with increasing the monoclinic to tetragonal phase ratio and was maximum at the ratio of about 18%. However, the hardness was decreased with increasing the ratio. The additions of CoO, Fe$_2$O$_3$ and MnO$_2$ together into Y-TZP resulted in more complex behaviors of fracture toughness and hardness. The specimen with the additions of 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$\^$$\frac{1}{2}$/ and Vickers hardness of 1201kgf/mm$^2$.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2001.07a
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• pp.211-214
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• 2001

The undesirable phase transformation of zirconium dioxide at high temperatures can be eliminated by stabilization of the cubic phase with an addition of a selected alkaline earth or rare-earth oxide. In this paper the ionic conductivity of cubic solid solutions in the stabilized ZrO$_2$ by CaO-Y$_2$O$_3$ system was examined. The higher ionic conductivity appears to be related to lower activation energy rather than to the number of oxygen vacancies dictated by composition. Those compositions of highest conductivity lie close to the cubic-monoclinic solid-solution phase boundary. Conductivity temperature data are presented that indicate a reversible order-disorder transition for Zr$_2$2-Y$_2$O$_3$cubic solid solutions containing 20 and 25 mole % $Y_2$O$_3$.

• Journal of the Korean Ceramic Society
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• v.28 no.1
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• pp.1-10
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• 1991

Zirconium dioxide(ZrO2) thin films have been deposited by chemical vapor deposition technique involving the application of gas mixture of ZrCl4, and H2O into silicon wafers. The relationships between the deposition rate and various reaction parameters such as the deposition time, the gas flow rate, the deposition temperature, and the composition of reactant gases were studied. The film was identified as nearly stoichiometric monoclinic ZrO2. The apparent activation energy is about 19Kcal/mole at surface chemical reaction controlled region. The deposition rate is mainly influenced by the H2O-forming reacting between CO2 and H2.

• Journal of the Korean Ceramic Society
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• v.20 no.3
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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.

• Journal of the Korean Ceramic Society
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• v.29 no.2
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• pp.119-126
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• 1992

3 mol% Y2O3-doped ZrO2 powders were prepared by hydrolysis with 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 mol/ιH2O/ethanol into 0.1 mol/ι zirconium and yttrium alkoside/ethanol. Spherical monodispersed yttria-partially stabilized zirconia particles with an average diameter of about 0.5 ${\mu}{\textrm}{m}$ were prepared by hydrolysis with 0.2 mol/ιH2O/ethanol. The as-prepared powder was amorphous and with heating it transformed into cubic up to 80$0^{\circ}C$ and into tetragonal over 100$0^{\circ}C$. 3 mol% Y2O3-doped ZrO2 powders calcined over and up to 80$0^{\circ}C$ were a mixture of tetragonal and monoclinic and only tetragonal as determined by X-ray diffraction, respectively.

• Journal of the Korean Ceramic Society
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• v.31 no.8
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• pp.879-885
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• 1994

Coprecipitation technique was used to synthesize ZrO2+12 mol% CeO2 powders with ZrOCl2.8H2O and Ce(NO3)3.6H2O as starting materials. The powders were dried on different conditions such as distilled water, ethanol, and azeotropic distillation. The powders prepared by azeotropic distillation showed weak aggregation of particles and the average particle size of powders calcined at 85$0^{\circ}C$ for 1 hour was 0.19 ${\mu}{\textrm}{m}$. The optimum sintering temperature and holding time are 130$0^{\circ}C$ and 2.5~10 hours, respectively. Beyond the optimum conditions, a phase transition from tetragonal to monoclinic causes to produce cracks in the sintered bodies and to decrease the density.

• Korean Journal of Materials Research
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• v.26 no.2
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• pp.95-99
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• 2016

In this study, 5 um sized $ZrSiO_4$ was ground to 1.9 um, 0.3 um, and 0.1 um sized powders by wet high energy milling process, and the sintering characteristics were observed. Pure $ZrSiO_4$ itself can-not be sintered to these levels of theoretical density, but it was possible to sinter $ZrSiO_4$ powder of nano-scale size of, -0.1 um to the theoretical density and to lower the sintering temperature for full density. Also, the decomposition of $ZrSiO_4$ with a size in the micron range resulted in the formation of monoclinic $ZrO_2$; however, in the nano sized range, the decomposition resulted in the tetragonal phase of $ZrO_2$. So, it was possible to improve the sintering characteristics of nano-sized $ZrSiO_4$ powders.

• Korean Journal of Materials Research
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• v.22 no.5
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• pp.220-226
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• 2012

Pure zirconia and $x$ mol% calcia partially stabilized zirconia ($x$ = 1.5, 3, and 8) nanopowders were synthesized by hydrothermal method with various reaction temperatures for 24 hrs. The precipitated precursor of pure zirconia and $x$ mol% calcia doped zirconia was prepared by adding $NH_4OH$ to starting solutions; resulting sample was then put into an autoclave reactor. The optimal experimental conditions, such as reaction temperatures and times and amounts of stabilizer CaO, were carefully studied. The synthesized $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5, 3, and 8) powders were characterized by XRD, SEM, TG-DTA, and Raman spectroscopy. When the hydrothermal temperature was as low as $160^{\circ}C$, pure $ZrO_2$ and $x$ mol% CaO-$ZrO_2$ ($x$ = 1.5 and 3) powders were identified as a mixture of monoclinic and tetragonal phases. However, a stable tetragonal phase of zirconia was observed in the 8 mol% calcia doped zirconia nanopowder at hydrothermal temperature above $160^{\circ}C$. To observe the phase transition, the 3 mol% CaO-$ZrO_2$ and 8 mol% CaO-$ZrO_2$ nanopowders were heat treated from 600 to $1000^{\circ}C$ for 2h. The 3 mol% CaO-$ZrO_2$ heat treated at above $1000^{\circ}C$ was found to undergo a complete phase transition from mixture phase to monoclinic phase. However, the 8 mol% calcia doped zirconia appeared in the stable tetragonal phase after heat treatment. The result of this study therefore should be considered as the preparation of 8 mol% CaO-$ZrO_2$ nanopowders via the hydrothermal method.

• Electrical & Electronic Materials
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• v.16 no.9
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• pp.64.2-65
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• 2003

A 4 nm layer of ZrOx (targeted x-2) was deposited on an interfacial layer(IL) of native oxide (SiO, t∼1.2 nm) surface on 200 mm Si wafers by a manufacturable atomic layer chemical vapor deposition technique at 30$0^{\circ}C$. Some as-deposited layers were subjected to a post-deposition, rapid thermal annealing at $700^{\circ}C$ for 5 min in flowing oxygen at atmospheric pressure. The experimental x-ray diffraction, x-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and high-resolution parallel electron energy loss spectroscopy results showed that a multiphase and heterogeneous structure evolved, which we call the Zr-O/IL/Si stack. The as-deposited Zr-O layer was amorphous $ZrO_2$-rich Zr silicate containing about 15% by volume of embedded $ZrO_2$ nanocrystals, which transformed to a glass nanoceramic (with over 90% by volume of predominantly tetragonal-$ZrO_2$(t-$ZrO_2$) and monoclinic-$ZrO_2$(m-$ZrO_2$) nanocrystals) upon annealing. The formation of disordered amorphous regions within some of the nanocrystals, as well as crystalline regions with defects, probably gave rise to lattice strains and deformations. The interfacial layer (IL) was partitioned into an upper Si $o_2$-rich Zr silicate and the lower $SiO_{x}$. The latter was sub-toichiometric and the average oxidation state increased from Si0.86$^{＋}$ in $SiO_{0.43}$ (as-deposited) to Si1.32$^{＋}$ in $SiO_{0.66}$ (annealed). This high oxygen deficiency in $SiO_{x}$ indicative of the low mobility of oxidizing specie in the Zr-O layer. The stacks were characterized for their dielectric properties in the Pt/{Zr-O/IL}/Si metal oxide-semiconductor capacitor(MOSCAP) configuration. The measured equivalent oxide thickness (EOT) was not consistent with the calculated EOT using a bilayer model of $ZrO_2$ and $SiO_2$, and the capacitance in accumulation (and therefore, EOT and kZr-O) was frequency dispersive, trends well documented in literature. This behavior is qualitatively explained in terms of the multi-layer nanostructure and nanochemistry that evolves.ves.ves.

• 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.