• Journal of the Korean Ceramic Society
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• v.56 no.2
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• pp.184-190
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• 2019

To improve resistance in thermal shock of zirconia setter which is frequently and repeatedly exposed to high temperature, high degree of porosity and control of thermal expansion are needed for which the fused CSZ (CaO stabilized zirconia) is used to produce the zirconia setter. In the present study, the effects of sintering temperature, cool down condition, addition of CaO stabilizer, and addition of other additives on phase transition and thermal expansion behavior of the fabrication process of zirconia setter, were examined. The zirconia setter, fabricated with fused CSZ at 1550℃, exhibited 20.4 MPa of flexural strength, 6.8% of absorbance, and 27.9% of apparent porosity. The rapid change in thermal expansion of zirconia setter is observed at temperature around 800℃, and it was reduced by low firing temperature, slowed cooled down, and addition of CaO.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.3
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• pp.124-128
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• 2013

In this research, cubic zirconia is synthesized with a refined CaO from shells as a stabilizer through Skull melting method. The proper process time and concentration are defined by Hydration reaction to produce the refined CaO after two different treatments using 0.1 mol% of HCl respectively with Cockle shell. The highest purity of CaO is reached when the shell is immersed in 1 mol% HCl. In Hydration reaction step, the pure $Ca(OH)_2$ is produced at $45^{\circ}C$ for 24 hours. The highest purity of CaO is measured when the $Ca(OH)_2$ is treated by heat at $1200^{\circ}C$ for 5 hours. The single crystals are grown through Skull melting method by adding the different contents of the refined CaO from 10 mol% to 30 mol% into $ZrO_2$. The frequency of High-frequency oscillator used for Skull melting method is 3.4 MHz. The descending speed of the single crystal is 3 mm/hour. The grown length of the single crystal is 4 cm. As a result of this study, 15 mol% of CaO has the best crystallinity.

• Journal of the Korean Ceramic Society
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• v.31 no.1
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• pp.104-114
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• 1994

ZrO2 fibers were fabricated by means of the Sol-Gel process using Zr(O-nC3H7)4-H2O-C2H5OH-HNO3 solution as a starting material. The optimum experimental parameters such as molar ratio of starting materials, concentration, temperature, viscosity, the amounts of stabilizer and the pH of solution were determined. The experimentally determined optimum variables which produce good ZrO2 fibers were used to manufacture the Y2O3-and CaO-ZrO2 fibers. The amounts of Y2O3 and CaO were varied within the range from 1.5~5 mol% and 3~15 mol% respectively. The phase transformation and microstructural evolution of the fabricated ZrO2 gel fibers were investigated after heat treatments up to 120$0^{\circ}C$ by X-ray diffraction, Raman microprobe spectroscopy, SEM, and specific surface area and pore volume measurements. From the analysis of X-ray diffraction and Raman spectra, the phase of heat treated Y2O3-and CaO partially stabilized ZrO2 gel fibers(Y2O3:2.5~3 mol%, CaO:6~9 mol%) were identified as a tetragonal phase up to 100$0^{\circ}C$. The maximum tensile strength of 2.5Y2O3-97.5ZrO2 and 6CaO-94ZrO2 (in mol%) fibers heat treated at 100$0^{\circ}C$ for 1 hr was found be 1.3~2 GPa with diameters of 10~20 ${\mu}{\textrm}{m}$.

• Korean Journal of Materials Research
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• v.30 no.4
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• pp.176-183
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• 2020

The high-temperature stability of YSZ specimens fabricated by die pressure and cold isostatic press (CIP) is investigated in CaCl₂-CaF₂-CaO molten salt at 1,150 ℃. The experimental results are as follows: green density 46.7 % and 50.9 %; sintering density 93.3 % and 99.3 % for die press and CIP, respectively. YSZ foremd by CIP exhibits higher stability than YSZ formed by die press due to denseness dependency after high-temperature stability test. YSZ shows peaks mainly attributed to CaZrO₃, with a small t-ZrO₂ peak, unlike the high-intensity tetragonal-ZrO₂ (t-ZrO₂) peak observed for the asreceived specimen. The t-ZrO₂ phase of YSZ is likely stabilized by Y₂O₃, and the leaching of Y₂O₃ results in phase transformation from t-ZrO₂ to m-ZrO₂. CaZrO₃ likely forms from the reaction between CaO and m-ZrO₂. As the exposure time increases, more CaZrO₃ is observed in the internal region of YSZ, which could be attributed to the inward diffusion of molten salt and outward diffusion of the stabilizer (Y₂O₃) through the pores. This results in greater susceptibility to phase transformation and CaZrO₃ formation. To use SOM anodes for the electroreduction of various metals, YSZ stability must be improved by adjusting the high-density in the forming process.

• 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.

• Journal of Conservation Science
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• v.33 no.3
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• pp.215-223
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• 2017

The purpose of this study is to reveal the characteristics, correlations, and colorant materials of those using the chemical compositions of 30 glasses excavated from the Sarari hall of the Mireuksaji stone pagoda, and to determine the correlations between them and other glass excavated from the Wanggungri site. The results of the chemical analysis of the 11 glass beads show that they are a soda glass group with high contents of $SiO_2$ and $Na_2O$; these can be further subdivided into soda-alumina groups ($Na_2O-Al_2O_3-CaO-Si_2O$). The characteristics of the stabilizer are classified as being of the high alumina glass group (LCHA), except for two glasses. It was concluded that colorant materials affected the coloring for glass beads by various components including Ti, Mn, Fe, Cu and Pb. In addition, we examined six lead glasses which are glass plate and unknown fragments that are of a common lead glass system ($PbO-SiO_2$) with respect to the average contents of PbO (70wt.%) and $SiO_2$ (30wt.%). As a result of comparing these relics with those of the glass beads excavated by Wanggungri, there is a similarity in that they belong to the soda glass group. However, the contents of $Na_2O$ are relatively higher than that of the glass beads in the Mireuksaji pagoda, and most of relics include glasses with a low content of $K_2O$ and CaO. In addition, the PbO and $SiO_2$ contents are slightly different in the lead glass. It seems that the glass relics made at two different sites may have used different raw materials or techniques.

• Journal of Conservation Science
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• v.31 no.3
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• pp.255-265
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• 2015

In this study, the potash glass beads of 281 samples in 30 sites analyzed until now were classified according to the chemical composition. And the color, size, manufacturing technique and distribution period were compared. Korea potash glass beads are divided into 3 types depending on the stabilizer content. I, II type is the CaO and $Al_2O_3$ content of less than 5%. Relatively, I type has a high CaO and II type has a high $Al_2O_3$. In contrast, III type comprises more than CaO 5%. I, II type is the saltpetre, III type is estimated using plant ash as row material of flux. A review of the properties by type, I type is cobalt blue, copper blue and purple beads. The outer diameter is sized to the range 1.4~7.4mm. Also it was produced by the drawing technique. It was used continuously from BC 1C until around AD 6C. On the other hand, II type is outer diameter of 1.9~3.6mm and a copper blue beads. manufacturing technique is the same as the I type. This seems to have been in use since around AD 1C to 4C. Finally, III type is brown, colorless, amber beads and an outer diameter of about 10mm. It was formed by winding technique and appeared in the tombs of Goryeo and Joseon Dynasty. As a result, 3 types of potash glass beads distributed in Korea is likely to flowing through the various trade routes from different provenances.

• 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.

• 보존과학연구
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• s.35
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• pp.5-23
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• 2014

The possibility of non-destructive inspection glass beads for verification. Conduct a comparative analysis of the Chungcheong area with glass beads excavated Age-specific characteristics of the glass beads shall be classified by region. Trace amounts of ingredients such as CaO, $Al_2O_3$ (stabilizer), MgO, the difference is negligible. $SiO_2$ (subjects), $Na_2O$ (flux) analysis and the difference between the values was greater than in the other ingredients. Composition differences occurred rough surface to a non-uniform cross-section analysis is considered. Minimize the error value, such as the surface of carbon-coated Study, there are additional requirements. Produced at the time of the social and cultural characteristics of ancient glass and important archaeological materials, and to inform the process of cultural exchange between each region in the production of glass technology era according to the level of science and technology, arts and crafts, can be identified.

• Korean Journal of Materials Research
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• v.24 no.12
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• pp.677-681
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• 2014

To increase the mechanical property of zirconia, we have investigated the phase change and the resulting hardness of zirconia ceramics by hydroxyapatite (HA) powder bed sintering. It was observed using X-ray diffraction that the cubic zirconia phase, which has a higher hardness value than that of the tetragonal phase, was obtained at the surface of 3 mol% $Y_2O_3$ doped tetragonal zirconia polycrystal (3Y-TZP) ceramics during the sintering process; in our experimental conditions, the phase change at the surface increased as the sintering time increased. We believe that the observed crystalline phase change originated from the decomposition of HA and the diffusion of CaO, as follows. CaO, which was derived from the decomposition of HA at high temperature ($1400^{\circ}C$), diffused into the surface of 3Y-TZP and acted as a stabilizer. As a result, the Vickers hardness value of the treated specimens was higher than that of the non-treated specimen due to the formation of the cubic phase on the surface of 3Y-TZP.