• Journal of the Korean Ceramic Society
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• v.31 no.9
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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 $700^{\circ}C$.

• Korean Journal of Materials Research
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• v.23 no.8
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• pp.441-446
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• 2013

There is increasing interest in zirconia as a dental material due to its aesthetics, as well as the exceptionally high fracture toughness and high strength that are on offer when it is alloyed with certain oxides like yttria. In recent years, many solution based chemical synthesis methods have been reported for synthesis of zirconia, of which the sol-gel method is considered to be best. Here, we synthesize zirconia by a sol gel assisted precipitation method using either PEG or PVA as a stabilizing agent. Zirconia sol is first synthesized using the hydrothermal method. We used NaOH as the precipitating agent in this method because it is easy to remove from the final solution. Zirconium and yttrium salts are used as precursors and PEG or PVA are used as stabilizers to separate the metal ions. The resulting amorphous zirconia powder is calcined at $900^{\circ}C$ for 2 h to get crystallized zirconia. XRD analysis confirmed the partially stabilized zirconia synthesis in all the synthesized powders. SEM was taken to check the morphology of the powder synthesized using either PEG or PVA as a stabilizing agent and finally the transparency was calculated. The results confirmed that the powder synthesized with 10 % PVA as the stabilizing agent had highest percentage of transparency among all the synthesized powder.

• Bulletin of the Korean Chemical Society
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• v.27 no.1
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• pp.65-70
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• 2006

An amperometric glucose biosensor has been developed based on the use of the nanoporous composite film of sol-gel-derived zirconia and perfluorosulfonated ionomer, Nafion, for the encapsulation of glucose oxidase (GOx) on a platinized glassy carbon electrode. Zirconium isopropoxide (ZrOPr) was used as a sol-gel precursor for the preparation of zirconia/Nafion composite film and the performance of the resulting glucose biosensor was tuned by controlling the water content in the acid-catalyzed hydrolysis of sol-gel stock solution. The presence of Nafion polymer in the sol-gel-derived zirconia in the biosensor resulted in faster response time and higher sensitivity compared to those obtained at the pure zirconia- and pure Nafion-based biosensors. Because of the nanoporous nature of the composite film, the glucose biosensor based on the zirconia/Nafion composite film can reach 95% of steady-state current less than 5 s. In addition, the biosensor responds to glucose linearly in the range of 0.03-15.08 mM with a sensitivity of 3.40 $\mu$A/mM and the detection limit of 0.037 mM (S/N = 3). Moreover, the biosensor exhibited good sensor-to-sensor reproducibility (~5%) and long-term stability (90% of its original activity retained after 4 weeks) when stored in 50 mM phosphate buffer at pH 7 at 4 ${^{\circ}C}$.

• Journal of the Korean Ceramic Society
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• v.30 no.7
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• pp.571-577
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• 1993

The effect of $\alpha$-Al2O3 seeding on preparation of zirconia/alumina gel fragment prepared by sol-gel processing was characterized through XRD, SEM, TG/DTA and IR analysis. Aluminum isopropoxide and zirconium butoxide were used as starting materials. $\alpha$-Al2O3 seeding restrained grain growth of alumina and zirconia, and decreased tetragonal to monoclinic phase transformation of zirconia on cooling. Therefore, fine zirconia-toughened alumina composite having the relative sintered density of about 98% of theoretical at 140$0^{\circ}C$ for 2h could be obtained.

• Journal of the Korean Applied Science and Technology
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• v.38 no.6
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• pp.1561-1567
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• 2021

In this study, we have studied synthesis of zirconia-alumina composite coating materials via a low-temperature sol-gel process. The zirconia-alumina composites were prepared by coating zirconia precursor, alumina precursor, and organosilane mixture on a polyethylene terephthalate substrate through three steps: sol-gel process, low-temperature photocuring process, and heat treatment process. The structural properties and element analysis of the composites were confirmed by FT-IR and XPS. The coated composite showed a transmittance of 96% or more in the visible light region with a wavelength of 420 nm or more and pencil hardness of 9H or more. In case of the composite of the molar ratio of zirconia and alumina of 1:4, the highest nanoindentation hardness was measured with 1.212 GPa.

• Journal of the Korean Ceramic Society
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• v.45 no.2
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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.

• Proceedings of the Korean Society of Tribologists and Lubrication Engineers Conference
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• 1998.10a
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• pp.265-271
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• 1998

High temperature wear behavior of plasma sprayed zirconia based coating sealing with zirconia sol were investigated for high temperature wear resistance application. The zirconia powders containing 2.5, 5.0, 7.5, 10.0 mol% of MoS$_2$, $Fe_2O_3$ for plasma spray were made by spray drying method. As-sprayed coating was sealed by zirconia-sol to fill up the pore and crack in coating. wear test were performed at temperature ranges from room temperature to 600$\circ$C. The microstructural changes of before and after sealing process were examined by SEM, XRD and EPMA. After sealing process, the porosity was decreased and micro-hardness was increased. The wear properties of coating after sealing process were improved by sealing of pores and cracks. The behavior of wear amount and coefficient of friction were same tendency to before sealing process.

• Journal of the Korean Ceramic Society
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• v.29 no.7
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• pp.544-550
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• 1992

Zirconia gel fibers could be made by drawing from polyester sol containing zirconyl oxychloride during the reaction between ethylen glycol and citric acid. In this case, the critical mole ratio of zirconyl oxychloride to citric acid was about 4 and by adding CaCl2 and calcining the gel fiber in the air, cubic stabilized zirconia fibers having much micropores at surface could be obtained.

• 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.

• Journal of the Korean Ceramic Society
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• v.47 no.4
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• pp.343-352
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• 2010

A zirconia gel/polymer hybrid nanofiber was produced in a nonwoven fabric mode by electrospinning a sol derived from hydrolysis of zirconium butoxide with a polyvinyl butyral. Results indicated that the hydroxyl groups on the vinyl alcohol units in the backbone of the polymer were involved in the hydrolysis as well as grafting the hydrolyzed zirconium butoxide. In addition, use of acetic acid as a catalyst resulted in further hydrolysis and condensation in the sol, which led to the growth of -Zr-O-Zr- networks among the polymer chains. These networks gradually transformed into a crystalline zirconia structure upon heating. The as-spun fiber was smooth but partially wrinkled on the surface. The average fiber diameter was $690{\pm}110\;nm$. The fiber exhibited a strong but broad blue photoluminescence with its maximum intensity at a wavelength of ~410 nm at room temperature. When the fiber was heat-treated at $400^{\circ}C$, the fiber diameter shrunk to $250{\pm}60\;nm$. Nanocrystals which belonged to a tetragonal zirconia phase and were ~5 nm in size appeared. A strong white photoluminescence was observed in this fiber. This suggests that oxygen or carbon defects associated with the formation of the nanocrystals play a role in generating the photoluminescence. Further heating to $800^{\circ}C$ resulted in a monoclinic phase beginning to form In the heat-treated fibers, coloring occurred but varied depending on the heating temperature. Crystallization, coloring, and phase transition to the monoclinic structure influenced the photoluminescence. At $600^{\circ}C$, the fiber appeared to be fully crystallized to a tetragonal zirconia phase.