• 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 $700^{\circ}C$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.5
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• pp.205-211
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• 2022

The Granule Spray in Vacuum (GSV) process is a method of forming a dense nanostructured ceramic coating film by spraying ceramic granules on a substrate at room temperature in a vacuum. In the Granule Spray, the granules made by agglomerating particles with the size from submicrometer to micrometer can be sprayed into the substrate. Once the granules were squashed upon collision with the substrate, they become several dozens of nanometer-sized crystals in vacuum process. The zirconia of the monoclinic phase transform into tetragonal phase at 1150℃. At this time, its volume is changed by about 6.5 %. For this reason, it is widely held that it is difficult to acquire a compact of monoclinic zirconia sinter. In this study, the effect of particle treatment temperature and standoff distance on the substrate of zirconia granules were investigated in GSV. Also, particle treatment temperature, standoff distance, coating efficiency, and microstructure of the film were considered in forming the monoclinic zirconia coating film in GSV without any heating process. The deposited films exhibited monoclinic zirconia phase without any other detectable phase by X-ray diffractometer (XRD).

• 한국신재생에너지학회:학술대회논문집
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• 2011.11a
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• pp.84.2-84.2
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• 2011

In this research, two thin film deposition techniques, Atomic Layer Deposition and Sputtering are carried out for the fabrication of Yittria Stabilized Zirconia electrolyte for thin film Solid Oxide Fuel Cell. Zirconium to Yittrium ratio for both cases is about 1/8. Scanning Electron Microscope(SEM) image shows that the growth rate per hour for Atomic Layer Deposition is faster than for sputtering. X-ray Photo-electron Spectroscopy(XPS) shows that the peaks of both Zirconia and Yittria shift towards higher bending energy for the case of Atomic Layer deposition and thus are more strongly attached to the substrate. Later, Nyquist plot was used to compare the conductivity of Yittria Stabilized Electrolyte for both cases. The conductivity at $300^{\circ}C$ for Atomic Layer Deposited Yittria Stabilized Zirconia is found to be $5{\times}10^{-4}S/cm$ while that for sputtered Yittria Stabilized Zirconia is $2{\times}10^{-5}S/cm$ at the same temperature. The reason for better performance for Atomic Layered YSZ is believed to be the Nano-structured layer fabrication that aids in along the plane conduction as compared to the columnarly structured Sputtered YSZ.

• 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.36 no.9
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• pp.991-996
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• 1999

Effect of solution property on the weight varation and microstructural change of film was studied by electrophoretic deposition in order to obtain a homogeneous and dense zirconia film. As a result of weight kinetics of film which obtained in alcohol or aqueous solution having different polarity experimental data showed large deviation from theoretical ones calculated by Zhang's kinetic model. It had been shown that the weight affecting factors was largely dependent on properties other than dielectric constant and viscosity of solvent zeta potential appiled field and time. In initial stage a main factor of the drastic weight increase was the capillary drag of porous substrate. The cause of weight decrease with time in aqueous solution after 300 s was attributed to the defect of film by sagging and electrolytic reaction. The electrolyte film which prepared in alcohol solution with good wetting for substrate had better homogeneous and dense microstructure than one in aqueous solution with high surface tension.

• Korean Journal of Materials Research
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• v.9 no.2
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• pp.155-162
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• 1999

Zirconia thin films of uniform structure were fabricated by plasma-enhanced metal-organic chemical vapor deposition. Deposition conditions such as substrate temperature were observed to have much influence on the formation of zirconia films, therefore the mechanism of decomposition of $Zr[TMHD]_4$precursor and film growth were examined by XRD, FT-IR etc., as well as the determination of the optimal deposition condition. From temperature dependence on zirconia, below the deposition temperature of 523K, the amorphous zirconia was formed while the crystalline of zirconia with preferred orientation of cubic (200) was obtained above the temperature. Deposits at low temperatures were investigated by FT-IR and the absorption band of films revealed that the zirconia thin film was in amorphous structure and has the same organic band as that of Zr precursor. In case of high temperature, it was found that Zr precursor was completely decomposed and crystalline zirconia was obtained. In addition, at 623K the higher RF power yielded the increased crystallinity of zirconia implying an increase in decomposition rate of precursor. However, it seems that RF power has nothing with the zirconia deposition process at 773K. It was found that the proper bubbler temperature of TEX>$Zr[TMHD]<_4$ precursor is needed along with high flow rate of carrier gas. Through AFM analysis it was determined that the growth mechanism of the zirconia thin film showed island model.

• Proceedings of the Materials Research Society of Korea Conference
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• 1997.10a
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• pp.116-116
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• 1997

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 1998.05a
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• pp.158-159
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• 1998

• 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 institute of surface engineering
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• v.30 no.3
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• pp.183-190
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• 1997

Fabrication and crystallization characteristics of yttria($T_2O_3$) stabilized zirconia(YSZ) thin film by sol-gel process were studied. YSZ sol was synthesized with zirconium n-propoxide($Zr(OC_3H_7)_4)$) and yttrium nitrate pentahydrate ($Y(NO_3)_3.5H_2O$). YSZ film was prepared by depositing the polymeric sol on porous $Al_2O_3$ substrate by spin-coating, and the film characteristics were investigated by FRIR, TG-DTA, XRD, DSC, optical microscopy and SEM. The film topology was uniform and cracks were not found. It was found that the annealing temperature and the concentration of stabilizer affect the crystallization of YSZ film. The YSZ film began to crystallize from amorphous to tetragonal phase at 40$0^{\circ}C$, and it was not converted to cubic structure until $1100^{\circ}C$. It seemed that the grains were formed over $700^{\circ}C$and the average grain size was obtained about 0.2$\mu\textrm{m}$.