• Bulletin of the Korean Chemical Society
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• 제28권12호
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• pp.2279-2282
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• 2007

Highly crystalline, uniform Fe nanoparticles were successfully synthesized and encapsulated in zirconia shell using sol-gel process. Two different approaches have been employed for the coating of Fe nanoparticle with zirconia. The thickness of zirconia shell can be readily controlled by altering molar ratio of Fe nanoparticle core to zirconia precursor in the first case where as reaction time was found to be most effective parameter to controlled the shell thickness in the second method. The structure and magnetic properties of the ZrO2-coated Fe nanoparticles were studied. TEM and HRTEM images show a typical core/shell structure in which spherical α-iron crystal sized of ~25 nm is surrounded by amorphous ZrO2 coating layer. TGA study showed an evidence of weight loss of less than 2% over the temperature range of 50-500 °C. The nanoparticles are basically in ferromagnetic state and their magnetic properties depend strongly on annealing temperature. The thermal treatment carried out in as-prepared sample resulted in reduction of coercivity and an increase in saturation magnetization. X-ray diffraction experiments on the samples after annealing at 400-600 °C indicate that the size of the Fe@ZrO2 particles is increased slightly with increasing annealing temperature, indicating the ZrO2 coating layer is effective to interrupt growing of iron particle according to heat treatment.

• 공업화학
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• 제25권6호
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• pp.564-569
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• 2014

지르코니아 나노분말을 수열합성법으로 제조하였으며, 반응온도, 반응시간, 침전제의 종류 및 농도, 전구체의 종류를 실험 변수로 하였고, 각각의 제조된 분말을 X-선 회절(XRD)과 주사전자현미경(FE-SEM)을 통해 입자크기 및 결정상을 측정하였다. 침전제의 농도 증가에 따라 지르코니아 입자크기가 증가하였으며, 입자의 결정화도도 높아졌고, KOH 보다 NaOH 침전제를 사용하였을 경우, 입자 성장 속도가 증가하였다. 이는 입자의 크기 컨트롤에 있어 NaOH를 사용하는 경우보다 KOH를 사용하는 것이 더 효과적이었다. 4 h의 수열반응시간에서는 4 h의 수열반응시간에서는 비정질의 지르코니아 입자가 발견되었지만, 8 h 이상 합성 시, 단사정상의 지르코니아 입자가 생성됨을 확인하였고, 반응시간이 길어짐에 따라 지르코니아 입자의 폭이 소폭으로 줄어들고, 길이는 소폭 늘어남을 확인하였다. 동일한 합성 조건에서 전구체로서 zirconium (IV) acetate, zirconium nitrate, zirconium chloride 중에서 zirconium chloride를 사용하여 합성하였을 경우, 입자의 크기가 가장 작게 형성되었다.

• 한국결정학회:학술대회논문집
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• 한국결정학회 2003년도 춘계학술연구발표회
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• pp.20-20
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• 2003

A new and simple method has been developed to synthesize highly crystalline and monodisperse maghemite (γ-Fe₂O₃) and zirconia (ZrO₂) nanocristallites. High temperature aging of metal-surfactant complex was founded to generate monodisperse nanoparticles, wherein the nuclei were prepared by the thermal decomposition of iron-oleate complex in case of iron oxide and nonhydrolytic sol-gel reaction in case of zirconia respectively. By varying the experimental conditions, in other words concentration of surfactants, kind of metal precursor, reaction temperature and so on, the diameter of spherical nanoparticles could be controlled at various size. The synthesized nanoparticles were characterized by electron diffraction, X-ray diffraction, and low- and high-resolution transmission electron microscope.

• 한국재료학회지
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• 제27권1호
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• pp.1-7
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• 2017

Zirconia nanoparticles were widely used as filler in order to get high refractive index layer. However, dispersion of nanoparticles is difficult due to their agglomeration in solvent. In this study, the dispersibility of the zirconia suspension is promoted by controlling the steric hindrance and electrostatic interactions through the adsorption of PEI according to alkali treatment time. Also, to induce improved dispersibility on suspension, we changed the dispersion conditions variously and fabricated an ink formulation method for the coating layer. Zirconia suspension was characterized by dynamic light scattering (DLS), Zeta potential measurement, Transmission Electron Microscope (TEM) and FT-IR. We were able to confirm that good dispersion of zirconia suspension by alkali treatment and PEI led to high refractive index.

• 한국결정성장학회:학술대회논문집
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• 한국결정성장학회 2000년도 Proceedings of 2000 International Nano Crystals/Ceramics Forum and International Symposium on Intermaterials
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• pp.143-150
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• 2000

Wet-chemical process using ammonia to precipitate aluminum ion dissolved in a zirconia sol solution is examined. Formation of crystalline bayerite is unfavorable for fine dispersion of zirconia nanoparticles in alumina matrix after heat treatment. To avoid the bayerite formation, it was preferred to make a precipitation with a diluted ammonia or with an ammonia gas flow at high temperature. By optimizing the precipitation process and the calcination temperature, we successfully prepared the uniform microstructure in which tetragonal zirconia particles of ∼30nm is finely dispersed within the alumina grains.

• 한국재료학회지
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• 제30권11호
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• pp.609-614
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• 2020

3 mol% yttria-doped stabilized zirconia (3YSZ) is synthesized by a solvothermal process, and its characteristics are investigated using various methods. Also, the dispersibility of synthesized 3YSZ nanoparticles is observed with the species of surface modifier. The 3YSZ nano sol prepared with an optimum condition is employed in prism coating and its properties are evaluated. The synthesized 3YSZ nanoparticles show a globular shape with about 10 to 20 nm crystallite size. The mixed phases with the nano sol show a high specific surface of 178 ㎡/g. The prism sheet coated with the 3YSZ nano sol present an excellent refractive index, transmittance, and luminance; refractive index is 1.603, transmittance is 90.2 %, and luminance of coating film is improved by 5.9 % compared to that of the film without 3YSZ nano sol. It is verified that the surface modified 3YSZ is suitable as the prism sheet for optical displays.

• 한국재료학회지
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• 제19권8호
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• pp.412-416
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• 2009

In this study, 3 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) nanoparticles were synthesized by the glycothermal method under various reaction temperatures and times. The co-precipitated precursor of 3Y-TZP was prepared by adding $NH_4OH$ to starting solutions, and then the mixtures were placed in an autoclave reactor. Tetragonal yttria-doped zirconia nanoparticles were afforded through a glycothermal reaction at a temperature as low as $220^{\circ}C$, using co-precipitated gels of $ZrCl_4$ and $YCl_3{\cdot}6H_2O$ as precursors and 1,4-butanediol as the solvent. The synthesized 3Y-TZP particles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Raman spectroscopy. The 3Y-TZP particles have a stable tetragonal phase only at glycothermal temperatures above $200^{\circ}C$. To investigate phase transition, the 3Y-TZP particles were heat treated from 400 to $1400^{\circ}C$ for 2 h. Raman analysis indicated that, after heat treatment, the tetragonal phase of the 3Y-TZP particles remained stable. The results of this study, therefore, suggest that 3Y-TZP powders can be prepared by the glycothermal method.

• 한국재료학회지
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• 제34권2호
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• pp.79-84
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• 2024

Thin films of yttria-stabilized zirconia (YSZ) nanoparticles were prepared using a low-temperature deposition and crystallization process involving successive ionic layer adsorption and reaction (SILAR) or SILAR-Air spray Plus (SILAR-A+) methods, coupled with hydrothermal (175 ℃) and furnace (500 ℃) post-annealing. The annealed YSZ films resulted in crystalline products, and their phases of monoclinic, tetragonal, and cubic were categorized through X-ray diffraction analysis. The morphologies of the as-prepared films, fabricated by SILAR and SILAR-A+ processes, including hydrothermal dehydration and annealing, were characterized by the degree of surface cracking using scanning electron microscopy images. Additionally, the thicknesses of the YSZ thin films were compared by removing diffusion layers such as spectator anions and water accumulated during the air spray plus process. Crack-free YSZ thin films were successfully fabricated on glass substrates using the SILAR-A+ method, followed by hydrothermal and furnace annealing, making them suitable for application in solid oxide fuel cells.

• 구강회복응용과학지
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• 제38권1호
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• pp.18-25
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• 2022

목적: 이 연구의 목적은 지르코니아 나노입자 첨가된 PEMA (Polyethyl Methacrylate)레진 표면의 색안정성 및 항균평가 하는 것이다. 연구 재료 및 방법: PEMA 레진의 모노머에 지르코니아 나노입자를 각각 2, 4, 8 w/v%을 첨가하여 교반기를 이용하여 2시간 동안 교반하였다. 각각의 용액에 폴리머를 혼합하여 직경 15 mm, 두께 2 mm의 디스크 형태의 시편을 제작하였다. 대조군은 PEMA 레진, 실험군은 2, 4, 8 w/v% 첨가한 지르코니아 나노입자를 Z2군, Z4군, Z8군으로 나누었다. 시편의 표면거칠기 및 색안정성을 분석한 후, Porphyromonas gingivalis (P. gingivalis)를 이용하여 항균평가 하였다. 통계 분석은 Shapiro-Wilk normality test에서 정규성을 만족하는 경우 일원분산분석으로 통계 분석하였으며 사후검정으로는 Tukey test을 이용하였고(P < 0.05), 정규성을 만족하지 못하는 경우 비모수 검정인 Kruskal Wallis test를 시행하였다(P < 0.05). 결과: 표면거칠기 측정결과, Z2군, Z4군, Z8군은 대조군과 비교하여 유의한 차이가 없었다. 색안정성 평가결과, Z2군, Z4군, Z8군은 자연치아의 색상 범위 내에 있었다. Z2군은 대조군과 비교하여 P. gingivalis 부착이 유의하게 감소하였다(P < 0.05). Z2군, Z4군, Z8군은 사멸된 박테리아가 대조군보다 더 많이 관찰되었다. 결론: 지르코니아 나노입자가 첨가된 PEMA 레진의 색상은 자연치아 범위 내에 있으며, P. gingivalis의 부착을 감소시킨다.

• 한국재료학회지
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• 제32권3호
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• pp.125-131
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• 2022

Effect of sulfation processes on the physicochemical properties of ZrO₂ and TiO₂ nanoparticles were thoroughly investigated. SO₄/ZrO₂ and SO₄/TiO₂ catalysts were synthesized to identify the acidity character of each. The wet impregnation method of ZrO₂ and TiO₂ nanoparticles was employed using H2SO₄ with various concentrations of 0.5, 0.75, and 1 M, followed by calcination at 400, 500, and 600 ℃ to obtain optimum conditions of the catalyst synthesis process. The highest total acidity was found when using 1 M SO₄/ZrO₂-500 and 1 M SO₄/TiO₂-500 catalysts, with total acidity values of 2.642 and 6.920 mmol/g, respectively. Sulfation increases titania particles via agglomeration. In contrast, sulfation did not practically change the size of zirconia particles. The sulfation process causes color of both catalyst particles to brighten due to the presence of sulfate. There was a decrease in surface area and pore volume of catalysts after sulfation; the materials' mesoporous structural properties were confirmed. The 1 M SO₄/ZrO₂ and 1 M SO₄/TiO₂ catalysts calcined at 500 ℃ are the best candidate heterogeneous acid catalysts synthesized in thus work.