• 한국광물학회지
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• 제3권2호
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• pp.65-71
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• 1990

Compositions and thermal changes of pyrrhotites from Ohtani and Uljin mines were examined by Arnold's method and DTA analysis. The results are as follow: 1) The compositions of hexagonal type pyrrhotite are in some range from 47.23-47.42 atom.% Fe in the Ohtani mine, and 47.40-47.64 atom.% Fe in the Uljin mine. 2) The compositions of hexagonal pyrrhotite with exsoluted lamellae of monoclinic pyrrhotite are in 47.35-47.50 atom.% Fe in the Ohtani mine, and 47.15-47.40 atom.% Fe in the Uljin mine. This fact does not agree with phase diagrams of Fe-S system shown by Nakazawa and Morimoto(1970) and Sugaki and Shima(1977). 3) DTA data show two endothermic peak corresponding to ${\gamma}$ and $\beta$ transformation. Sturctural conversions from order(intermediate) to disorder(high) forms occur at about $300^{\circ}C$ for hexagonal type and further lower temperature with increasing Fe-content.

• 한국표면공학회지
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• 제55권4호
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• pp.187-195
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• 2022

WO₃ thin films were synthesized by electrodeposition, and their electrochromic properties were investigated. The application of static voltage produced WO₃ films with a smooth, compact surface morphology, and the film thickness linearly increased with the application time. The thicker film showed a strong color contrast but a slow color-switching speed. High-temperature heat treatment exceeding 300 ℃ induced a phase transformation from an amorphous to a monoclinic structure and resulted in degraded electrochromic performance. Furthermore, the optimized WO₃ thin films demonstrated their potential application as electrochromic boards for writing and erasing letters using a simple modified 3D printer in a rapid, accurate process

• 한국세라믹학회지
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• 제34권2호
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• pp.145-156
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• 1997

2성분계(CaO-, Y2O3-, MgO-ZrO2) 및 3성분계(MgO-ZrO2-Al2O3)ZrO2분말의 안정화제 종류, 첨가량 및 열처리온도 변화에 따른 ZrO2의 상전이를 X-선 회절과 Raman분광법으로 연구하였다. CaO-, 및 Y2O3-ZrO2계에서 CaO와 Y2O3의 첨가량이 각각 6~15mol% 및 3~15mol%로 증가에 따른 정방정상에서의 입방정상으로의 상전이를 X-선회절 pattern으로는 판별하기 어려웠으나, Raman spectra에서는 모든 Raman band가 저파수쪽으로 이동하고 band의 수 및 그 세기가 현저히 감소함을 관찰할 수 있었다. 이것은 정방정$\longrightarrow$입방정의 상전이가 발생한 것으로 ZrO2 격자내에서 Zr4+ 이온과 Ca2+ 혹은 Y3+이온의 치환에 의해 산소이온의 빈자리 생성으로 인한 구조적 불규칙성과 선택규칙(k=0)의 파괴에 기인한 것으로 해석된다. MgO의 경우에는 10mol%에서 단사정에서 입방정으로 상전이가 발생하였다. MgO-ZrO2-Al2O3계에서는 Al2O3의 첨가에 의해 입방정$\longrightarrow$단사정의 상전이가 발생하는데 이것은 MgO와 Al2O3의 반응에 의해 spinel(MgAl2O4)의 형성으로 인하여 MgO가 충분히 안정화제로서의 역할을 하지 못하기 때문으로 판단된다. 또한, 안정화제의 종류와 첨가량 변화에 따른 ZrO2의 상전이를 ZrO2의 격자상수값의 변화와 관련하여 설명할 수 있는데, 즉, 안정화제의 첨가량이 증가할수록 격자상수 a값은 증가하고 c값은 감소하여 10~13mol%사이에서는 c/a의 축비가 1에 근접하고, 따라서 정방정$\longrightarrow$입방정의 상전이가 진행됨을 알 수 있었다.

• The Journal of Advanced Prosthodontics
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• 제8권2호
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• pp.137-143
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• 2016

PURPOSE. Grinding with less stress on 3Y-TZP through proper selection of methods and instruments can lead to a long-term success of prosthesis. The purpose of this study was to compare the phase transformation and physical properties after zirconia surface grinding with 3 different grinding burs. MATERIALS AND METHODS. Forty disc-shaped zirconia specimens were fabricated. Each Ten specimens were ground with AllCeramic SuperMax (NTI, Kahla, Germany), Dura-Green DIA (Shofu Inc., Kyoto, Japan), and Dura-Green (Shofu Inc., Kyoto, Japan). Ten specimens were not ground and used as a control group. After the specimen grinding, XRD analysis, surface roughness test, FE-SEM imaging, and biaxial flexural strength test were performed. RESULTS. After surface grinding, small amount of monoclinic phase in all experimental groups was observed. The phase change was higher in specimens, which were ground with Dura-Green DIA and AllCeramic SuperMax burs. The roughness of surfaces increased in specimens, which were ground with Dura-Green DIA and AllCeramic SuperMax burs than control groups and ground with Dura-Green. All experimental groups showed lower flexural strength than control group, but there was no statistically significant difference between control group and ground with Dura-Green DIA and AllCeramic SuperMax burs. The specimens, which were ground with Dura-Green showed the lowest strength. CONCLUSION. The use of dedicated zirconia-specific grinding burs such as Dura-Green DIA and AllCeramic SuperMax burs decreases the grinding time and did not significantly affect the flexural strength of zirconia, and therefore, they may be recommended. However, a fine polishing process should be accompanied to reduce the surface roughness after grinding.

• 한국세라믹학회지
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• 제54권4호
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• pp.285-291
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• 2017

This study investigated the effects of grain size and phase constitution on the mechanical properties of $3Y-ZrO_2$ by varying the sintering conditions. The raw powder prepared by a low-cost wet milling using the coarse solid oxide powders was sintered by both pressureless sintering and hot-pressing, respectively. As increasing holding time at $1450^{\circ}C$ for pressureless sintering, it promoted the microstructural coarsening of matrix grains and the phase transformation to tetragonal phase, whereas the bimodal microstructure embedded with abnormal $cubic-ZrO_2$ grains was observed regardless of sintering time. On the other hand, the specimens hot-pressed at $1300^{\circ}C$ for 2 h reached ~ 97% of relative density with homogeneous fine microstructure and mixed phase constitution. It was found that the proportion of untransformed monoclinic zirconia had the most adverse effect on the biaxial strength compared to the impacts of grain size and density. The pressureless sintering of the low-cost powder for prolonged sintering time to 8 h led to a decent combination of mechanical properties ($H_V=13.2GPa$, $K_{IC}=8.16MPa{\cdot}m^{1/2}$, ${\sigma}=981MPa$).

• The Journal of Advanced Prosthodontics
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• 제12권5호
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• pp.265-272
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• 2020

PURPOSE. The aims of this study were to investigate mechanical properties and hydrothermal degradation behaviour of the cubic-containing translucent yttrium oxide stabilized tetragonal zirconia polycrystal (Y-TZP). MATERIALS AND METHODS. Four groups of Y-TZP (T, ST, XT, and P), containing different amount of cubic crystal, were examined. Specimens were aged by autoclaving at 122℃ under 2 bar pressure for 8 h. Phase transformation was analyzed using X-ray diffraction (XRD) to measure phase transformation (t→m). Kruskal-Wallis test was used to determine the difference. Surface hardness, biaxial flexural strength, and fracture toughness in values among the experimental groups and verified with Wilcoxon matched pairs test for hardness values and Mann Whitney U for flexural strength and fracture toughness. RESULTS. XRD analysis showed no monoclinic phase in XT and P after aging. Only Group T showed statistically significant decreases in hardness after aging. Hydrothermal aging showed a significant decrease in flexural strength and fracture toughness in group T and ST, while group XT and P showed no effect of aging on fractural strength and fracture toughness with P<.05. CONCLUSION. Hydrothermal aging caused reduction in mechanical properties such as surface hardness, biaxial flexural strength, and fracture toughness of Y-TZP zirconia. However, cubic-containing zirconia (more than 30% by volume of cubic crystal) was assumed to have high resistance to hydrothermal degradation. Clinical significance: Cubic-containing zirconia could withstand the intraoral aging condition. It could be suggested to use as a material for fabrication of esthetic dental restoration.

• 한국재료학회지
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• 제9권9호
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• pp.943-947
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• 1999

$La(Mg_{1/2}Ti_{1/2})O_3$ 세라믹스의 구조 및 고주파 유전특성에 관한 연구를 하였다. $La(Mg_{1/2}Ti_{1/2})O_3$ 는 B site 양이온이 1:1 규칙화된 단사정 구조를 가지고 있었고 격자상수는 $a = 5.5467(3) {\AA}, b = 5.5616(3) {\AA}, c = 7.8426(5) {\AA} 그리고 \beta = 89.9589 (2)^{\circ}$ 로 밝혀졌고. $P2_1/n$의 공간군을 가지고 있었다. $La(Mg_{1/2}Ti_{1/2})O_3$ 내부에는 산소팔면체의 동상 및 역상 기울림이 존재하고 $a^_a^_c^_$ 기울림 구조를 가지고 있음을 알수 있었다. 또한 A site 양이온의 역 평행이동도 발견되었다. $1600^{\circ}C$ 이상에서 소결된 시료는 모두 95% 이상의 상대이론 밀도를 가지고 있었고 유전상수는 대략 28 정도였다. $1630^{\circ}C$ 에서 5시간 소결된 시료에서 최고높은 $Q\timesf_0$값, 63,000을 얻었다. LMT의 공진주파수 온도 계수는 $>-77 ppm/^{\circ}C ~ -79 ppm/^{\circ}C$였다.

• 한국재료학회지
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• 제22권4호
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• pp.207-210
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• 2012

The preparation of $Sm_2O_3$ doped $CeO_2$ in Igepal CO-520/cyclohexane reverse micelle solutions has been studied. In the present work, we synthesized nanosized $Sm_2O_3$ doped $CeO_2$ powders by reverse micelle process using aqueous ammonia as the precipitant; hydroxide precursor was obtained from nitrate solutions dispersed in the nanosized aqueous domains of a micro emulsion consisting of cyclohexane as the oil phase, and poly (xoyethylene) nonylphenylether (Igepal CO-520) as the non-ionic surfactant. The synthesized and calcined powders were characterized by Thermogravimetry-differential thermal analysis (TGA-DTA), X-ray diffraction analysis (XRD), and Transmission electron microscopy (TEM). The crystallite size was found to increase with increase in water to surfactant (R) molar ratio. Average particle size and distribution of the synthesized $Sm_2O_3$ doped $CeO_2$ were below 10 nm and narrow, respectively. TG-DTA analysis shows that phase of $Sm_2O_3$ doped $CeO_2$ nanoparticles changed from monoclinic to tetragonal at approximately $560^{\circ}C$. The phase of the synthesized $Sm_2O_3$ doped $CeO_2$ with heating to $600^{\circ}C$ for 30 min was tetragonal $CeO_2$. This study revealed that the particle formation process in reverse micelles is based on a two step model. The rapid first step is the complete reduction of the metal to the zero valence state. The second step is growth, via reagent exchanges between micelles through the inter-micellar exchange.

• 한국세라믹학회지
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• 제32권1호
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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.

• 한국결정성장학회지
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• 제10권3호
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• pp.233-238
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• 2000

생체적합성과 상 안정성이 우수한 t-$ZrO_2/Al_2O_3$복합체에 $Eu_2O_3$을 0~4 mol%첨가한 복합체를 $1600^{\circ}C$ 온도에서 1 시간 소결하여 상 안정성, 색상변화, 기계적 특성을 조사하였다. $180^{\circ}C$, 3.5MPa의 수증기 압력 하에서 20시간 열처리 후 X-선 회절법으로 관찰한 결과 $Eu_2O_3$가 첨가된 (Y,Nb,Eu)-TZP/$Al_2O_3$복합체는 우수한 상 안정성이 유지되었다. $Eu_2O_3$의 양이 증가함에 따라 백색계통의 상아색에서 미색의 핑크색으로 서서히 변화하였다 $Eu_2O_3$가 3 mol%까지 첨가된 복합체의 경우 620MPa, 7.6MPa.$m^{1/2}$ 이상의 강도와 인성값이 관찰되었다.