• 한국재료학회지
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• 제20권4호
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• pp.217-222
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• 2010

Zirconium diboride (ZrB2) and mixed diboride of (Zr0.7Ta0.3)B2 containing 30 vol.% silicon carbide (SiC) composites were prepared by hot-pressing at $1800^{\circ}C$. XRD analysis identified the high crystalline metal diboride-SiC composites at $1800^{\circ}C$. The TaB2 addition to ZrB2-SiC showed a slight peak shift to a higher angle of 2-theta of ZrB2, which confirmed the presence of a homogeneous solid solution. Elastic modulus, hardness and fracture toughness were slightly increased by addition of TaB2. A volatility diagram was calculated to understand the oxidation behavior. Oxidation behavior was investigated at $1500^{\circ}C$ under ambient and low oxygen partial pressure (pO2~10-8 Pa). In an ambient environment, the TaB2 addition to the ZrB2-SiC improved the oxidation resistance over entire range of evaluated temperatures by formation of a less porous oxide layer beneath the surface SiO2. Exposure of metal boride-SiC at low pO2 resulted in active oxidation of SiC due to the high vapor pressure of SiO (g), and, as a result, it produced a porous surface layer. The depth variations of the oxidized layer were measured by SEM. In the ZrB2-SiC composite, the thickness of the reaction layer linearly increased as a function of time and showed active oxidation kinetics. The TaB2 addition to the ZrB2-SiC composite showed improved oxidation resistance with slight deviation from the linearity in depth variation.

• 한국세라믹학회지
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• 제34권11호
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• pp.1113-1120
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• 1997

The 2, 4, 6 and 8mol% Y2O3 doped-ZrO2 powders (20 kinds) with the addedtion of Al2O3 upto 8wt% were prepared by coprecipitation method using the zirconium oxyacetate, yttrium chloride and aluminum nitrate as starting materials. The coprecipitated powders were characterized by XRD, TG-DTA, FT-IR and SEM. The sintering properties of zirconia-alumina composites prepared by 2YSZ and 8YSZ powders containing various Al2O3 contents were also investigated. With increasing the yttria stabilizer contents, the amount of exothermic heat for zirconia crystallization decreased. And it was confirmed that the crystallizing temperature of coprecipitated zirconia powders increased and the crystallization process occurred in a wide temperature range, as Al2O3 content increased in 8YSZ.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2014년도 제46회 동계 정기학술대회 초록집
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• pp.389.1-389.1
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• 2014

최근의 환경 및 에너지에 대한 관심으로 수요가 증가하고 있는 하이브리드 및 전기 자동차나 태양광발전, 풍력발전용의 인버터기기에는 고에너지밀도 커패시터가 필수적이 되었다. 높은 에너지 밀도를 요구하는 전력전자, 펄스파워 등의 응용분야에 사용되는 고에너지밀도 커패시터는 PET (Polyethylene terephtalate)와 PP (Polypropylene)와 같은 폴리머 유전체를 사용하는 범용 필름 커패시터가 사용되었으나 사용 요구 조건의 한계에 도달하여, 새로운 유전체를 적용하는 커패시터가 절실히 필요한 상황이다. PET와 PP와 같은 유전체는 유전상수가 2~3의 낮은 값을 가지고 있어 고에너지밀도를 구현하기가 어렵다. 본 연구에서는 새롭게 요구되고 있는 고에너지 밀도 커패시터의의 성능을 만족시키기 위하여 $20{\sim}50{\mu}m$ 두께의 PET 필름상에 세라믹 유전체인 $ZrO_2$ 박막을 스퍼터(Sputter) 증착법에 의해 코팅하여 종래의 필름 커패시터와 세라믹 커패시터의 장점을 갖는 커패시터를 제조하기 위한 박막 유전재료의 개발을 목표로 하였다. 수백 nm~수 ${\mu}m$ 두께의 $ZrO_2$ 박막을 스퍼터링 공정조건에 따라 증착한 후 박막의 결정성, 기판과의 부착성, 증착속도, 유전상수, 절연파괴강도, 온도안정성 등을 XRD, SEM, AFM, EDS, XPS, Impedance analyzer 등에 의해 평가하였다. $ZrO_2$ 유전체막은 상온에서 증착하였음에도 정방정(tetragonal)구조의 결정질로 성장하였고 증착압력이 증가함에 따라 주피크의 세기가 감소하였다. 증착 중 산소가스를 주입하였을 경우에도 결정질막으로 성장하였다. 증착막들은 산소가스의 양이 증가함에 따라 짙은 흰색으로 변하였으며 PET 기판과의 접착력도 약해졌다. 또한 거칠기는 Ar가스만으로 증착한 경우보다 증가하였으며 24~66 nm의 평균 거칠기값을 보였다. PET위에 Ar가스만으로 증착한 $ZrO_2$의 비유전율은 1kHz에서 116~87의 비유전율을 보여 PET에 비해 매우 우수한 특성을 보였다. $ZrO_2$ 막들은 300kV/cm의 전계에서 대략 10-8A 이하의 누설전류를 보였다. 증착가스비를 달리하여 제조된 시편에서도 유사한 누설전류값을 나타내었다. 300 kV/cm 전후의 전계까지 측정한 $ZrO_2$ 막의 P-E (polarization-electric field) 특성을 확인하였는데, 5 mTorr의 압력에서 증착한 막은 253 kV/cm에서 $5.5{\mu}C/cm^2$의 분극값을 보였다. P-E커브의 기울기와 분극량에 따라 에너지밀도가 달라지므로 공정조건에 따라 에너지밀도가 변화됨을 예측할 수 있었다. PET위에 스퍼터 증착한 $ZrO_2$ 유전체막은 5mTorr의 Ar가스분위기에서 제조할 때 가장 안정적인 구조를 보였으며, 고에너지밀도 커패시터에의 적용가능성을 보였다.

• 한국산학기술학회논문지
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• 제8권5호
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• pp.995-999
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• 2007

저온 소결용 압전 세라믹 소결체의 치밀화에 미치는 첨가제의 영향을 조사하기 위하여 $PbZrTiO_3$(PZT) 분말을 제조하였으며, 이 PZT 분말을 이용하여 제조한 압전 세라믹스의 치밀화에 미치는 첨가제의 영향을 조사하였다. 첨가제는 $wB_2O_3-xBi_2O_3-zCuO$와 $LiBiO_2-CuO$ 두 종류가 제조되었으며 이 들 첨가제의 양을 변화 시켜 효과를 조사하였다. PZT 분말에 소결조제로서 1wt.% 의 $LiBiO_2-CuO$를 첨가하여 시편을 제조한 후, $800{\sim}1200^{\circ}C$까지의 온도 범위에서에서 소결한 결과 $900^{\circ}C$에서 최고의 소결밀도를 나타내었다. 소결된 압전체의 결정상을 분석하기 위하여 X-선회절분석을 시행하였으며, $900^{\circ}C$의 저온에서 소결한 $PbZrTiO_3$의 시편의 미세조직을 관찰하기 위하여 주사전자현미경(SEM)을 이용하였다. X-선 회절분석에서는 잘 발달된 PZT 상이 나타났으며, SEM 관찰 결과 평균입경은 $2{\sim}4\;{\mu}m$의 페로브스카이트 결정으로 균일하고 치밀한 조직을 나타내었으며, 높은 소결성은 첨가제에 의한 액상소결에 기인한다.

• 한국세라믹학회지
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• 제28권5호
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• pp.399-405
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• 1991

Mullite-PSZ powders were synthesized by the sol-gel process using Al(sec-OC4H9)3, Si(OC2H5)4, ZrOCl2$.$8H2O and YCl3 solution and the characteristics of synthesized powders were studied. The sinterability and mechanical properties of powder compacts sintered at 1670$^{\circ}C$ for 4hr were also studied for various PSZ contents. ${\gamma}$-Al2O3(Al-Si spinel) formed at 980$^{\circ}C$ from amorphous dried gel, and mullite as well as ZrO2 formed above 1200$^{\circ}C$. At the room temperature, ZrO2 was a mixture of tetragonal and monoclinic phases. The specimens were densified to 97∼98% except the specimen containing 25 vol% PSZ which showed the relative density of 94%. The K1c value increased with the PSZ content and showed a maximum value of 4.1 MN/m3/2 at 25 vol% PSZ; this value was about 50% higher than that of the mullite without PSZ. Flexural strength had a maximum value of 280 Mn/㎡ at 20 vol% PSZ. In contrast, at 25 vol%, the flexural strength was even lower than that of the mullite possibly due to higher porosity of 6%.

• 한국세라믹학회지
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• 제31권4호
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• pp.448-456
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• 1994

The reaction-sintered alumina and zirconia-alumina ceramics were fabricated from the Al/Al2O3 or Zl/ZrO2(Ca-PSZ) powder mixtures via the attrition milling. And the effects of the milling characteristics of used raw powders on reaction sintering were investigated. After attrition milling and isopressing at 400 MPa the Al/Al2O3 specimen was oxidated at 1200℃ for 8 hours followed by sintering at 1550℃ for 3 hours. Because mixed powders of flake-type Al with coarse alumina was much more effectively comminuted than the globular-type Al with coarse alumina powders, it's sintered body of more than 97% theoretical density was achived, but low contents of Al leads to relatively higher shrinkage of about 8%. And because coarse alumina particles was much more beneficial in cutting and reducing the ductile Al particles, using the coarse alumina powder was much more effective in reaction sintering. Fused Ca-PSZ powder was reaction sintered with Al at 1550℃ for 3 hours and low shrinkage ZrO2-Al2O3 composites were fabricated. But because Al/Ca-PSZ powder mixtures were not effectively milled the reaction sintering and densification was difficult. And the Ca ion in Ca-PSZ grains diffused into alumina grains during sintering so that the unstabilization of Ca-PSZ body was occured which gave the microcracks in the specimens.

• 한국재료학회지
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• 제20권7호
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• pp.379-384
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• 2010

The usual ceramic process of mixing and milling in state of oxides $ZrO_2$ and $CeO_2$ was adopted in this study in a wet process to manufacture Ce-TZP. $CeO_2$-$ZrO_2$ ceramics containing 8~20 mol% $CeO_2$ were made by heat treatment at $1250\sim1500^{\circ}C$ for 5hr. The maximum dispersion point of every slurry manufactured with a mixture of $ZrO_2$ and $CeO_2$ was neat at pH10. A stable slurry with average particle size of 90 nm can be manufactured when it is dispersed with the use of ammonia water and polycarboxylic acid ammonium. The sintered Ce-TZP ceramics manufactured with the addition of $CeO_2$ in a concentration of less than 10 mol% progressed to the fracture of the specimen due to the existence of a monoclinic phase of more than 30% at room temperature. More than 99% of the tetragonal phase was created for the sintered body with the addition of $CeO_2$ beyond 18 mol%, but the degradation of the mechanical properties on the entire specimen was brought about due to the $CeO_2$ existing in a percentage above 3%. Consequently, the optimal Ce-TZP level combined in the oxide state was identified to be 16 mol% of $CeO_2$ contents.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 1998년도 추계학술대회 논문집
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• pp.311-314
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• 1998

The effects of the additions of transition metal oxides on ZrO$_2$ - Y$_2$O$_3$ (Y$_2$O$_3$ - containing tetragonal zirconia polycrystals : Y-TZP) system has been studied by investigating fracture toughness and phase stability of the sintered specimens. In the specimens sintered at 1450$^{\circ}C$ for 2hrs in air the phase transformation from tetragonal to monoclinic was observed. The ratios of monoclinic phase to tetragonal phase were changed with the additions of CoO, Fe$_2$O$_3$ and MnO$_2$, respectively, from 0.00 to 8.00wt%. The fracture toughness was increased with increasing the monoclinic to tetragonal phase ratio and was maximum at the ratio of about 18%. However, the hardness was decreased with increasing the ratio. The additions of CoO, Fe$_2$O$_3$ and MnO$_2$ together into Y-TZP resulted in more complex behaviors of fracture toughness and hardness. The specimen with the additions of 1.5wt% Fe$_2$O$_3$, 3.0wt% Al$_2$O$_3$ and 1.5wt% CoO showed the monoclinic to tetragonal phase ratio of 18% and the highest toughness of 10.8 MPa.m$\^$$\frac{1}{2}$/ and Vickers hardness of 1201kgf/mm$^2$.

• 한국세라믹학회지
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• 제16권3호
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• pp.155-163
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• 1979

This study was to explore the characteristics of 6 mole% CaO stabilized $ZrO_2$ prepared by wet chemical methods. The results of the experiments were as follows: 1. The powder calcined at 1000$^{\circ}$-110$0^{\circ}C$ was partly agglomerated. The morphology of agglomerate was spherical of 0.5-1$\mu{m}$ in size for Hot Petroleum Drying Method, chain-like of 1-2$\mu{m}$ for Freeze Drying Method, and irreqular of 2-3$\mu{m}$ for Coprecipitation Method. 2. Optimum calcining conditions for powder prepared by wet chemical methods were found: 110$0^{\circ}C$, 2h in air for Hot Petroleum Drying Method and Freeze Drying Method, and 100$0^{\circ}C$, 2h in air for Coprecipitation Method. 3. When specimen was calcined at 1000$^{\circ}$-110$0^{\circ}C$ in air for 2h and then sintered at 1$600^{\circ}C$ in air for 4h, the specimens prepared by wet chemical methods showed a high sintered density (94% of theoretical density) and a low open porosity (<0.8%); however, the sintered density of the specimen prepared by Oxide Wet Mixing Method was 90%. 4. The amount of cubic phase of sintered body prepared by wet chemical methods was observed to be higher than the one prepared by Oxide Wet Mixing Method. 5. It was found that Hot petroleum Drying Method, Freeze Drying Method and Coprecipitation Method were nearly the same in respect of the results of stabilization grade and sintered density of CaO-stabilized $ZrO_2$.

• 한국재료학회지
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• 제7권9호
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• pp.772-780
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• 1997

Zr-Nb-Sn 의 3원계 합금에서 Sn 함량 변화가 부식에 미치는 영향과 석출물 특성에 미치는 영향을 평가하여 신합금 개발을 위한 Sn의 최적 함유량을 도출하고자 Zr-0.4Nb-xSn(x=0.4,0.8, 1.2, 1.6)계의 4종 합금을 제조하여 여러 가지 특성시험을 실시하였다. 부식특성은 42$0^{\circ}C$ steam(1500psi)조건의 autoclave를 이용하여 시험하였으며 부식과정에서 발생하는 무게증가량을 측정하였고 산화막 특성은 X-ray를 이용하여 조사하였다. 부식관점에서 Sn량이 적을수록 내식성은 증가하는 경향을 보였다. 즉, 0.4Sn합금에서 가장 낮은 무게증가량과 1.6Sn 합금에서 가장 높은 무게 증가량을 보였다. 그러나 수소흡수성면에서는 Sn량이 많을수록 수소흡수율이 작아지는 경향을 보였다. 산화막내에서 tetra-ZrO$_{2}$량은 Sn량이 많을수록 적게 나타나는데, 이같은 결과로부터 Sn량이 많을수록 tetra-ZuO$_{2}$에서 mono-ZrO$_{2}$로의 상변태가 가속되어 Sn이 많이 함유된 합금에서 부식 저항성은 저하된다고 사료된다. Sn량이 증가함에 따라 강도는 점차적으로 증가하는 경향을 보였다. Sn량 변화에 따른 석출물의 특성을 조사한 결과, Zr-0.4Nb-xSn계 합금에서는 Sn이 석출물 형성에 거의 영향을 미치지 않으며, 또한 석출물 크기도 내식성에 커다란 영향을 미치지 않는 것을 확인하였다.