• Korean Chemical Engineering Research
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• 제57권1호
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• pp.133-141
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• 2019

침전법으로 환류방법 또는 수열합성법을 이용하여 산 염기점을 갖는 고비표면적 지르코니아를 합성하였다. 제조된 지르코니아는 침전제로 수산화암모늄 수용액을 사용하여 Zr 용액의 pH를 2에서 10 범위 내에서 조절하였으며 질소흡착분석, X-선 회절분석(XRD), 이소프로판올 승온탈착법(IPA-TPD), 주사전자현미경 분석, X-선 광전자분광분석, 산-염기점 분석을 통해 IPA 분해반응의 촉매활성과 연관하여 특성분석을 수행하였다. 환류방법을 사용할 시, tetragonal 상이 높은 지르코니아를 얻기 위해서는 Zr 용액의 pH가 높아야 하며, pH 9 이상에서는 순수한 tetragonal 상의 지르코니아 합성이 가능하였다. 또한, 비표면적이 큰 지르코니아를 얻기 위해서는 높은 pH가 요구되었으며, pH 10에서 합성한 경우에는 $600^{\circ}C$에서 소성 후에도 $260m^2g^{-1}$의 높은 비표면적이 얻어졌다. 하지만 같은 조건 하에서 고압이 수반되는 수열합성에는 $40m^2g^{-1}$ 이하의 매우 낮은 비표면적을 보였으며, monoclinic 상의 지르코니아가 합성되었다. 고 비표면적 tetragonal 상의 지르코니아를 얻기 위해서는 용액의 pH가 가장 큰 영향을 미쳤으며, 용액의 pH와 무관하게 높은 압력이 필요한 수열합성에서는 monoclinic 지르코니아가 생성되었으며 상대적으로 비표면적이 낮게 나타났다. 높은 비표면적과 tetragonal 상을 갖는 지르코니아는 염기점에 비해 산점이 우세하여 IPA 분해반응에서 선택적 탈수반응만 진행되는 프로필렌만 생성되었다.

• 한국재료학회:학술대회논문집
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• 한국재료학회 1994년도 추계 학술발표 강연 및 논문 개요집
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• pp.138-139
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• 1994

• 한국세라믹학회:학술대회논문집
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• 한국세라믹학회 2003년도 추계총회 및 연구발표회 초록집
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• pp.48.2-48
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• 2003

• 한국분말재료학회지
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• 제8권2호
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• pp.98-103
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• 2001

Metallic tin powder with diameter less than 50 nm was synthesized by inert gas condensation method and subsequently oxidized to tin oxide ($SnO_2$) along the two heat-treatment routes. The $SnO_2$ powder of single phase with a tetragonal structure was obtained by the heat-treatment route with intermediate annealing step-wise oxidation, whereas the $SnO_2$ powder with mixture of orthorhombic and tetragonal phases was obtained by the heat-treatment route without intermediate annealing (direct oxidation). $SnO_2$ gas sensors fabricated from the nano-phase $SnO_2$ powders were investigated by structural observations as well as measurement of electrical resistance. The $SnO_2$ gas sensors fabricated from the mixed-phase powder exhibited much lower sensitivity against $H_2$ gas than those fabricated from the powder of tetragonal phase. Reduced sensitivity of gas sensors with the new orthorhombic phase was attributed to detrimental effects of phase boundaries between orthorhombic and tetragonal phases and many twin boundaries on the charge mobility.

• 한국세라믹학회지
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• 제40권6호
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• pp.513-518
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• 2003

La/sub 2/3-x/Li/sub 3x/□/sub 1/3-2x/TiO₃ compounds with x=0.13 and 0.12 were prepared by slow cooling (x=0.13) and rapid quenching (x=0.12) into the liquid nitrogen after sintering at 1350℃ for 6 h. Their crystal structure has been determined by Rietveld refinement of both the powder neutron and X-ray diffraction data. From neutron diffraction data, we found that the main phase was not tetragonal (P4/mmm), but trigonal (R3cH). The refinement of neutron diffraction for the slow cooled samples were in a good agreement with a new model; a mixture of trigonal (R3cH, 45.7 wt％), tetragonal (p4/mmm, 37.0 wt％), and Li/sub 0.57/Ti/sub 0.86/O₂(pbnm, 17.2 wt%), but the quenched sample was found not to contain tetragonal (p4/mmm). X-ray diffraction data couldn't be well fitted because of the Poor scattering factor of lithium ions and the similar reflection patterns among trigonal (R3cH), tetragonal (p4/mmm), and cubic (Pm3m). We also knew that one transport bottlenecks is destroyed by one La vacancy in the case of trigonal (R3cH).

• 한국세라믹학회지
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• 제27권2호
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• pp.233-243
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• 1990

For theinvestigation of MgO addition effect on 12Ce-TZP ceramics, MgO-CeO2-ZrO2 ceramics was fabricated using commercial powders under sintering condition of 130$0^{\circ}C$-1$600^{\circ}C$ for 2hr. Fully tetragonal phase could be obtained by proper heat treatment and MgO addition amount. Minor cubic phase was appeared in relatively high MgO content composition at each sintering temperature. As alloying amount of MgO increased, tetragonal stability increased and grain size decreased. Grain size dependence on MgO content was verified by SEM observation of fractured surface. Surface bloating was observed from the 2 m/o to 6m/o in the temperature range of 150$0^{\circ}C$ to 1$600^{\circ}C$. In spite of very porous microstructure owing to surface bloating, 100% TZP could be maintained in 2.0m/o MgO composition by heat treatment of 150$0^{\circ}C$. This result indicated that MgO was more powerful stabilizer than CeO2. Mechanical proprties of MgO-CeO2-ZrO2 ceramics were consistent with the stability observation of tetragonal phase very well.

• 한국세라믹학회지
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• 제45권3호
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• pp.139-141
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• 2008

The piezoelectric properties of tetragonal 0.88Pb$(Zn_{1/3}Nb_{2/3)O_3-0.12PbTiO_3$ single crystals are characterized along the <111> direction, which composed the engineering domain configuration in the tetragonal phase. The <111>-oriented crystal possessed smaller $d_{33}$ values compared to the crystal along the <001> spontaneous polarization direction. Based on phenomenological theory, it is shown that the engineering domain configuration does not enhance the piezoelectric constant in tetragonal 0.88Pb$(Zn_{1/3}Nb_{2/3)O_3-0.12PbTiO_3$ single crystals. In addition, the electrostrictive coefficients of $Q_{12}=-0.03706m^4/C^2,\;Q_{11}=0.10765m^4/C^2,\;and\;Q_{44}=0.02020m^4/C^2$ of tetragonal 0.88PZN-0.12PT single crystals were calculated.

• 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.

• The Korean Journal of Ceramics
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• 제4권4호
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• pp.297-303
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• 1998

The effect of aliovalent dopants, $ Nb_2O_5$ and MnO, on the phase stability of 12 mol% ceria partially-stabilized zirconia (Ce-TZP) polycrystals was studied. Both dopants (MnO and $ Nb_2O_5$) significantly increased the stability of the tetragonal zirconia phase (Mb temperature lower than liquid nitrogen temperature). The enhancement of the stability of the tetragonal phase in Ce-TZP doped with 1 mol% of Mno(Ce-TZP/MnO) andCe-TZP doped with 1 mol% of $ Nb_2O_5$(Ce-TZP/$ Nb_2O_5$) were explained by the significant reduction of the driving force, -${\Delta}$Gchem, for the tetragonal-to-mono-clinic phase transformation caused by the addition of MnO and $ Nb_2O_5$. The enhanced stability of the tetragonal phase in the Ce-TZP and Al2O3 composite (Ce-TZP/$Al_2O_3$) is believed to be caused by smaller grain size, moderate reduction in the chemical driving force and increase in the strain energy barrier to the transformation. Mechanical properties of the Ce-TZP and the Ce-TZP/$Al_2O_3$ with (i) the same grain size and (ii) the same Mb temperature were examined by measuring stress-strain behavior in 3 point bending. The Ce-TZP/$Al_2O_3$ composite doped with 1.3w% MnO (Ce-TZP/$Al_2O_3$/MnO), which had the same grain size as the Ce-TZP and De-TZP/$Al_2O_3$ showed more transformation plasticity than either the Ce-TZP or the Ce-TZP/$Al_2O_3$ composite. The Ce-TZP wihch had the same Mb temperature as that of the Ce-TZP/$Al_2O_3$/MnO did not show any transformation plasticity.

• 한국재료학회지
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• 제2권5호
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• pp.320-329
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• 1992

2mol%의 이트리아로 안정화된 정방정상 지르코니아 분말을 80$0^{\circ}C$부터 150$0^{\circ}C$ 까지 온도별로 열처리하여 분말내 입자크기 및 입자간에 존재하는 구속력을 변화시킨 다음, 정방정상의 전이도 및 안정화효과가 무열상전이, 응력유기상전이, 등온상전이 에 미치는 영향을 고찰하였다. 그 결과 Y-TZP 분말내 정 방정상의 전이도는 고용체의 양이 일정할 경우 열처리온도의 변화에 따른 입자크기와 입자간에 존재하는 구속력의 크기에 의존하였는데 열처리온도가 증가함에 따라 전이도가 점차 증가하여 130$0^{\circ}C$로 열처리한 분말에서 최대값을 보였다. 그러나 130$0^{\circ}C$ 이상으로 열처리한 분말에서는 열처리온도가 증가함에 따라 구속효과의 증가에 따라 전이도가 정차로 감소하였다. 전이도가 큰 분말에서는 정방정상이 무열상전이, 응력유기상전이, 등온상전이를 쉽게 일으켜 단사정상으로 전이하였다.