• Korean Chemical Engineering Research
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• v.44 no.2
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• pp.160-165
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• 2006

A Pd-Cu-Ni alloyed hydrogen membrane has fabricated on porous nickel support formed by nickel powder. Porous nickel support made by sintering shows a strong resistance to hydrogen embrittlement and thermal fatigue. Plasma surface modification treatment is introduced as pre-treatment process instead of conventional HCl wet activation. Nickel was electroplated to a thickness of $2{\mu}m$ in order in to fill micropores at the nickel support surface. Palladium and copper were deposited at thicknesses of $4{\mu}m$ and $0.5{\mu}m$, respectively, on the nickel coated support by DC sputtering process. Subsequently, copper reflow at $700^{\circ}C$ was performed for an hour in $H_2$ ambient. And, as a result PdCu-Ni composite membrane has a pinhole-free and extremely dense microstructure, having a good adhesion to the porous nickel support and infinite hydrogen selectivity in $H_2/N_2$ mixtures.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.259-279
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• 1996

최근 정보·전자산업의 발전으로 고 신뢰성 전자재료에 대한 수요가 증대되고 있으며 이러한 첨단산업의 기반의 될 신소재 중 전자세라믹스가 차지하는 비중이 그 대부분을 차지하고 있으며 이에 대한 수요와 기대가 점점 커지고 있다. 이러한 전자세라믹스는 유전재료, 자성재료, 압전재료, 도전성 재료 등으로 나뉘게 된다. 어떠한 분류에 들어가든 그 조성은 금속의 산화물 형태가 일반적이며 미세한 분말의 성형체를 소결(sintering) 함으로써 최종제품으로 완성된다. 이러한 전잣라믹스가 최근 요구되는 고 신뢰성, 고 밀도화를 달성하기 위해선 원료 분말 제조단계부터 제어가 필요하다. 원료분말의 균일·균질성과 그 입도는 소결특성 뿐만아니라 전기적 특성에도 큰 영향을 미치기 때문이다. 세라믹스의 분말제조 방법 중 일반적으로 사용되는 방법으로는 고상 산화물을 혼합하여 하소(calcination)한 후 분쇄하는 '고상합성법'과 금속의 염 또는 alkoxide 용액을 이용하여 화학적으로 제조하는 '습식 화학적 합성법'이 있다. 고상합성법은 합성온도가 높고 기계적 분쇄와 혼합에 의존하므로 균일·균질성이 떨어지고 분말크기를 1㎛ 이하로 만들기 힘들다. 반면에 습식화학적 합성법은 기계적인 분쇄와 혼합에선 얻을 수 없는 원자 혹은 분자단위의 균일한 혼합과 submicron 이하의 미세한 분말을 얻을 수 있다. 따라서 이러한 습식 화학적 합성으로 얻은 분말을 사용하면 미세한 입자의 특성으로 인해 소결온도를 낮출 수 있으며 균일한 미세구조와 균질한 조성을 갖게되어 기계적·전기적 물성증진도 가져올 수 있게 된다. 습식 화학적 분말합성법은 전술하였듯이 alkoxide의 가수분해를 이용하는 sol-gel 법과 금속의 염(salt) 용액을 이용하여, 화학적으로 화합물 침전을 얻거나 또는 공침전물(coprecipitate) 형태의 분말을 얻는, 침전법으로 나뉠 수 있다. 침전법의 근본원리는 pH 및 pCO3 등에 따른 이온종의 용해도 차이를 이용하는 것으로써 각 이온종에 따른 solubility product(ksp)를 이용하여 설명된다. 본 연구에서는 침전법을 사용한 Ba-, Pb-계 전자세라믹스의 분말합성에 대한 이론적 고찰과 공정개발 및 실험을 통한 물성증진 효과에 대해 알아보았다. 본 실험상의 전자세라믹스 조성은 강유전체, 세라믹반도체, 압효과에 대해 알아보았다. 본 실험상의 전자세라믹스 조성은 강유전체, 세라믹 반도체, 압전재료로 널리 사용되는 BaTiO3, PZT(PbZrO3-PbTiO3)와 수직 자기기록매체로 큰 가능성이 있으며 hard ferrite로 널리쓰이는 Ba-feerite(BaFe12O19)로써 수산화물 형태의 침전에 대한 기구(mechanism)와 물성에 대해 살펴보았다. 이러한 침전법에 의한 분말합성 과정에는 소결체의 물성에 영향을 미치는 pH 조절제나 원료에서 혼입될 수 있는 Na+, K+, Cl-, SO4- 등의 제거(washing 혹은 filtering)가 필수적이다. 그러나 침전법에서 얻게 되는 분말은 매우 미세하여 colloid를 형성하게 되며, 이러한 colloid 상태의 미세한 침전입자가 filtering media에 끼이게 되어 견고하면서도 상당한 부피를 가지는 filter cake을 형성하기 때문에 filtering에 많은 시간과 다량의 filtering agent (본 실험의 경우엔 증류수)가 필요하게 된다. 따라서 이러한 문제점을 해결하기 위하여 colloid 상태의 침전물을 얼렸다 녹이는 freezing process를 개발, 적용하여 그 원리 및 효과, 그로인한 분말형태를 관찰하여 보았다.

• Membrane Journal
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• v.21 no.1
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• pp.55-61
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• 2011

$BaCo_{0.7}Fe_{0.22}Nb_{0.08}O_{3-{\delta}}$ oxide was synthesized by solid state reaction method. Dense ceramic membrane was prepared using as-prepared powder by pressing and sintering at $1,200^{\circ}C$. XRD result of membrane showed single perovskite structure. Leakage and oxygen permeation test were conducted on the membrane sealed by glass ring as a sealing material. The oxygen permeation flux increased with increasing temperature and pressure difference and maximum oxygen permeation flux was $2.3mL/min{\cdot}cm^2$ at $950^{\circ}C$ with $Po_2$ = 0.63 atm of oxygen partial pressure. The oxygen permeation in the condition of air with $CO_2$ (300 ppm) as feed stream decreased as much as only maximum 2.9% in comparison with air feed stream. It indicated $BaCo_{0.7}Fe_{0.22}Nb_{0.08}O_{3-{\delta}}$ membrane is more stable than another membrane for carbon dioxide.

• Journal of the Korean Ceramic Society
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• v.39 no.9
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• pp.846-850
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• 2002

A PMN-PT-BT/Ag composite was prepared by surface modification with MgO sol with hoping to suppress silver's migration during sintering. The mixture of PbO, $N_2O_5,\;TiO_2\;with\;Mg(NO_3)_2$ instead of MgO was ball milled, the solvent was removed and then the dried powders were calcined at 950$^{\circ}C$/1h. The calcined powder were treated with 3.0 mol% $Ag_2O$ and 1.0 wt% MgO sol and calcined at 550$^{\circ}C$/1h. The dielectrics sintered at 1000$^{\circ}C$/4h under a flowing oxygen showed the density of 7.84g/$cm^3$, the room temperature dielectric constant of 18400, the dielectric loss of 2.4%, the specific resistivity of $0.24{\times}10^{12}{\Omega}{\cdot}cm$. It also showed the bending strength of $120.7{\pm}11.26$ MPa and the fracture toughness of $0.87{\pm}0.002\;MPam^{1/2}$ which were comparable to commercial PZT. The microstructure sonsisted of grains of ∼4${\mu}m$. SEM and SIMS analysis showed that Ag grew as ∼1${\mu}m$ and excess MgO as ∼0.5${\mu}m$.

• Membrane Journal
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• v.25 no.5
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• pp.415-421
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• 2015

$SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ oxide was synthesized by solid state reaction method. Dense ceramic membrane was prepared using as-prepared powder by pressing and sintering at $1250^{\circ}C$. XRD result of membrane showed single perovskite structure. The oxygen permeability were measured under 0.21 atm of oxygen partial pressure ($P_{O_2}$) and between 800 and $950^{\circ}C$. The oxygen permeation flux of $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ membrane was increased with the increasing temperature. The maximum oxygen permeation flux was $1.839mL/min{\cdot}cm^2$ at $950^{\circ}C$. Long period permeability experiment was carried out to confirm the phase stability and $CO_2$-tolerance of membrane containing Nb in the condition of air with $CO_2$ (500 ppm) as feed stream at $900^{\circ}C$. The phase stability and $CO_2$-tolerance of $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ were investigated by XRD and TG analysis. The result of $SrCo_{0.8}Fe_{0.1}Nb_{0.1}O_{3-{\delta}}$ which exposed carbon dioxide for 100 hours indicated 8wt% of $SrCO_3$. But it was known that the level of $SrCO_3$ production dose not have a significant effect on oxygen permeability.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.5
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• pp.203-207
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• 2019

Calcium phosphates such as hydroxyapatite (HAp), tricalcium phosphate (${\beta}$-TCP), and biphasic calcium phosphate (BCP, HAp/${\beta}$-TCP) have been prepared via hydrothermal treatment. The synthesis was conducted by reacting ($Ca(OH)_2$) aqueous solution with phosphoric acid ($H_3PO_4$) under different hydrothermal synthesis conditions (temperatures up to $150^{\circ}C$ and pH lower than 12). The effects of initial precursor Ca/P ratio (1.30, 1.50 and 1.67) and post heat treatment on the phase evolution behavior of the powders and sintered ceramics were investigated. The phases of resulting powders and sintered ceramics were controllable by adjusting the initial Ca/P ratio. A single HAp phase without any noticeable second phase was obtained for the initial Ca/P ratio of 1.67 in the overall heat treatment range. Pure ${\beta}$-TCP and biphasic calcium phosphate (HAp/${\beta}$-TCP) were synthesized from precursor solutions having Ca/P molar ratios of 1.30 and 1.50, respectively, after having been heat treated at $900^{\circ}C$ or higher. Dense ceramics with translucency were obtained at considerably lower sintering temperatures.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.4
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• pp.136-142
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• 2022

The crystal structure, grain growth behavior, and dielectric properties of BaTiO₃ have been studied with the addition of Dy₂O₃. The powders were synthesized at ratios of (100-x)BaTiO₃-xDy₂O₃ (mol%, x = 0, 0.5, 1.0, 2.0) by a conventional solid-state synthesis, and the powder compacts were sintered at 1250℃ for 2 hours in air. As the amount of added Dy₂O₃ was increased, the crystal structure of the sintered samples changed from a tetragonal to a pseudo-cubic structure, and the tetragonality decreased. In addition, a secondary phase of Ba₁₂Dy_4.67Ti₈O₃₅ appeared when Dy₂O₃ was added. The average grain size after sintering decreased and abnormal grains appeared as the amount of Dy₂O₃ increased. It can be explained that the grain growth behavior of the Dy₂O₃ added-BaTiO₃ occurs due to the two-dimensional nucleation and growth, and is governed by the interface reaction. Further, the correlation between crystal structure, microstructure, and dielectric properties was discussed.

• The Journal of Korean Academy of Prosthodontics
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• v.48 no.2
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• pp.143-150
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• 2010

Purpose: The purpose of this study is to fabricate the new zirconia block (CNU block) and to evaluate fit of core and porcelain veneered zirconia crown. Material and methods: The experimental blocks were fabricated from the commercial ytrria-stabilized zirconia powder (KZ-3YE Type A). The powder was uniaxial pressing and the green bodies were conducted using the Cold Isostatic Pressing. The zirconia blocks were presintered at $1040^{\circ}C$ and the final sintering was performed at $1450^{\circ}C$. The Kavo Everest ZS $blank{(R)}$ (KaVo, Biberach/ $Ri{\beta}$.) was used as a control group. The linear shrinkage of CNU block and Kavo block were compared. Twenty-one cores for porcelain veneered crowns were fabricated with CAD/CAM system ($Everest{(R)}$, Biberach/ $Ri{\beta}$.). Group I; seven cores fabricated from Kavo blocks, Group II; seven cores fabricated from CNU blocks, Group III; seven cores from CNU blocks and porcelain veneering for crowns. All specimens were cemented and sectioned into two planes; diagonal and bucco-lingual. The measurement of the marginal, internal, and occlusal fit was carried out using SEM ($S-4800^{(R)}$) at $30{\times}$. The results were analyzed by one-way ANOVA test. Results: The linear shrinkage of the CNU block and the KaVo block was 19.00% and 20.09%. The marginal gap of cores ($29.67{\pm}6.58{\mu}m$) fabricated from CNU blocks showed significantly smaller than that of the cores of Kavo blocks ($36.84{\pm}7.18{\mu}m$) (P < .05). The internal gaps of the porcelain veneered crowns ($32.23{\pm}6.33{\mu}m$) were larger than those of the other two groups ($37.57{\pm}6.81{\mu}m$ and $38.14{\pm}6.81{\mu}m$). Conclusion: No statistically significant difference was found in between experimental groups and control group. The experimental groups in marginal gap showed significantly smaller than the control group.

• Journal of the Korean Ceramic Society
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• v.34 no.2
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• pp.145-156
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• 1997

ZrO2 phase transformations depending on the type and amount of dopants and the sintering temperatures were studied for the 2 components (CaO-, Y2O3-, MgO-ZrO2) and the 3 components(MgO-ZrO2-Al2O3)ZrO2 powder by X-ray diffraction and Raman spectroscopy. In the CaO- and Y2O3-ZrO2 systems, as the CaO and Y2O3 contents increased to 6~15mol% and 3~15mol% respectively, we were not able to identify between tetragonal and cubic in the X-ray diffraction patterns. On the other hand, all Raman modes shifted to lower wavenumbers, decreasing in intensity and the number of bands, markedly. These phenomena were caused by tetragonallongrightarrowcubic phase transformation and interpreted by the breakdown of the wave vector selection rule(k=0) and the structural disorder associated with the formation of oxygen sublattice which was caused by the substitution between Zr4+ ion and Ca2+ or Y3+ ion in ZrO2 matrix. The monoclinic to cubic phase transformation occurred in 10mol% MgO-ZrO2 system. As the Al2O3 content increased from 0 to 20mol% in the MgO-ZrO2-Al2O3 systems, cubic phase transformed to monoclinic phase, this is because the MgO didn't play a role in a stabilizer because of the formation of the spinel(MgAl2O4) by the reaction between MgO and Al2O3, Also, the ZrO2 phase transformation was explained by the change of it's lattice parameters depending on the type and amount of dopants. Namely, as the amount of dopant increased to 10~13mol%, the axial ra-tio c/a came close to unity with increasing the lattice parameter a and decreasing the lattice parameter c. At that time, the tetragonallongrightarrowcubic phase transformation occurred.

• The Journal of Korean Academy of Prosthodontics
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• v.49 no.1
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• pp.73-79
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• 2011

Purpose: The aim of this study was to evaluate the effect of repeated firings on the color of zirconia restoration with different shading method. Materials and methods: Three different types of zirconia frameworks (adding metallic pigments to the initial zirconia powder before sintering (Group NM), dipping the milled frameworks in dissolved coloring agents (Group KI), or application of liner material to the sintered white frameworks (Group KW) were used to support A3 shade dentin porcelain. Repeated firings (3, 5, or 7) were performed, color differences among ceramic specimens were measured using a colorimeter. Repeated measurements analysis of variance (ANOVA) was used to analyze the data for significant difference. The Tukey Honestly Significant Different (HSD) test was used to perform multiple comparisons (${\alpha}$ = .05). Results: 1. $L^*a^*b^*$ values of the ceramic systems were affected by the number of firings (1, 3, 5 or 7 firings) (P < .001) and shading methods (P < .001). 2. As the number of firings increased, the $L^*$ (for all groups) and $a^*$ value (for KW and NM groups) decreased and the $b^*$ value(for all groups) increased. 3. The mean color differences caused by repeated firings were perceptible (${\Delta}E$ > 1) for group KW and KI fired after 3 times, except for group NM fired after 7 times. 4. In order of decreasing ${\Delta}E$ value fired after 7 times, the values were group KI(${\Delta}E$ = 2.26) > group KW (${\Delta}E$ = 1.47) > group NM (${\Delta}E$ = 1.08) (P < .001). Conclusion: Repeated firings influenced the color of the zirconium-oxide all-ceramic specimens with different shading methods.