$Al_2O_3$로 피복시킨 세라믹 복합분체의 제조 및 특성: (III) $Al_2O_3-ZrO_2$ 복합분체

현상훈,이지현,송원선 한국세라믹학회 1992 한국세라믹학회지 Vol.29 No.8

The alumina-zirconia composite powders of core particle ZrO2 coated with Al2O3 were prepared by the hydrolysis-deposition of the mixed aluminum salt solution of Al2(SO4)3-Al(NO3)3-Urea. The effects of hydrolysis reaction and coating parameters on characteristics of coated powders and composites were also investigated. The degree of coating could be estimated from the ratio of tetra-/mono-ZrO2 present at the room temperature after heat-treating coated powders at 120$0^{\circ}C$ and the result of TEM observations. When the content of ZrO2 in the dispersed coating system, the coating time, and the volume ratio of water/solution were 50 mg/g, 180 min, and 5, respectively the coating efficiency was maximum (the ratio of tetra-/mono-ZrO2 was 87/13). The relative densities of coated Al2O3-ZrO2 composites sintered at 1$650^{\circ}C$ for 4 hrs were about 91~98% and the maximum ratio of tetra-/mono-ZrO2 in Al2O3-20wt% ZrO2 composites was 62/38.

졸-겔법에 의한 $\gamma-LiAlO_2$ 단섬유의 제조

현상훈,이재현,홍성안 한국세라믹학회 1996 한국세라믹학회지 Vol.33 No.10

Discontinuous ${\gamma}$-LiAlO2 fibers for fiber-reinforcing MCFC matrixes have been produced by the sol-gel process using the centrifugal spinning apparatus of the Rotary type. Gel fibers could be obtained through spinning of stable LiAlO2 complex polymetric sols under the optimum spinning conditions (hollow-disc rotating velocity 9000 rpm sol feeding rate of 4ml/min flowing N2 temperature of 4$0^{\circ}C$ and flowing N2 pressure of 4 bar). It was found that defect free and densified ${\gamma}$-LiAlO2 fibers with the relative density of 98% and the mean diameter of 4.7${\mu}{\textrm}{m}$ were prepared when the spinned fibers were heat-treated to 100$0^{\circ}C$ on the specified heating schedule. in particular the mean diameter and length of fibers could be controlled by the pressure of flowing N2 and the chopping-sieving method respectively.

기체분리용 세라믹 복합분리막의 개발 : V. 가압 졸-겔 코팅법에 의한 rrmaltp입자 실리카 막의 합성

현상훈,윤성필,김준학 한국세라믹학회 1993 한국세라믹학회지 Vol.30 No.3

A new pressurized sol-gel coating technique forming membrane layers inside pores of the porous support by the simple operation has been developed. Crack-free and reproducible nanoparticulate silica membranes supported on the porous $\alpha$-alumina tube are synthesized by pressurized coating at 600kPa for 2hr. The pore radius and N2 gas permiability at the room temperature of silica membrane layers are 8$\AA$ and 7.0$\times$10-7mol/$m^2$.s.Pa, respectively. The mechanism of N2 gas transfer through synthesized membrane layers is the perfect Knudeen flow, and the thermal stability of the silica composite membranes is excellent upto 40$0^{\circ}C$.

용융탄산염 연료전지용 화이버 강화 $\gamma$-LiAlO$_2$ 매트릭스의 적층에 의한 강도 증진

현상훈,조성철,홍성안 한국세라믹학회 1999 한국세라믹학회지 Vol.36 No.2

용융탄산염 연료전지(Molten Carbonate Fuel Cell)용 알루미나 화이버 강화 ${\gamma}$-LiAlO2 매트릭스의 적층방법에 따른 미세구조 변화 및 강도 증진 효과에 대하여 연구하였다. 테이프 캐스팅법으로 제조한 green sheet 2장을 45$^{\circ}C$에서 1kg/$ extrm{cm}^2$의 압력으로 1분간 hot pressing 하여 제조한 적층 매트릭스와 double casting 시 1단계 캐스팅한 green sheet를 3.5 시간 정도 건조한 뒤 2 단계 캐스팅 하여 제조한 적층 매트릭스의 기공율은 모두 50% 이상이었다. 알루미나 화이버 강화 적층 매트릭스의 강도는 비적층 매트릭스(115gf/$ extrm{mm}^2$)에 비해 70% 이상 증진되었으며 적층에 의해 화이버 배향성에 따른 강도의 편향성을 제거할 수 있었다. Triple casting에 의한 적층 메트릭스의 강도는 double casting 시에 비해 약간 증진되었으나 캐스팅 방향에 따른 강도의 편향성이 존재할 뿐만 아니라 기공율도 50% 이하였다. Double casting에 의한 적층 매트릭스의 강도 (195 gf/$\textrm{mm}^2$)는 hot pressing 하여 제조한 매트릭스 (212gf/$\textrm{mm}^2$)에 비해 약간 낮지만 MCFC 매트릭스 제조공정 면에서 double casting 법이 효율적인 적층공정으로 평가되었다. Microstructural variation and strengthening effects with lamination methods of alumina fiber-reinforced ${\gamma}$-LiAlO2 matrixes for Molten Carbonate Fuel Cell(MCFC) were studied. The porosities of all matrix laminated by hot-pressing of two green sheets under 1 kg/$\textrm{cm}^2$ at 45$^{\circ}C$ for 1 min and by double-casting which the second layer cast on the first green sheet dried for 3.5h were more than 50%. The strength of the Al2O3 fiber-reinforced matrix prepared by lamination was enhanced by 70% in comparison with the non-laminated matrix (115 gf/$\textrm{mm}^2$) and the strength-directionality due to fiber-orientation also could be removed. The strength of matrixes laminated by triple-casting was higher than that of the double-cast matrix, but triple-cast matrix showed the directionality with the casting direction, and furthermore its porosity was less than 50%. Although the strength of matrixes laminated by double-casting (195 gf/$\textrm{mm}^2$) is slightly less than that of matrixes laminated by hot-pressing (212 gf/$\textrm{mm}^2$), the double-casting method was evaluated to be more efficient laminating process in MCFC matrix processing.

세라믹 멤브레인의 현황과 제법

현상훈 한국막학회 1993 멤브레인 Vol.3 No.1

막분리 공정의 응용범위 및 시장규모가 증가함에 따라 최근 기능성 멤브레인의 개발에 대한 많은 연구가 시도되고 있으나 아직까지도 매우 한정된 범위의 유기질 분리막만이 실용화되고 있을 뿐이다. 막분리 공정의 응용성은 분리막의 특성에 의하여 좌우될 수 있는데 현재 주로 사용되고 있는 유기질막은 열적, 기계적, 화학 및 생물학적 안정성이 낮고 세척에 의한 재생성이 용이하지 않기 때문에 차후 이들을 대체하여 모든 조업조건하에서 효율적으로 장기간 사용될 수 잇는 세라믹 멤브레인의 개발이 요구되고 있는실정이다. 특히 2000년도 초반부터는 종래의 유기질막으로서는 기대할 수 없는 고기능성을 부여할 수 있는 세라믹 멤브레인의 공업적 수요가 급증하여 분리막 공정에서 상당한 비중을 점유하게 될것으로 예상되고 있으나 현재 막의 제조 및 응용에 대한 기술이 확립되어 있지 않아서 공업적인 실용화가 이루어지지 못하고 있다.

$TiO_2$ 복합 분리막의 제조를 위한 졸-겔 코팅공정 분석

현상훈,최영민 한국세라믹학회 1992 한국세라믹학회지 Vol.29 No.5

The titania membrane thickness coated on the porous alumina support by the sol-gel method was analyzed using the slipcasting model. The thickness of calcined membrane layers increased linearly from 1.3 to 3.8 ${\mu}{\textrm}{m}$ with the square root of the dipping time (4~40 min). Growth rates of the thickness of wet gels and calcined layers were well described quantitatively by the slipcasting model. Through the regression of experimental data using model equations, the permeability and the pressure drop across wet gels, and the thickness and their growth rate constants of wet gels and calcined layers could be determined. It was also known that the gellation concentration of the TiO2 sol used in this work and the porosity of wet gel layes were 25 mol/ι and 0.53, respectively.

$NH_3-AlCl_3-H_2$ 기상반응계의 열역학적 평형조성 및 고순도 AIN 합성

현상훈,김준학 한국세라믹학회 1986 한국세라믹학회지 Vol.23 No.1

The synthesis of high-purity AlN by a vapor-phase reaction was investigated using the $NH_3-AlCl_3-H_2$ reacting system. The theoretical yields of AlN were determined from th thermodynamic equilibrium composi-tions. It was shown that the yields above 90% could by obtained even in the range of relatively low temper-ature of 600-1200K. The reaction temperature and the initial amounts/ratios of the reacting gases showed significant effects on the yields but the total pressure did not. The experimental results showed that a high-purity AlN having a needle shape was the only product as a solid phase and its amount produced increased with the reaction temperature. While the degree of agglmera-tion of the synthesized AlN increased with the reaction temperature the size of each particle consisting of the agglomerates was independent of the temperature but grew from 0.09 to 0.115${\mu}{\textrm}{m}$ with the flow rate of NH3. These experimental results were compared with the theoretical aspects for the synthesis of a high-purity AlN.

테이프캐스팅법에 의한 화이버 강화 $\gamma-LiAlO_2$ 메트릭스의 제조

현상훈,백계현,홍성안 한국세라믹학회 1997 한국세라믹학회지 Vol.34 No.3

용융탄산염 연료전지(Molten Carbonate Fuel Cell) 메트릭스의 성형성 및 강도 증진을 위한 알루미나/${\gamma}$-LiAlO2 화이버 강화 매트릭스에 대하여 연구하였다. ${\gamma}$-LiAlO2 입자에 10~30wt%의 화이버를 첨가한 슬러리를 테이프캐스팅 한 후 $650^{\circ}C$까지 열처리하여 두께가 500~600$\mu\textrm{m}$인 MCFC 매트릭스를 제조하였다. 화이버의 첨가량이 증가할수록 매트릭스의 기공율은 감소하였으나 입자크기가 대략 50$\mu\textrm{m}$인 ${\gamma}$-LiAlO2 분체의 첨가비를 50wt%까지 증가시킴으로써 MCFC 매트릭스에 적합한 기공율(50~60%)을 얻을 수 있었다. 알루미나 화이버의 첨가량이 20wt% 이고 길이가 250$\mu\textrm{m}$이하인 화이버를 사용하였을 때 매트릭스내의 분산성 및 강도 증진 효과가 가장 우수하였다. 반면에 본 연구에서 제조한 ${\gamma}$-LiAlO2 화이버를 이용한 강화 매트릭스의 강도(156 gf/$\textrm{mm}^2$)는 알루미나 화이버 강화 매트릭스에 비해 20~40% 정도 증진되었다. 또한 알루미나 화이버 강화 매트릭스는 용융탄산염에 의하여 부식되지만 ${\gamma}$-LiAlO2 화이버 강화 매트릭스는 전혀 부식되지 않음을 알 수 있었다. To enhance the strength and formability of MCFC matrixes, alumina/${\gamma}$-LiAlO2 fiber-reinforced ${\gamma}$-LiAlO2 ma-trixes have been investigated. The MCFC matrixes with the thickness of 500~600 ${\mu}{\textrm}{m}$ were prepared by tape-casting of the slurry containing 10~30wt% fibers, followed by heat-treating up to $650^{\circ}C$. The porosity of fi-ber-reinforced matrixes decreased with the content of fibers, while the appropriate porosity(50~60%) for MCFC matrixes could be attained by adding larger ${\gamma}$-LiAlO2 particles with the diameter of about 50${\mu}{\textrm}{m}$ up to 50 wt%. The optimum length and content of the alumina fiber, both in the alignment of fibers and the enhancement of the strength, were found to be below 250${\mu}{\textrm}{m}$ and 20 wt%, respectively. On the other hand, the strength(156 gf/$\textrm{mm}^2$) of the ${\gamma}$-LiAlO2 matrix reinforced with ${\gamma}$-LiAlO2 fibers prepared in this study was improved by 20~40% in comparison with the alumina-fiber-reinforced matrix. It was also found that the alu-mina-fiber-reinforced matrix was completely corroded in molten carbonates but the ${\gamma}$-LiAlO2 was not.

극미세 입자 Aluminosilicate계 졸의 합성 및 응용 (II) Al_2O_3-SiO_2$계 혼합졸

현상훈,김승구,이성철 한국세라믹학회 1995 한국세라믹학회지 Vol.32 No.1

A crack-free ceramic composite membrane with micropores has been synthesized by the pressurized sol-gel coating technique using the mixed Al2O3-SiO2 sols. The mixed sols were prepared by mixing nanoparticulate SiO2 and boehmite sols. These sols were more stable at lower pH, but very unstable when their copositions were in the range of 50~75mol% of SiO2 at the same pH. The mixed Al2O3-SiO2 membrane prepared from the mixed sol (0.2mol/$\ell$ of solid content and pH=2) containing 40mol% of SiO2 had the mean pore radius of 0.80nm and the specific surface area of 280$m^2$/g. The nitrogen permeability through the coated Al2O3-SiO2 layer was 42$\times$107mol/$m^2$.s.Pa. It was found that the thermal stability of aluminosilicate membranes, even through similar to that of SiO2 membranes, was much improved in comparison with ${\gamma}$-alumina membranes.

기체분리용 세라믹 복합분리막의 개발: I. 극미세 입자 실리카 졸의 코팅 특성

현상훈,윤성필,Marc A. Anderson 한국세라믹학회 1992 한국세라믹학회지 Vol.29 No.6

Alumina tubes suitable for the support of gas separation membranes have been prepared by the slipcasting technique. These supports have the average pore size of 0.1 ${\mu}{\textrm}{m}$ within the narrow distribution. The sol-gel dipcoating process of nanoparticulate sols is very sensitive to microstructure of the support, and the coating on the inside surface of the tube is found to be more successful than on the outside surface. Nanoparticulate silica sols (0.82 mol/ι) have been synthesized by an interfacial hydrolysis reaction between TEOS and high alkaline water. When coating an alumina tube with these sols, the minimum limits of the particle size and the aging time required for forming the coated gel layer at the given pH are provided. It is optimum to coat the support with less concentrated sols stabilized through aging for the appropriate time (more than 22 days) at the lower pH (pH 2.0) for producing a reproducible crack free thin film coating in composite membranes.