실리카 에어로겔 박막의 극저 유전특성

현상훈,김중정,김동준,조문호,박형호 한국세라믹학회 1997 한국세라믹학회지 Vol.34 No.3

극저 유전특성을 갖는 SiO2 에어로겔의 박막화의 층간 절연막으로써의 응용성이 연구되었다. 점도가 10~14cP인 SiO2 폴리머 졸을 이소프로판을 분위기 하에서 1000~7000m으로 p-Si(111) 웨이퍼 상에 스핀코팅한 습윤겔 박막을 25$0^{\circ}C$와 1160 psing 조건에서 초임계건조하여 0.5 g/㎤ 정도의 밀도(78% 기공율) 와 4000~21000$\AA$ 범위의 두께를 갖는 SiO2 에어로겔 박막을 제조하였다. 박막의 두께와 미세구조를 제어할 수 있는 주요 인자는 졸의 농도, 회전속도 및 습윤겔 숙성시간임을 알 수 있었다. SiO2 에어로겔 박막의 유전상수 값은 giga급 이상의 차세대 반도체 소자에 충분히 응용될 수 있을 정도로 낮은 2.0 정도이었다. The thin film processing and the applicability as a IMD material of SiO2 aerogels providing ultralow dielec-tric properties were studied. The SiO2 aerogel films with 0.5g/㎤ density (78% porosity) and 4000~21000$\AA$ thickness could be prepared at 25$0^{\circ}C$ and 1160 psig by supercritical drying of wet-gel films, which were spin-coated at the spin rate of 1000~7000 rpm on p-Si(111) wafer under the isopropanol atmosphere. The optimum viscosity of polymeric SiO2 sols for spin coating was in the range of 10~14 cP. The main fac-tors being able to control the film thickness and microstructures were found to be sol concentration, spin rpm, and aging time of wet-gel films. The dielectric constant of the SiO2 aerogel thin film was around 2.0 low enough to be applied to the next generation semiconductor device beyond the giga level.

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.

$NH_3-AlCl_3-H_2$ 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.

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.

순수/불투명화 실리카 에어로겔의 기계적 강도 및 열전도도

현상훈,이찬호,김동준,성대진 한국세라믹학회 1997 한국세라믹학회지 Vol.34 No.9

The properties of microstructure, hydrophobicity/hydrophilicity, mechanical strength, and thermal conduction of pure/opacified silica aerogels synthesized by the sol-gel supercritical drying technique were investigated. The hydrophobic surface of opacified silica aerogels doped with carbon (0.13 g/cm3 density, 94% porosity, 580 m2/g specific surface area) transformed to hydrophilic surface after heat-treated above 30$0^{\circ}C$. The values of compressive modulus (1.85 MPa) and strength (0.5 MPa) of opacfied silica aerogels were about 20 times higher than those of pure silica aerogels. The mechanical properties of pure silica aerogels heat-treated at $700^{\circ}C$ were also considerably improved without changing their porosity and density. Particularly, compressive modulus and compressive strength of pure silica aerogels GPSed under 100$0^{\circ}C$ and 80 bar were improved 140 and 37 times, respectively. Thermal conductivities of pure/opacified silica aerogels measured at room temperature and 227$^{\circ}C$ were about 0.013 and 0.019 W/m.K, respectively, and were to be found very low value of 0.004 W/m.K below 10 torr pressure at room temperature.

$TiO_2$ 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.

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.

실리카 졸 침투법을 이용한 $ZrO_2/Al_2O_3-Mullite$ 복합체의 제조

현상훈,최지영 한국세라믹학회 1992 한국세라믹학회지 Vol.29 No.9

ZrO2/Al2O3-Mullite composites were prepared by infiltration of the silica sol to the porous ZrO2/Al2O3 bodies. The porous ZrO2/Al2O3 bodies for infiltration were fabricated using ZrO2 (20wt%)/Al2O3 composite powders synthesized by the emulsion-hot kerosene drying method. The preparation of silica sols was conducted by the hydrolysis-peptization of an alcoholic TEOS solution. When ZrO2/Al2O3-Mullite and ZrO2/Al2O3 composites were sintered at 1$650^{\circ}C$ for 4 hrs, both of them showed an excellent sinterability. As the amount of mullite added in the composites increased, the ratio of the tetragonal phase of zirconia to the monoclinic phase at the room temperature became higher. It was known that values of the fracture toughness of the ZrO2/Al2O3-Mullite composites were about 5.48 MPa.m1/2 much larger than that of the ZrO2/Al2O3 system.