• Composites Research
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• v.35 no.1
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• pp.23-30
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• 2022

Polycarbosilane(PCS) is an important precursor for melt-spinning the silicon carbide(SiC) fibers and manufacturing ceramics. The PCS is a metal-organic polymer precursor capable of producing continuous SiC fibers having excellent performance such as high-temperature resistance and oxidation resistance. The SiC fibers are manufactured through melt-spinning, stabilization, and heat treatment processes using the PCS manufactured by synthesis, purification, and control of the molecular structure. In this paper, we analyzed the effect of purification of unreacted substances and low molecular weight through solvent treatment of PCS and the effect of heat treatment at various temperatures change the polymerization and network rearrangement of PCS. Especially, we investigated the complex viscosity and structural arrangement of PCS precursors according to solvent treatment and heat treatment through the rheological properties.

• Proceedings of the Korean Ceranic Society Conference
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• 2003.10a
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• pp.151.2-151
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• 2003

• Proceedings of the Korean Nuclear Society Conference
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• 2005.10a
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• pp.386-387
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• 2005

• Journal of Radiation Industry
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• v.4 no.3
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• pp.265-269
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• 2010

Silicon-based non-oxide ceramic carbide fiber is one of the leading candidate ceramic materials for engineering applications because of its excellent mechanical properties at high temperature and good chemical resistance. In this study, polycarbosilane(PCS) and zirconium butoxide were used as a precursor to prepare polyzirconocarbosilane (PZC) fibers. A polymer solution was prepared by dissolving PCS in zirconium butoxide (50/50 wt%). This solution was heated at $250^{\circ}C$ in a nitrogen atmosphere for 2 hour with stirring, and then dried in a vacuum oven for 48 hour. PZC fibers were fabricated using an electrospinning technique. The fibers were irradiated with an electron beam to induce structural crosslinking. Crosslinked PZC fibers were heat treated at $1,300^{\circ}C$ in a nitrogen atmosphere. The microstructures of PZC fibers were examined by SEM. Chemical structures of PZC fibers were examined by FT-IR and XRD. Thermal stability of PZC fibers was investigated by TGA.

• Composites Research
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• v.30 no.2
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• pp.102-107
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• 2017

The preceramic polymer can realize a variety of complex ceramic structures that can not be obtained by conventional ceramic processes. Polycarbosilane, which is a typical preceramic polymer, can control the molecular structure, molecular weight and molecular weight distribution for preparing complex morphology and microstructure of SiC ceramics, including SiC fiber. In this paper, synthesis and molecular structure control technique of polycarbosilane is explained. The silicon carbide fiber prepared by melt spinning, stabilization and heat treatment, and ceramic fiber composites technology made by PIP process are also discussed. In addition, we introduce an example of the development of a complex silicon carbide material such as a silicon carbide hollow fiber having a nanoporous structure.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.20 no.3
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• pp.29-34
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• 2019

Silicon carbide is considered to be a potentially useful material for high-temperature electronic devices, as its large energy band gap and the p-type and/or n-type conduction can be controlled by impurity doping. Particularly, electric conductivity of porous n-type SiC semiconductors fabricated from ${\beta}-SiC$ powder at $2000^{\circ}C$ in $N_2$ atmosphere was comparable to or even larger than the reported values of SiC single crystals in the temperature region of $800^{\circ}C$ to $1000^{\circ}C$, while thermal conductivity was kept as low as 1/10 to 1/30 of that for a dense SiC ceramics. In this work, for the purpose of decreasing sintering temperature, it was attempted to fabricate porous reaction-sintered bodies at low temperatures ($1400-1600^{\circ}C$) by thermal decomposition of polycarbosilane (PCS) impregnated in n-type ${\beta}-SiC$ powder. The repetition of the impregnation and sintering process ($N_2$ atmosphere, $1600^{\circ}C$, 3h) resulted in only a slight increase in the relative density but in a great improvement in the Seebeck coefficient and electrical conductivity. However the power factor which reflects the thermoelectric conversion efficiency of the present work is 1 to 2 orders of magnitude lower than that of the porous SiC semiconductors fabricated by conventional sintering at high temperature, it can be stated that thermoelectric properties of SiC semiconductors fabricated by the present reaction-sintering process could be further improved by precise control of microstructure and carrier density.

• Korean Journal of Materials Research
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• v.24 no.9
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• pp.474-480
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• 2014

Process conditions for the impregnation of polycarbosilane preceramic polymer into SiC-based composites were investigated. Two kinds of preceramic polymer (PCP) was impregnated into SiC-fiber fabrics with different solvents of n-hexane and divinylbenzene (DVB). Both microstructural observations and mechanical tests were conducted to evaluate the impregnation. The matrix phases were particulated in the case of hexane solvents. Apparent relative density of the matrix was about 78.8%. The density of matrix was increased to about 96.1-98.8% when the DVB was used; however, brittle fracture was observed during a bending test. The modulus of toughness was less than $0.74J/m^3$. The fabric impregnated with a mixed PCP-dissolved solution showed intermediate characteristics with relative high density of filling (apparent density of ~96.1%) as well as proper bending behavior. The modulus of toughness was increased to about $5.31J/m^3$. The composites developed by changing the precursor and solvent suggested the possibility of fabricating SiCf/SiC composites without a fiber to matrix interphase coating.

• Korean Journal of Materials Research
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• v.20 no.9
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• pp.451-456
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• 2010

A promising candidate material for a $H_2$ permeable membrane is SiC due to its many unique properties. A hydrogen-selective SiC membrane was successfully fabricated on the outer surface of an intermediate multilayer $\gamma-Al_2O_3$ with a graded structure. The $\gamma-Al_2O_3$ multilayer was formed on top of a macroporous $\alpha-Al_2O_3$ support by consecutively dipping into a set of successive solutions containing boehmite sols of different particle sizes and then calcining. The boehmite sols were prepared from an aluminum isopropoxide precursor and heated to $80^{\circ}C$ with high speed stirring for 24 hrs to hydrolyze the precursor. Then the solutions were refluxed at $92^{\circ}C$ for 20 hrs to form a boehmite precipitate. The particle size of the boehmite sols was controlled according to various experimental parameters, such as acid types and acid concentrations. The topmost SiC layer was formed on top of the intermediate $\gamma-Al_2O_3$ by pyrolysis of a SiC precursor, polycarbosilane, in an Ar atmosphere. The resulting amorphous SiC-on-$Al_2O_3$ composite membrane pyrolyzed at $900^{\circ}C$ possessed a high $H_2$ permeability of $3.61\times10^{-7}$ $mol{\cdot}m^{-2}{\cdot}s^{-1}{\cdot}Pa^{-1}$ and the $H_2/CO_2$ selectivity was much higher than the theoretical value of 4.69 in all permeation temperature ranges. Gas permeabilities through a SiC membrane are affected by Knudsen diffusion and a surface diffusion mechanism, which are based on the molecular weight of gas species and movement of adsorbed gas molecules on the surface of the pores.

• Journal of the Korean Ceramic Society
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• v.48 no.6
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• pp.499-503
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• 2011

Recently, variety of organic and inorganic hybrid materials have recently investigated as alternative routes to SiOC, $SiO_2$ thin film formation at low temperatures for applications in electronic ceramics. Specially, silicon based polymers, such as polycarbosilane, polysilane and polysilazane derivatives have been studied for use in electronic ceramics and have been applied as dielectric or insulating materials. In this study, Polycarbosilane(PCS), which Si-$CH_2$-Si bonds build up the backbone of the polymer, has been investigated as low-k materials using a solution process. After heat treatment at 350$^{\circ}C$ under $N_2$ atmosphere, chemical composition and dielectric constant of the thin film were $SiO_{0.27}C_{1.94}$ and 1.2, respectively. Mechanical property measured using nanoindentor shows 1.37 GPa.

• Journal of the Korean Ceramic Society
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• v.41 no.7
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• pp.528-533
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• 2004

Macroporous SiC with pore size 84∼658 nm and mesoporous SiC with pore size 15∼65 nm were respectively prepared by infiltrating low viscosity preceramic polymer solutions into the various sacrificial templates obtained by natural sedimentation or centrifuge of 20∼700 nm silica sol, which were subsequently etched off with HF after pyrolysis at 1000∼140$0^{\circ}C$ in an argon atmosphere. Three-dimensionally long range ordered macroporous SiC ceramics derived from polymethylsilane (PMS) showed surface area 584.64$m^2$g$^{-1}$ when prepared with 112nm silica sol and at 140$0^{\circ}C$, whereas mesoporous SiC from polycarbosilane (PCS) exhibited the highest surface area 619.4 $m^2$g$^{-1}$ with random pore array when prepared with 20-30 nm silica sol and at 100$0^{\circ}C$. Finally, tile pore characteristics of porous SiC on the types of silica sol, polymers and pyrolytic conditions were interpreted with the analytical results of SEM, TEM, and BET instruments.