• Journal of the Korean Applied Science and Technology
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• v.30 no.1
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• pp.9-15
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• 2013

A new process for the synthesis of polyphenylcarbosilane (PPCS) via thermal rearrangement of polymethylphenylsilane (PMPS) in supercritical cyclohexane was proposed and investigated at reaction temperatures of $380-420^{\circ}C$, reaction times of 1-2 h, and a pressure of 15 MPa. The structure, molecular weight, and molecular weight distribution of the product were characterized by FT-IR, Si-NMR, and GPC. The ceramic yield was also measured by TGA analysis. High-quality PPCS with high molecular weight and ceramic yield can be synthesized via a supercritical process. Furthermore, this process, when compared to the conventional method, tends to moderate the reaction conditions such as reaction temperature and time. It is concluded that thermal rearrangement in supercritical fluid is an efficient and viable process in terms of the resulting yield, efficiency, and reaction time compared with those of the conventional PCS production process.

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.11a
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• pp.34.2-34.2
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• 2009

The ceramic coatings on metallic materials have attracted by many researchers due to the chemical inertness of ceramic materials. In such aspect, SiOC is a promising material tobe used as protective coating layer on metallic materials due to its outstanding thermal stability and chemical inertness. In this research, SiOC coating was carried out onto SuS-316 substrate using Cl free preceramic polymers such aspolyphenylcarbosilane. 20% of polymethylphenylsilane in cyclohexane solution was coated onto metal surface by dip coating method. Thermal oxidation was carried out at $200^{\circ}C$ for crosslink of the preceramic polymer and the sample was pyrolysized at $800^{\circ}C$ under argon to convert the preceramic polymer to amorphous SiOCx state. The microstructure of the SiOCx film after pyrolysis was investigated using FE-SEM. Corrosion resistance of SiOC coated SuS-316 substrate has been investigated using 5% HCl solution at 25, 40, 60 and $80^{\circ}C$ for 7days. The data revealed that the corrosion resistance increased with SiOC coating on SuS-316 substrate.

• Applied Chemistry for Engineering
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• v.1 no.2
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• pp.161-167
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• 1990

Polymethylphenylsilane(PMPS) was synthesized with methylphenyldichlorosilane using metal sodium. Various sample coated on quartz plate were exposed and the yield of residual film was calculated. To obtain the fine image forming after developing and drying, optical transmittance characterization have to be considered. Exposure is described by three optical parameters X, Y, and Z. There parameters are normally determined from optical transmittance measurements of exposed PMPS films. Z parameter was determined from the initial slope of a transmittance according to exposure time. This set of function parameters provided a complete description of photoresist exposure and development and became the basis for the theoretical process models.

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.11a
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• pp.36.2-36.2
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• 2009

Low dielectric materials have been great attention in the semiconductor industry to develop high performance interlayer dielectrics with low k for Cu interconnect technology. In our study, the dielectric properties of SiOC /SiO2 thin film derived from polyphenylcarbosilane were investigated as a potential interlayer dielectrics for Cu interconnect technology. Polyphenylcarbosilane was synthesized from thermal rearrangement of polymethylphenylsilane around $350^{\circ}C{\sim}430^{\circ}C$. Characterization of synthesized polyphenylcarbosilane was performed with 29Si, 13C, 1H NMR, FT-IR, TG, XRD, GPC and GC analysis. From FT-IR data, the band at 1035 cm-1 is very strong and assigned to CH2 bending vibration in Si-CH2-Si group, indicating the formation of the polyphenylcarbosilane. Number average of molecular weight (Mn) of the polyphenylcarbosilane synthesized at $400^{\circ}C$ for 6hwas 2, 500 and is easily soluble in organic solvent. SiOC/SiO2 thin film was fabricated on ton-type silicon wafer by spin coating using 30wt % polyphenylcarbosilane incyclohexane. Curing of the film was performed in the air up to $400^{\circ}C$ for 2h. The thickness of the film is ranged from $1{\mu}m$ to $1.7{\mu}m$. The dielectric constant was determined from the capacitance data obtained from metal/polyphenylcarbosilane/conductive Si MIM capacitors and show a dielectric constant as low as 2.5 without added porosity. The SiOC /SiO2 thin film derived from polyphenylcarbosilane shows promising application as an interlayer dielectrics for Cu interconnect technology.

• Applied Chemistry for Engineering
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• v.7 no.5
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• pp.954-962
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• 1996

Four kind of polysilanes which had side chains of methyl, phenyl, and mixed structures, were synthesized and modified by doping with iodine. The structural, thermal, and electric characteristics of obtained polymers were systematically observed with iodine, The structural, thermal, and electric characteristics of obtained polymers were systematically observed with FT-IR, UV/VIS, TGA/DTG, DSC, and measurement of electric conductivity. From FT-IR spectra, it was confirmed that the synthesized polysilanes had side chains of methyl, phenyl, and mixed structures. The thermal stabilities of the polymers were found to increase with phenyl substituents. The polysilanes with phenyl side groups showed ${\sigma}-{\sigma}*$ transition absorption at wavelengths longer than 350 nm. The bathochromic shift of polysilanes with phenyl substituents relates probably to the narrowed band gap caused by delocalization of ${\pi}$-electron. The polymers doped with iodine showed multi-step pyrolysis behavior and higher residue compared with that of the undoped polymers. The electric conductivities of the undoped and doped polysilanes were $10^{-5}S/cm$ and $10^{-4}S/cm$, respectively.