• Korean Journal of Materials Research
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• v.18 no.12
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• pp.664-668
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• 2008

Vapor phase polymerization of a conductive polymer on a $SiO_2$ surface can offer an easy and convenient means to depositing pure and conductive polymer thin films. However, the vapor phase deposition is generally associated with very poor adhesion as well as difficulty when patterning the polymer thin film onto an oxide dielectric substrate. For a significant improvement of the patternability and adhesion of Poly(3-hexylthiophene) (P3HT) thin film to a $SiO_2$ surface, the substrate was pre-patterned with n-octadecyltrichlorosilane (OTS) molecules using a ${\mu}$-contact printing method. The negative patterns were then backfilled with each of three amino-functionalized silane self-assembled monolayers (SAMs) of (3-aminopropyl) trimethoxysilane (APS), N-(2-aminoethyl)-aminopropyltrimethoxysilane (EDA), and (3- trimethoxysilylpropyl)diethylenetriamine (DET). The quality and electrical properties of the patterned P3HT thin films were investigated with optical and atomic force microscopy and a four-point probe. The results exhibited excellent selective deposition and significantly improved adhesion of P3HT films to a $SiO_2$ surface. In addition, the conductivity of polymeric thin films was relatively high (${\sim}13.51\;S/cm$).

• Korean Journal of Materials Research
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• v.22 no.6
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• pp.275-279
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• 2012

(3-mercaptopropyl)trimethoxysilane (MPTMS) was used as a silylation agent, and modified silica nanoparticles were prepared by solution polymerization. 2.0 g of silica nanoparticles, 150 ml of toluene, and 20 ml of MPTMS were put into a 300 ml flask, and these mixtures were dispersed with ultrasonic vibration for 60 min. 0.2 g of hydroquinone as an inhibitor and 1 to 2 drops of 2,6-dimethylpyridine as a catalyst were added into the mixture. The mixture was then stirred with a magnetic stirrer for 8 hrs. at room temperature. After the reaction, the mixture was centrifuged for 1 hr. at 6000rpm. After precipitation, 150 ml of ethanol was added, and ultrasonic vibration was applied for 30 min. After the ultrasonic vibration, centrifugation was carried out again for 1 hr. at 6000rpm. Organo-modification of silica nanoparticles with a ${\gamma}$-methacryloxypropyl functional group was successfully achieved by solution polymerization in the ethanol solution. The characteristics of the ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) were examined using X-ray photoelectron spectroscopy (XPS, THERMO VG SCIENTIFIC, MultiLab 2000), a laser scattering system (LSS, TOPCON Co., GLS-1000), Fourier transform infrared spectroscopy (FTIR, JASCO INTERNATIONL CO., FT/IR-4200), scanning electron microscopy (SEM, HITACHI, S-2400), an elemental analysis (EA, Elementar, Vario macro/micro) and a thermogravimetric analysis (TGA, Perkin Elmer, TGA 7, Pyris 1). From the analysis results, the content of the methacryloxypropyl group was 0.98 mmol/g and the conversion rate of acrylamide monomer was 93%. SEM analysis results showed that the organo-modification of ultra-fine particles effectively prevented their agglomeration and improved their dispensability.

• Corrosion Science and Technology
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• v.12 no.1
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• pp.27-33
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• 2013

According to its merits about high curing speed and low emission of volatile organic compounds, UV curable inorganic-organic coating technology has been developed as an alternative for toxic and carcinogenic chromate-based treatments for years. It is consistently observed that ultra-thin films offer excellent corrosion protection as well as paint adhesion to metals. Based on the tetra-ethylorthosilicate(TEOS) and methacryloxypropyl trimethoxysilane(MPTMS), inorganic sol was synthesized and formed hybrid networks with UV curable acrylic monomer, 6-hexanediol diacrylate(HDDA), trimethylolpropane triacrylate(TMPTA), pentaerylthritol triacrylate(PETA). Several methods were used to test their properties such as salt spray test, potentiodynamic measurement, tape peel test, etc. It was shown that anti-corrosive property and stability of storage were affected by the molecular ratios of inorganic and organic compounds. It was not only the stability of storage, but had a excellent anti-corrosive, paint adhesive, and anti-solvent properties in a final molar ratios of 0.6/0.04/0.86/0.005 (TEOS/MPTMS/Acetone/HNO3) and 0.08/0.106/0.081/0.02 (TMPTA/HDDA/PETA/photo initiator).

• Korean Journal of Materials Research
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• v.20 no.11
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• pp.600-605
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• 2010

In order to meet the requirements of faster speed and higher packing density for devices in the field of semiconductor manufacturing, the development of Cu/Low k device material is explored for use in multi-layer interconnection. SiOC(-H) thin films containing alkylgroup are considered the most promising among all the other low k candidate materials for Cu interconnection, which materials are intended to replace conventional Al wiring. Their promising character is due to their thermal and mechanical properties, which are superior to those of organic materials such as porous $SiO_2$, SiOF, polyimides, and poly (arylene ether). SiOC(-H) thin films containing alkylgroup are generally prepared by PECVD method using trimethoxysilane as precursor. Nano voids in the film originating from the sterichindrance of alkylgroup lower the dielectric constant of the film. In this study, methyltriphenylsilane containing bulky substitute was prepared and characterized by using NMR, single-crystal X-ray, GC-MS, GPC, FT-IR and TGA analyses. Solid-state NMR is utilized to investigate the insoluble samples and the chemical shift of $^{29}Si$. X-ray single crystal results confirm that methyltriphenylsilane is composed of one Si molecule, three phenyl rings and one methyl molecule. When methyltriphenylsilane decomposes, it produces radicals such as phenyl, diphenyl, phenylsilane, diphenylsilane, triphenylsilane, etc. From the analytical data, methyltriphenylsilane was found to be very efficient as a CVD or PECVD precursor.

• Korean Chemical Engineering Research
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• v.47 no.4
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• pp.430-435
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• 2009

Spiropyran-doped organic-inorganic hybrid coatings were prepared starting from glycidoxypropyl triethoxysilane and vinyltriethoxysilane by a sol-gel method. They were applied as a thin layer to polycarbonate sheets and their photochromic properties were investigated. The effect of polarity of solvents dissolving the spiropyran was investigated on the photochromic properties. The decoloration rate of the spiropyran decreased with increasing the polarity of solvents dissolving the spiropyran because the open form of the spiropyran was easily stabilized in the polar gel matrix.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.6
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• pp.220-224
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• 2016

Anti-reflection (AR) thin films were fabricated on a glass substrate by using an ultrasonic spray. Glycidoxypropyl trimethoxysilane (GPTMS) and tetraethyl orthosilicate (TEOS) were used to synthesize a sol-gel hybrid coating solution. The moving speed of spray nozzle was changed from 15~25 mm/s to control the coating thickness of AR thin film. As the moving speed of spray nozzle increased, the thickness of AR thin film decreased from 138 nm to 86 nm. When the AR thin film was fabricated by nozzle moving speed of 20 mm/s, the refractive index and thickness of AR thin film was measured to be 1.31 and 104 nm, respectively. The average reflectance and transmittance of AR thin film coating glass was measured to be 0.75 % and 94 %, respectively into the visible light range of 380~780 nm.

• Korean Journal of Materials Research
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• v.22 no.8
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• pp.433-438
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• 2012

A chemical process involves polymerization within microspheres, whereas a physical process involves the dispersion of polymer in a nonsolvent. Nano-sized monodisperse microspheres are usually prepared by chemical processes such as water-based emulsions, seed suspension polymerization, nonaqueous dispersion polymerization, and precipitation polymerizations. Polymerization was performed in a four-necked, separate-type flask equipped with a stirrer, a condenser, a nitrogen inlet, and a rubber stopper for adding the initiator with a syringe. Nitrogen was bubbled through the mixture of reagents for 1 hr. before elevating the temperature. Functional silane (3-mercaptopropyl)trimethoxysilane (MPTMS) was used for the modification of silica nanoparticles and the self-assembled monolayers obtained were characterized by X-ray photoelectron spectroscopy (XPS), laser scattering system (LSS), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), elemental analysis (EA), and thermogravimetric analysis (TGA). In addition, polymer microspheres were polymerized by radical polymerization of ${\gamma}$-mercaptopropyl modified silica nanoparticles (MPSN) and acrylamide monomer via precipitation polymerization; then, their characteristics were investigated. From the elemental analysis results, it can be concluded that the conversion rate of acrylamide monomer was 93% and that polyacrylamide grafted to MPSN nanospheres via the radical precipitation polymerization with AAm in ethanol solvent. The microspheres were successfully polymerized by the 'graft from' method.

• Korean Chemical Engineering Research
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• v.54 no.5
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• pp.653-658
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• 2016

Poly(ether-block-amide)(PEBAX$_{(R)}$) resin is a thermoplastic elastomer combining linear chains of hard-rigid polyamide block interspaced soft-flexible polyether block. It was believed that the hard polyamide block provides the mechanical strength and permselectivity, whereas gas transport occurs primarily through the soft polyether block. The objective of this work was to investigate the gas permeation properties of carbon dioxide and methane for PEBAX$^{(R)}$-1657 membrane, and compare with those obtained for other grade of pure PEBAX$^{(R)}$, PEBAX$^{(R)}$-2533 and PEBAX$^{(R)}$ based hybrid membranes. The hybrid membranes based PEBAX$^{(R)}$ were obtained by a sol-gel process using GPTMS ((3-glycidoxypropyl) trimethoxysilane) as the only inorganic precursor. Molecular structure and morphology of membrane were analyzed by $^{29}Si$-NMR, DSC and SEM. PEBAX$_{(R)}$-2533 membrane exhibited higher gas permeability coefficients than PEBAX$^{(R)}$-1657 membrane. This was explained by the increase of chain mobility. In contrast, ideal separation factor of $CO_2/CH_4$ for PEBAX$^{(R)}$-1657 membrane was higher than PEBAX$^{(R)}$-2533 membrane. It was explained by the decrease of diffusion selectivity caused by increase of chain mobility. For PEBAX$^{(R)}$/GPTMS hybrid membrane, gas permeability coefficients were decreased with reaction time. Gas permeability coefficient of $CH_4$ was more significantly decreased than $CO_2$. It can be explained by the reduction of chain mobility caused by the sol-gel process, and strong affinity of PEO segment with $CO_2$. Comparing with pure PEBAX$^{(R)}$-1657 membrane, ideal separation factor of $CO_2/CH_4$ for PEBAX$^{(R)}$/GPTMS hybrid membrane has decreased to 4.5%, and gas permeability coefficient of $CO_2$ has increased 3.5 times.

• Polymer(Korea)
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• v.29 no.3
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• pp.242-247
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• 2005

Two kinds of colloidal silica(CS)/silane sol solutions were prepared in variation with synthesizing parameters such as kinds of CS, ratio of CS to silane and reaction time. Such sol solutions were obtained from 1034A Cs/methyl-trimethoxysilane(MTMS) and HSA CS/MTMS solutions. In the case of 1034A CS/MTMS CS/silane sol, coating film had high contact angle and more enhanced flat surface than those in the case of HSA CS/MTMS sol. In the case of thermal stability, thermal dissociation of 1034A CS/MTMS sol did not occur up to $550^{circ}$. The thickness of coating film obtained from 1034A CS/MTMS sol increased with increasing the amount of MTMS. The hardness of coating films obtained from 1034A CS/MTMS sol decreased with increasing the amount of MTMS. Surface free energy of CS/silane sol-gel coating film decreased with increasing amount of MTMS.

• Journal of Technologic Dentistry
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• v.29 no.1
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• pp.121-131
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• 2007

A preparation process's conditions of aqueous sol which contains anatase-type nano titania particles with photocatalyic properties was established by using Yoldas process, so called, DCS(Destabilization of Colloidal Solution) process in this study. And crystal size change and phase transformation of titania particles in aqueous titania sol depending on reaction conditions was investigated by a light scattering method and XRD analysis of frozen dried powders, respectively. This sol with photo catalytic nano titania particles was used to the following hydrophilic hybrid coating film's fabrication and its properties was evaluated. Subsequently, for coating film using the above mentioned aqueous titania sol, non-aqueous titania sol was prepared without any chemical additives and its time stability according to aging time was investigate. By using the above mentioned aqueous titania sol and non-aqueous sol, a complex oxide coating sol for metal and ceramic substrate and a organic-inorganic hybrid coating sol for polymer substrate was prepared and it's hydrophilicity depending on UV irradiation conditions was evaluated. As a conclusions, the following results were obtained. (1)Aqueous titania sol The average particle size of titania in formed aqueous titania sol was distributed between 20$\sim$90nm range depending on reaction conditions. And the crystal phase of titania powders obtained by frozen drying method was changed from amorphous state to anatase and subsequently transformed to rutile crystal phase and it is attributed to concentration gradient in aqueous sol. (2)Non-aqueous titania sol Non-aqueous titania sol was prepared using methanol as a solvent and a little distilled water for hydrolysis and nitric acid as a catalyst were used. The obtained non-aqueous titania sol was stable at room temperature for 20 days. Additionally, non-aqueous titania sol with addition of chealating reagent such as acethylaceton and ethylene glycol prolonged the stability of sol by six months. (3)Complex sol and hybrid sol with super hydrophilicity The above mentioned aqueous titania sol as a main photocataylic component and non-aqueous titania sol as a binder for coating process was used to prepare a complex sol used for metal, ceramic and wood material substrate and also to prepare the organic-inorganic hybrid sol for polymer substrate such as polycarbonate and polyethylene, in which process APMS(3-Aminopropyltrimethoxysilane), GPTS(3-Glycidoxypropyl-trimethoxysilane) as a hydrophilic silane compound and HEMA(2-Hydroxyethyl methacrylate) as a forming network in hybrid coating film were used. The hybrid coating film such as prepared through this process showed a superhydrophilicity below 1$10^{\circ}$ depending on processing conditions and a pencil's hardness over 6 H.