Browsing by Author "Kim, You Na"
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Item Enhancement of electroconductivity of polyaniline/graphene oxide nanocomposites through in situ emulsion polymerization(Journal of Material Science, 2013-10-23) Imran, S.M; Shao, Godlisten N.; Kim, You Na; Hussain, Manwar; Choa, Yong-Ho; Kim, HTThe present study introduces a systematic approach to disperse graphene oxide (GO) during emulsion polymerization (EP) of Polyaniline (PANI) to form nanocomposites with improved electrical conductivities. PANI/ GO samples were fabricated by loading different weight percents (wt%) of GO through modified in situ EP of the aniline monomer. The polymerization process was carried out in the presence of a functionalized protonic acid such as dodecyl benzene sulfonic acid, which acts both as an emulsifier and protonating agent. The microstructure of the PANI/GO nanocomposites was studied by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, UV–Vis spectrometry, Fourier transform infrared, differential thermal, and thermogravimetric analyses. The formed nanocomposites exhibited superior morphology and thermal stability. Meanwhile, the electrical conductivities of the nanocomposite pellets pressed at different applied pressures were determined using the fourprobe analyzer. It was observed that the addition of GO was an essential component to improving the thermal stability and electrical conductivities of the PANI/GO nanocomposites. The electrical conductivities of the nanocomposites were considerably enhanced as compared to those of the individual PANI samples pressed at the same pressures. An enhanced conductivity of 474 S/m was observed at 5 wt% GO loading and an applied pressure of 6 t. Therefore, PANI/GO composites with desirable properties for various semiconductor applications can be obtained by in situ addition of GO during the polymerization process.Item Enhancement of porosity of sodium silicate and titanium oxychloride based TiO2–SiO2 systems synthesized by sol–gel process and their photocatalytic activity(Microporous and Mesoporous Materials, 2012-11-09) Shao, Godlisten N.; Kim, You Na; Imran, S.M; Jeon, Sunjeong; Sarawade, Pradip B.; Hilonga, Askwar; Kim, Jong-gil; Kim, Hee TaikThe textural properties of TiO2–SiO2 composites (TSCs) were successively enhanced using three approaches; (1) washing the hydrogels with different solvents, (2) using surfactant and (3) forming the TiO2 sol in ethanol medium. The sol–gel process was exquisitely used to form the composites using cost effective precursors. Initially, the precipitated hydrogels were washed with water or alcohol to evaluate the influence of washing on the dried hydrogels. Consequently, two composites were formed differently in the presence of stearic acid (SA) as a surfactant and the other by forming TiO2 sol in ethanol medium prior to reaction with silica source. The TSC powders were examined by XRD, N2 physisorption studies, FTIR, TGA, SEM, XRF and HRTEM. The BET surface area of the sample obtained after washing the hydrogels with ethanol (TSCE) was the largest (594 m2/g) while porosities of the composites obtained using stearic acid as a surfactant (TSCSA, 0.96 cm3/g) and ethanol as a medium to form the TiO2 sol (TSCES, 1.85 cm3/g) were relatively superior to those obtained under influence of changing washing solvent. Photocatalytic decolorization of methylene blue by the composites calcined at 800 C revealed that the TSCES-800 possessed the highest activity of all the composites due to its superior properties.Item A Gentle Method to Graft Thiol-Functional Groups onto Silica Gel for Adsorption of Silver Ions and Immobilization of Silver Nanoparticles(2012-10-22) Quang, Dang Viet; Lee, Jae Eun; Kim, Jong-gil; Kim, You Na; Shao, Godlisten N.; Kim, Hee TaikThiol-functionalized silica that has been used to remove heavymetal from an aqueous solution and supportmetallic nanoparticles is usually synthesized by reflux in an organic solvent containing 3-mercaptopropyltrimethoxysilane (MPTMS). In this paper, we report a gentle method for grafting thiol-functional groups onto silica gel by an aging process that does not require mixing and refluxing in an organic solvent. Silica gel was synthesized by a sol–gel method from H2SO4 (40%) and sodium silicate, which was crushed into beads with sizes ranging from 180 to 450 μm. Silica beads (50 g) were mixed with 75 mL of a functionalization solution consisting of MPTMS, H2O, and C2H5OH and aged at 50 °C for 36 h in a box dryer. The success of the functionalization process was confirmed by FT-IR, BET, SEM and elemental analyses. The functionalization solution was percolated into pores and thiolfunctional groups were grafted onto the surface and pore walls of the silica beads. The ability of these functionalized silica beads to adsorb silver ionswas determined by the Langmuir isotherm equationwith amaximumadsorption of 75.8 mg/g. Silver nanoparticles with sizes ranging from 2 to 6 nmformed by chemical reductionwere located inside the pores and on the surfaces.Item Peptization technique in the synthesis of titania–silica composites and their photocatalytic properties(Chemical Engineering Journal, 2012-05-18) Shao, Godlisten N.; Hilonga, Askwar; Kim, You Na; Kim, Jong-gil; Elineema, Gideon; Quang, Dang Viet; Jeon, Sunjeong; Kim, Hee TaikA comparative study of titania–silica composite (TSC) synthesized via peptization sol–gel method was conducted. Typically, titanium hydroxide gel (Ti(OH)4) was formed by condensation of titanium oxychloride solution using adequate amount of ammonium hydroxide solution. The preformed gel was peptized either in silicic acid (SA) or nitric acid (NA) to form a sol. The composite was characterized by XRD, FTIR, SEM, TEM, TGA, and N2 physisorption studies. The XRD patterns and the TEM micrographs confirmed that thermal-derived samples of the composite, formed using silicic acid as a silica source and peptizing agent (TSC–SA), yielded TiO2ASiO2 composite with a single-phase (anatase phase); while a mixture of both anatase and rutile phases were observed in the composite (TSC–NA), where nitric acid was used as a peptizing agent. FTIR analysis showed the vibration band assignable to the TiAOASi bond at 945 cm 1, suggesting that titania was incorporated into silica to form a composite. Furthermore, a simple experiment of photodegradation of methyl orange in the presence of sunlight was performed to demonstrate the practical efficacy of the composites synthesized via this method. The results indicated that the calcined samples of TSC–NA-800 had the highest activity due to its superior properties.Item Quantitative Recovery of High Purity Nanoporous Silica from Wste Products of the Phosphate Fertilizer Industry(2012-06-12) Elineema, Gideon; Kim, Jong-gil; Hilonga, Askwar; Shao, Godlisten N.; Kim, You Na; Quang, Dang Viet; Sarawade, PB; Kim, Hee TaikThis study reports on the quantitative recovery of high purity nanoporous silica from wastes material (H2SiF6) of the phosphate fertilizer industry and Na2O SiO2. The silica recovered from the wastes was compared with silica from the reaction of H2SO4 and Na2O SiO2 because H2SO4 is commonly used. The product recovered from the wastes material and H2SO4 were 99.3% and 99.1% pure, respectively. The quantity recovered were 22.30 g and 20.11 g, respectively. The product had superior properties suitable for applications such as chromatography, reinforcing material for rubber and plastics. The process may significantly reduce the release of SiF4 gas into the environment.Item Sol–gel synthesis of sodium silicate and titanium oxychloride based TiO2–SiO2 aerogels and their photocatalytic property under UV irradiation(Chemical Engineering Journal, 2013-07-26) Kim, You Na; Shao, Godlisten N.; Jeon, Sunjeong; Imran, S.M; Sarawade, PB; Kim, HTBinary titania–silica metal oxides (TiO2–SiO2) have preferentially been used as photocatalysts for the degradation of organic contaminants under UV irradiation. Herein we synthesized TiO2–SiO2 aerogel powders with different Si-to-Ti ratios suitable for decolorization of organic pollutants using less expensive silica source (sodium silicate) and titanium oxychloride as a titania precursor. Consequently, the surfaces of the alcogels were hydrophobized using trimethylchlorosilane (TMCS) as a silylating agent to yield hydrophobic aerogel powders at ambient pressure drying. The as-prepared samples were calcined at different temperatures ranging from 200 to 1000 C to evaluate the effect of the heat treatment in the microstructure of the aerogels. The physico-chemical properties of the aerogels were examined by XRD, FTIR, XRF, TEM, SEM, N2 gas physisorption studies, TGA/DTA and diffusive reflectance spectrometry analyses. It was found that calcination temperature is an important factor in improving the porosity and crystallinity of the aerogels however; it has a detrimental effect on the hydrophobicity and photochemical performance of the aerogels. The as-synthesized aerogels were hydrophobic and exhibited the highest activity toward decolorization of methylene blue. The hydrophilic aerogels were obtained after calcination at temperature P500 C however; the formed samples possessed lower activities. Hydroxyl radicals ( OH) detection experiment performed in the presence of the photocatalysts indicated that the generation of radicals during irradiation increases with increasing illumination time.Item Sol–gel synthesis of sodium silicate and titanium oxychloride based TiO2–SiO2 aerogels and their photocatalytic property under UV irradiation(Elsevier, 2013-07-26) Kim, You Na; Shao, Godlisten N.; Jeon, Sunjeong; Imran, S.M; Sarawade, PB; Kim, HTBinary titania–silica metal oxides (TiO2–SiO2) have preferentially been used as photocatalysts for the degradation of organic contaminants under UV irradiation. Herein we synthesized TiO2–SiO2 aerogel powders with different Si-to-Ti ratios suitable for decolorization of organic pollutants using less expensive silica source (sodium silicate) and titanium oxychloride as a titania precursor. Consequently, the surfaces of the alcogels were hydrophobized using trimethylchlorosilane (TMCS) as a silylating agent to yield hydrophobic aerogel powders at ambient pressure drying. The as-prepared samples were calcined at different temperatures ranging from 200 to 1000 C to evaluate the effect of the heat treatment in the microstructure of the aerogels. The physico-chemical properties of the aerogels were examined by XRD, FTIR, XRF, TEM, SEM, N2 gas physisorption studies, TGA/DTA and diffusive reflectance spectrometry analyses. It was found that calcination temperature is an important factor in improving the porosity and crystallinity of the aerogels however; it has a detrimental effect on the hydrophobicity and photochemical performance of the aerogels. The as-synthesized aerogels were hydrophobic and exhibited the highest activity toward decolorization of methylene blue. The hydrophilic aerogels were obtained after calcination at temperature P500 C however; the formed samples possessed lower activities. Hydroxyl radicals ( OH) detection experiment performed in the presence of the photocatalysts indicated that the generation of radicals during irradiation increases with increasing illumination timeItem Two step synthesis of a mesoporous titania–silica composite from titanium oxychloride and sodium silicate(Powder Technology, 2011-11-15) Shao, Godlisten N.; Elineema, Gideon; Quang, Dang Viet; Kim, You Na; Shim, YoungHo; Hilonga, Askwar; Kim, Jong-gil; Kim, Hee TaikMesoporous titania–silica composite (MTSC) with a large surface area (387 m2/g) and large pore volume was synthesized by a two step condensation sol–gel method. Transparent TiO2 sol was formed at room temperature through condensation and peptization of titanium oxychloride solution using ammonium hydroxide and aqueous nitric acid respectively. Sodium silicate was used as a silica source to form a composite with the preformed TiO2 sol. The physical properties of the composite were examined by Fourier Transform infrared (FTIR), BET surface area, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The nitrogen physisorption behavior of the synthesized composite was compared to that obtained from grafting and one-pot co-condensation methods using the same precursors in the presence of cetyltrimethylammonium bromide (CTAB). It was found that MTSC synthesized under this method possessed large pore sizes and pore volume but its thermal stability was comparatively low. FTIR spectra showed the formation of a Ti\O\Si bond at 940 cm−1 suggesting that titania was incorporated in silica to form a composite. The XRD patterns showed that the major phase of the titania had an anatase phase up to 900 °C but it transforms into rutile when calcined at 1000 °C. Furthermore the EDS studies of the as-synthesized and calcined samples substantiated the formation of titania–silica composites.