• Title/Summary/Keyword: Sol-Gel reaction

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Synthesis and Characterization of Fe Doped TiO2 Nanoparticles by a Sol-Gel and Hydrothermal Process

  • Kim, Hyun-Ju;Jeong, Kwang-Jin;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.22 no.5
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    • pp.249-252
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    • 2012
  • Fe doped $TiO_2$ nanoparticles were prepared under high temperature and pressure conditions by mixture of metal nitrate solution and $TiO_2$ sol. Fe doped $TiO_2$ particles were reacted in the temperature range of 170 to $200^{\circ}C$ for 6 h. The microstructure and phase of the synthesized Fe doped $TiO_2$ nanoparticles were studied by SEM (FE-SEM), TEM, and XRD. Thermal properties of the synthesized Fe doped $TiO_2$ nanoparticles were studied by TG-DTA analysis. TEM and X-ray diffraction pattern shows that the synthesized Fe doped $TiO_2$ nanoparticles were crystalline. The average size and distribution of the synthesized Fe doped $TiO_2$ nanoparticles were about 10 nm and narrow, respectively. The average size of the synthesized Fe doped $TiO_2$ nanoparticles increased as the reaction temperature increased. The overall reduction in weight of Fe doped $TiO_2$ nanoparticles was about 16% up to ${\sim}700^{\circ}C$; water of crystallization was dehydrated at $271^{\circ}C$. The transition of Fe doped $TiO_2$ nanoparticle phase from anatase to rutile occurred at almost $561^{\circ}C$. The amount of rutile phase of the synthesized Fe doped $TiO_2$ nanoparticles increased with decreasing Fe concentration. The effects of synthesis parameters, such as the concentration of the starting solution and the reaction temperature, are discussed.

Properties of Sol-Gel Materials Synthesized from Colloidal Silica and Alkoxysilane Containing Epoxysilane (에폭시 실란을 함유한 콜로이드 실리카와 알콕시 실란간의 졸겔코팅제 합성과 특성)

  • Kang, Dong-Pil;Park, Hoy-Yul;Ahn, Myeong-Sang;Myung, In-Hye;Choi, Jae-Hoon;Kim, Hyun-Joong
    • Applied Chemistry for Engineering
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    • v.16 no.6
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    • pp.822-826
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    • 2005
  • Colloidal Silica (CS)/methyltrimethoxysilane (MTMS) and CS/MTMS/epoxysilane (ES) sol solutions were prepared using various synthesizing parameters such as reaction time and types of CS and silane. In order to understand their physical and chemical properties, sol-gel coating films on glass were fabricated. In the case of the CS/MTMS sol, the coating films had high contact angle and more enhanced flat surface than the CS/MTMS/ES sol. In the case of thermal stability, thermal degradation of the CS/MTMS and CS/MTMS/ES coating films did not occur up to $550^{\circ}C$ and $440^{\circ}C$, respectively. The coating films prepared from the CS/MTMS sol were thicker than those of the CS/MTMS/ES sol. In addition, the coating films prepared from single CS were thicker than those of mixed CS. Hardness of the coating films prepared from CS/MTMS increased by adding ES. In case of the mixed CS, the hardness decreased by adding ES.

A Study on the Sol-Gel Reaction Kinetics of Sodium Silicate Solution (규산(硅酸)나트륨 수용액(水溶液)의 솔-젤 반응속도론적(反應速度論的) 고찰(考察))

  • Kim, Chul-Joo;Yoon, Ho-Sung;Jang, Hee-Dong
    • Resources Recycling
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    • v.17 no.6
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    • pp.34-42
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    • 2008
  • The properties of sodium silicate solution were surveyed by using the yellow silicomolybdic method, and the formation of silica sol from sodium silicate solution and the growth of silica sol were investigated in this study. The $SiO_2$ content of 2 wt% in sodium silicate solution was proper to oxidize sodium silicate with sulfuric acid. After the removal of sodium ions in sodium silicate solution, the pH of silicate solution had to be controlled above 9 for the stabilization of silicate solution. The condensation between silicic acid species and silica nuclei surfaces has been studied at $20{\sim}80^{\circ}C$ and pH 10 in silicate solutions with silica nuclei. The reaction falls into two kinetics regimes, limited at high silicic acid species concentration by polymerization, but at lower concentration by a process whereby deposited silicic acid species condenses further to silica. The overall condensation is first-order in silicic acid species concentration, proceeded toward to pseudo equilibrium concentration, $C_x$, rather than the solubility of amorphous silica. The heat of solution of amorphous silica was 3.34 kcal/mol and exhibits an Arrhenius temperature dependence with an apparent activation energy of 3.16 kcal/mol in the range of $20{\sim}80^{\circ}C$.

Easy and Simple Synthesis of CdSe Nanocrystals: The Effect of Reaction Temperature for The Determination of Nanoparticle Size (간편한 CdSe 나노 입자의 합성: 입자크기를 결정하는 반응온도의 효과)

  • Kim, Sungjin
    • Journal of Integrative Natural Science
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    • v.2 no.3
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    • pp.219-223
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    • 2009
  • Easy and simple synthesis of CdSe nanocrystals was achieved through sol-gel process. CdSe nanocrystals were synthesized from the reaction of cadmium oxide and selenium in the prescence of trioctylphosphine oxide, tributylphosphine, octadecene, octadecylamine, and stearic acid. The effect of reaction temperature for the determination of size of CdSe nanocrystals was investigated after the addition of selenium. The reaction temperature for the growth of CdSe nanocrystals was increased by every $20^{\circ}C$ from 170 to 190, 210, 230, 250, 270, and $290^{\circ}C$. When the reaction temperature was higher, the absorption wavelength in the absorption spectrum was increased which indicated that the size of CdSe nanocrystals was increased. The emission wavelength in the photoluminescence spectrum was increased from 438 to 489, 542, 591, 643, 692, and 745 nm, as the size of CdSe nanocrystals was increased. The control of the reaction temperature illustrated that the color tuning of emission wavelength were successfully obtained.

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Hard Coatings on Polycarbonate Plate by Sol-Gel Reaction of (3-glycidoxypropyl)trimethoxysilane (폴리카보네이트 판 위에 (3-glycidoxypropyl)trimethoxysilane의 졸-겔 반응을 이용한 하드 코팅)

  • Kim, Ju Youn;Shin, Young Jae;Shin, Youn Rok;Ji, Young Jon;Yoon, Yeo Seong;Shin, Jae Sup
    • Applied Chemistry for Engineering
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    • v.17 no.2
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    • pp.170-176
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    • 2006
  • The hard coatings on the polycarbonate plate were performed with the object of substitution the glass in the car to the polycarbonate plate. In this research, (3-glycidoxypropyl)trimethoxysilane (GPTMS), (3-aminopropyl)triethoxysilane (APS), and diethylenetriamine (DETA) were used to prepare the coatings by a sol-gel process. The optimum conditions and formulation to achiere the excellent physical properties of the coating were determined. In the case of using GPTMS and DETA, the smooth coating which had the 2 H class in pencil hardness was formed. In the case of using GPTMS and APS, the coating which had the 2 H class in pencil hardness was also formed. And the coatings with GPTMS and DETA showed an excellent abrasion resistant.

Influence of PVP on the Thickness of Ferroelectric (Na,K)NbO3 Film by Sol-Gel (솔-젤 법을 통해 제조된 강유전체 (Na,K)NbO3 막의 두께에 미치는 PVP의 영향)

  • Kim, Dae-Gun;Yoo, In-Sang;Kim, Sae-Hoon;Kim, Jin-Ho
    • Korean Journal of Materials Research
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    • v.22 no.12
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    • pp.696-700
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    • 2012
  • (Na, K) $NbO_3$ thick film was successfully achieved using a sol-gel coating process with the addition of polyvinylpyrrolidone (PVP) to a metal alkoxide solution. The transparent coating solution, mixed with Nb:PVP = 1:1 in a molar ration, was synthesized by evaporating the solvent to over 62.5 wt%. Additive PVP increased the viscosity of the solution so that the coating thickness could be enhanced. The thickness of the (Na, K) $NbO_3$ film assisted by PVP was ca. 320 nm at the time of deposition; this value is four times thicker than that of the sample fabricated without PVP. Also, due to PVP binding with the OH groups of the metal alkoxide, the condensation reaction in the film was suppressed. The crystalline size of the (Na, K) $NbO_3$ films assisted by PVP was ca. 15 nm smaller than that of the film fabricated without PVP. After the sintering process at $700^{\circ}C$, the (Na, K) $NbO_3$ films were mainly composed of randomly oriented (Na, K) $NbO_3$ phase of perovskite crystal structure, including a somewhat secondary phase of $K_2Nb_4O_{11}$. However, by adding PVP, the content of the secondary phase became quite smaller than that of the sample without PVP. It was thought that the addition of PVP might have the effect of restraining the loss of potassium and that PVP could hold metalloxane by strong hydrogen bonding before complete decomposition. Therefore, the film thickness of the (Na, K) $NbO_3$ films could be considerably advanced and made more crack-free by the addition of PVP.

Characteristics of Polyimide-silica Hybrid Materials Prepared from Alkoxide Precursor Using Sol-gel Process (졸-겔법을 이용하여 알콕사이드 전구체로부터 합성된 Polyimide-silica 혼성체의 특성)

  • Kim, Byoung-Woo;Lee, Sung-Hwan;Kim, Sung-Wan;Park, Jae-Hyun;Kim, Jun-Ho;Park, Seong-Soo;Park, Hee-Chan
    • Journal of the Korean Ceramic Society
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    • v.39 no.11
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    • pp.1063-1068
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    • 2002
  • Polyimide/silica(PI/silica) hybrid materials having physical or chemical bonds between the PI and silica network were prepared using sol-gel process through hydrolysis and polycondensation of tetraethoxysilane with the polyamic Acid(PAA) or end-capped PAA solution. PAA solution was synthesized by ring opening reaction of pyromellitic dianhydride and oxydianiline monomers in dimethyl acetamide solution. End-capped PAA solution was synthesized by the addition of 3-aminopropyltriethoxysilane in PAA solution. PI/silica hybrid samples were characterized by infrared spectroscopy, differential thermogravimetry, X-ray diffractometry, scanning electron microscopy, and tensile tester. It has been demonstrated that the properties of hybrid samples were affected by the silica content and the bond type between PI and silica.

Synthesis of Li4/3Mn5/3O4 by Sol-Gel Process and its Electrochemical Properties (졸-겔법에 의한 Li4/3Mn5/3O4의 합성 및 전기화학적 특성)

  • Lee, Jin-Sik;Lee, Chul-Tae
    • Applied Chemistry for Engineering
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    • v.10 no.1
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    • pp.80-84
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    • 1999
  • $Li_{4/3}Mn_{5/3}O_4$ having a defect structure was prepared by sol-gel process using lithium acetate and manganese acetate as starting materials, and their electrode characteristics in the lithium secondary battery was investigated. The reaction mole ratio was determined as $AA/Mn(OAc)_2$ of 0.2 and $NH_4OH/Mn(OAc)_2$ to $H_2O/Mn(OAc)_2$ of 0.4. The product was obtained through heat treatment at $350^{\circ}C$ for 12hrs after 1'st heat treatment at $150^{\circ}C$ of xerogel under oxygen atmosphere. When the charge and discharge cycles were performed between 2.0 V and 3.2 V, $Li/Li_{4/3}Mn_{5/3}O_4$ cell showed the dicharge capacity of 84.23 mAh/g and the good cycleability was obtained in the plateau region.

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A Study on the Photocatalytic Degradation of VOC over TiO2 Coated on Glass Bead (산화티탄 광촉매를 이용한 VOC 가스 처리효과에 관한 연구)

  • Yun, Seok-Yeong;No, Jun-Hyeong;Park, Sun-Je;Lee, Seung-Ho
    • Korean Journal of Materials Research
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    • v.10 no.5
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    • pp.328-334
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    • 2000
  • The photocatalyst of $TiO_2$coated on glass bead was prepared from sol-gel method to remove the VOC (vola-tile organic compounds) by the photocatalytic reaction. The coated films were characterized by X-ray diffraction(XRD), specific surface area(BET), and scanning electron microscopy observation (SEM), The gas-phase photocatalytic degradation of trichloroethylene(TCE) and benzene with coated titanium dioxide on glass beads was in-vestigated using a fixed bed reactor. The degradation was calculated by the concentration difference with the retained on the reactor with aid of gas chromatography. At steady state, conversion yields were obtained for 80% of trichloroeth-vlene in 400 ppmv concentration and 65% on benzene in the range of concentration from 50 to 300 ppmv, respectively.

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Catalytic Effects and Characteristics of Ni-based Catalysts Supported on TiO2-SiO2 Xerogel

  • Jeong, Jong-Woo;Park, Jong-Hui;Choi, Sung-Woo;Lee, Kyung-Hee;Lee, Chang-Seop
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2288-2292
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    • 2007
  • The catalytic activities of nickel-based catalysts were estimated for oxidizing acetaldehyde of VOCs exhausted from industrial facilities. The catalysts were prepared by sol-gel methods of SiO2 and SiO2-TiO2 as a xerogel followed by impregnating Al2O3 powder with the nickel nitrate precursor. The crystalline structure and catalytic properties for the catalysts were investigated by use of BET surface area, X-ray diffraction (XRD), Xray photoelectron spectroscopy (XPS) and temperature programmed reduction (TPR) techniques. These results show that nickel oxide is transformed to NiAl2O4 spinel structure at the calcination temperature of 400 °C in response to the steps with after- and co-impregnation of Al2O3 powder in sol-gel process. The NiAl2O4 could suppress the oxidation reaction of acetaldehyde by catalysts. The NiO is better dispersed on SiO2-TiO2/Al2O3 support than SiO2/Al2O3 and SiO2-TiO2-Al2O3 supports. From the testing results of catalytic activities for oxidation of acetaldehyde, Catalysts showed a big difference in conversion efficiencies with the way of the preparation of catalysts and the loading weight of nickel. The catalyst of 8 wt.% Ni/TiO2-SiO2/Al2O3 showed the best conversion efficiency on acetaldehyde oxidation with 100% conversion efficiency at 350 °C.