• Title/Summary/Keyword: Sol-Gel reaction

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The synthesis of Highly Crystalline and monodisperse maghemite and zirconia Nanocrystallites without size-selection process

  • Park, Jong-Nam;Joo, Jin;Yoo, Tae-kyung;Na, Hyun-Bin;Lee, Soo-Sung;Park, Hyun-Min;Kim, Young-Woon;Hyun, Taek-Hwan
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2003.05a
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    • pp.20-20
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    • 2003
  • A new and simple method has been developed to synthesize highly crystalline and monodisperse maghemite (γ-Fe₂O₃) and zirconia (ZrO₂) nanocristallites. High temperature aging of metal-surfactant complex was founded to generate monodisperse nanoparticles, wherein the nuclei were prepared by the thermal decomposition of iron-oleate complex in case of iron oxide and nonhydrolytic sol-gel reaction in case of zirconia respectively. By varying the experimental conditions, in other words concentration of surfactants, kind of metal precursor, reaction temperature and so on, the diameter of spherical nanoparticles could be controlled at various size. The synthesized nanoparticles were characterized by electron diffraction, X-ray diffraction, and low- and high-resolution transmission electron microscope.

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Synthesis and Magnetic Properties of Nanosized Ce-substituted Yttrium Iron Garnet Powder Prepared by Sol-gel Method (졸-겔법에 의한 Cerium 치환 Nanosize YIG 분말의 합성 및 자기적 특성)

  • 장학진;김광석;윤석영;김태옥
    • Journal of the Korean Ceramic Society
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    • v.38 no.11
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    • pp.1008-1014
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    • 2001
  • Nanosize YIG powders added by Cerium which is exellent element in magneto-optical effect were synthesized by Sol-Gel method using Ethylene Glycol solvent. In 120 to 150 minute reaction time, stable sol solution which showed no change in viscosity, pH, and aging time was obtained. Monolithic YIG was synthesized at 80$0^{\circ}C$ with DTA and XRD measurement and its lattice parameter had a tendency to increase from 12.3921 $\AA$. Increasing annealing temperature from 80$0^{\circ}C$ to 105$0^{\circ}C$, average particle size was in the range of 40 nm to 330 nm. Saturation magnetization (M$_{s}$) value was increased from 18.37 to 21.25 emu/g due to enhancement of YIG crystallity and decreasing of orthoferrite phase. On the other hand, coercivity (H$_{c}$) value increased up to 90$0^{\circ}C$ and then decreased above 90$0^{\circ}C$. With increasing Ce addition, coercivity was almost not changed but saturation magnetization value was maximum at Ce 0.1 mol% and then decreased because of increasing a orthoferrite amount. Also, curie temperature (T$_{c}$) of YIG were not changed with Ce addition.ion.

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Synthesis and Physical Properties of MO·Fe12O18 (M/Ba and Sr) Nanoparticles Prepared by Sol-Gel Method Using Propylene Oxide (Propylene Oxide를 이용한 졸-겔법에 의한 MO·Fe12O18 (M/Ba, Sr) 나노 분말의 합성과 물리적 특성)

  • Lee, Su Jin;Choe, Seok Burm;Gwak, Hyung Sub;Paik, Seunguk
    • Applied Chemistry for Engineering
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    • v.17 no.4
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    • pp.420-425
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    • 2006
  • Nano sized mixed metal hexagonal ferrite powders with improved magnetic properties have been prepared by sol-gel method using propylene oxide as a gelation agent. To obtain the desired ferrite, two different metal ions were used. One of the ions has only +2 formal charge. The key step in the processes is that hydrated $Ba^{2+}$ or $Sr^{2+}$ ions are hydrolyzed and condensed at the surface of the previously formed $Fe_{2}O_{3}$ gel. In this processes, all the reaction can be finished within a few minutes. The magnetic properties of the produced powder were improved by heat treatment. The highest values of the magnetic properties were achieved at temperature $150^{\circ}C$ lower than those of the previously published values. The highest observed values of coercivity and the saturation magnetization of Sr-ferrite and Ba-ferrite powder were 6198 Oe, 5155 Oe and 74.4 emu/g, 68.1 emu/g, respectively. The ferrite powder annealed at $700^{\circ}C$ showed spherical particle shapes. The resulting spheres which were formed by the aggregation of nanoparticles with size 3~5 nm have diameter around 50 nm. The powder treated at $800^{\circ}C$ showed hexagonal-shaped grains with crystallite size above 500 nm.

An Efficient and Green Approach for the Esterification of Aromatic Acids with Various Alcohols over H3PO4/TiO2-ZrO2

  • Kalbasi, Roozbeh Javad;Massah, Ahmad Reza;Barkhordari, Zeynab
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2361-2367
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    • 2010
  • $TiO_2-ZrO_2$ was prepared with surfactant through a sol-gel method. Catalysts containing 5 - 35% $H_3PO_4$ were prepared using these oxides. Subsequently the catalytic performance of prepared catalysts was determined for liquid phase esterification of aromatic acids. $H_3PO_4/TiO_2-ZrO_2$ has been used as catalyst to synthesize various novel esters by esterification of some aromatic acids with aliphatic alcohols (2-propanol, 1-butanol, iso butanol, 3-pentanol, 1-hexanol, heptanol, cyclo heptanol, octanol and decanol). Under optimized conditions, maximum yields and selectivity (100%) to the corresponding ester, was obtained by using 25 wt % $H_3PO_4/TiO_2-ZrO_2$ as catalyst. The Catalyst can be easily recycled after reaction and can be reused without any significant loss of activity/selectivity performance. No by-product formation, high yields, short reaction times, mild reaction conditions, operational simplicity with reusability of the catalyst are the salient features of the present synthetic protocol. The reaction was carried out under solvent-free condition.

Improved Photo Degradation of Rhodamine B Dye using Iron Oxide/Carbon Nanocomposite by Photo-Fenton Reaction

  • Kim, Min-Il;Im, Ji-Sun;In, Se-Jin;Kim, Hyuk;Kim, Jong-Gyu;Lee, Young-Seak
    • Carbon letters
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    • v.9 no.3
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    • pp.195-199
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    • 2008
  • A nanocomposite consisting of $Fe_3O_4$ and MWCNT was produced via sol-gel technique using $FeCl_3$ along with MWCNT by calcination at $300^{\circ}C$. The degradation effect of rhodamine B dye has been investigated under UV illumination in a darkroom. The degradation reaction was studied by monitoring the discoloration of dye as a function of irradiation time using UV-visible spectrophotometeric technique. The $Fe_3O_4$-MWCNT samples have continuous degradation ability under the UV illumination with the first order kinetics and the dye removal was better than in the pristine $Fe_3O_4$. The resultant composite catalyst was found to be efficient for the photo-Fenton reaction of the dye.

Fabrication of Silica-Containing Breathable Waterproof Polyurethane Dispersion Film (Silica를 함유하는 Polyurethane dispersion 투습방수 Film의 제조)

  • Shin, Hyun-Ki;Huh, Man-Woo;Yoon, Nam-Sik
    • Textile Coloration and Finishing
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    • v.27 no.2
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    • pp.126-131
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    • 2015
  • Silica-polyurethane hybrid breathable films were prepared and their breathabilities were assessed. Appropriately aggregated silica was prepared through sol-gel reaction of water glass and its particle size ranged 360~500nm. The polyurethane dispersion was prepared by the reaction of isophorone diisocyanate(IPDI) as diisocyanate and polytetramethylene glycol(PTMG) and dimethylol propionic acid(DMPA) as polyol, particle size ranging 30~120nm. The reaction between isocyanate and hydroxyl group to form urethane bonding was checked by the intensity of the stretch peak of isocyanate at $2270cm^{-1}$ in the FT-IR. The silica was incorporated into polyurethane dispersion and casted into film. It was shown that the incorporated silica(1~5wt.%) increased water vapour permeability of the films by 30~100%, and decreased the hydrostatic pressure by 10~40%. From the results, it could be concluded that the appropriate hybridization of silica can increase the breathability of polyurethane dispersion film, while minimizing the loss of hydrostatic pressure.

Synthesis of Solid Electrolyte Nasicon by Solid State Reaction

  • Kim, Cheol-Jin;Chung, Jun-Ki;Lim, Sung-Ki;Rhee, Meung-Ho
    • The Korean Journal of Ceramics
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    • v.2 no.1
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    • pp.25-32
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    • 1996
  • Solid electroyte nasion was synthesized by the optimized solid state reaction minimizing the volume fraction of secondary $ZrO_2$ and glassy phases. To compensate for the evaporation of Na and P during heat-treatment, excess Na and P were added to the starting composition $Na_{1+x} Zr_2 Si_x P_{d-x} O_{12}$ (x=2.1). Phases pure nasicon comparable in volume fraction to the one obtaied from sol-gel process were synthesized after the reaction at $1100~1150^{\circ}C$,$ P_{O2}>=0.1-0.15 $$ZrO_2$ increased with the heat-treatment time due to the decomposition of nasicon phase and that of glassy phase increased as partial oxygen pressure decreased. The synthesized nasion showed a good electrical conductivity of $-1{\times}10^{-2}({\omega}{\cdot}cm)^{-1}$ at $350^{\circ}C$.

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Synthesis of Fe/SiO2 Core-Shell Nanoparticles by a Reverse Micelle and Sol-Gel Processes

  • Son, Jeong-Hun;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.22 no.6
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    • pp.298-302
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    • 2012
  • Fe/$SiO_2$ core-shell type composite nanoparticles have been synthesized using a reverse micelle process combined with metal alkoxide hydrolysis and condensation. Nano-sized $SiO_2$ composite particles with a core-shell structure were prepared by arrested precipitation of Fe clusters in reverse micelles, followed by hydrolysis and condensation of organometallic precursors in micro-emulsion matrices. Microstructural and chemical analyses of Fe/$SiO_2$ core-shell type composite nanoparticles were carried out by TEM and EDS. The size of the particles and the thickness of the coating could be controlled by manipulating the relative rates of the hydrolysis and condensation reaction of TEOS within the micro-emulsion. The water/surfactant molar ratio influenced the Fe particle distribution of the core-shell composite particles, and the distribution of Fe particles was broadened as R increased. The particle size of Fe increased linearly with increasing $FeNO_3$ solution concentration. The average size of the cluster was found to depend on the micelle size, the nature of the solvent, and the concentration of the reagent. The average size of synthesized Fe/$SiO_2$ core-shell type composite nanoparticles was in a range of 10-30 nm and Fe particles were 1.5-7 nm in size. The effects of synthesis parameters, such as the molar ratio of water to TEOS and the molar ratio of water to surfactant, are discussed.

Revealing Strong Metal Support Interaction during CO Oxidation with Metal Nanoparticle on Reducible Oxide Substrates

  • Park, Dahee;Kim, Sun Mi;Qadir, Kamran;Park, Jeong Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.264-264
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    • 2013
  • Strong metal-support interaction effect is an important issue in determining the catalytic ac-tivity for heterogeneous catalysis. In this study, we investigated the support effect and the role of organic capping layers of two-dimensional Pt nanocatalysts on reducible metal oxide supports under the CO oxidation. Several reducible metal oxide supports including CeO2, Nb2O5, and TiO2 thin films were prepared via sol-gel techniques. The structure, chemical state and optical property were characterized using XRD, XPS, TEM, SEM, and UV-VIS spectrometer. We found that the reducible metal oxide supports have a homogeneous thin thickness and crystalline structure after annealing at high temperature showing the different optical band gap energy. Langmuir-Blodgett technique and arc plasma deposition process were employed to ob-tain Pt nanoparticle arrays with capping and without capping layers, respectively on the oxide support to assess the role of the supports and capping layers on the catalytic activity of Pt catalysts under the CO oxidation. The catalytic performance of CO oxidation over Pt supported on metal oxide thin films under oxidizing reaction conditions (40 Torr CO and 100 Torr O2) was tested. The results show that the catalytic activity significantly depends on the metal oxide support and organic capping layers of Pt nanoparticles, revealing the strong metal-support interaction on these nanocatalysts systems.

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The Syntheses, Characterizations, and Photocatalytic Activities of Silver, Platinum, and Gold Doped TiO2 Nanoparticles

  • Loganathan, Kumaresan;Bommusamy, Palanisamy;Muthaiahpillai, Palanichamy;Velayutham, Murugesan
    • Environmental Engineering Research
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    • v.16 no.2
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    • pp.81-90
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    • 2011
  • Different weight percentages of Ag, Pt, and Au doped nano $TiO_2$ were synthesized using the acetic acid hydrolyzed sol-gel method. The crystallite phase, surface morphology combined with elemental composition and light absorption properties of the doped nano $TiO_2$ were comprehensively examined using X-ray diffraction (XRD), $N_2$ sorption analysis, transmission electron microscopic (TEM), energy dispersive X-ray, and DRS UV-vis analysis. The doping of noble metals stabilized the anatase phase, without conversion to rutile phase. The formation of gold nano particles in Au doped nano $TiO_2$ was confirmed from the XRD patterns for gold. The specific surface area was found to be in the range 50 to 85 $m^2$/g. TEM images confirmed the formation a hexagonal plate like morphology of nano $TiO_2$. The photocatalytic activity of doped nano $TiO_2$ was evaluated using 4-chlorophenol as the model pollutant. Au doped (0.5 wt %) nano $TiO_2$ was found to exhibit higher photocatalytic activity than the other noble metal doped nano $TiO_2$, pure nano $TiO_2$ and commercial $TiO_2$ (Degussa P-25). This enhanced photocatalytic activity was due to the cathodic influence of gold in suppressing the electron-hole recombination during the reaction.