• Title/Summary/Keyword: Sol-gel chemistry

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Sol-gel TiO2/Carbon Paste Electrode Nanocomposites for Electrochemical-assisted Sensing of Fipronil Pesticide

  • Maulidiyah, Maulidiyah;Azis, Thamrin;Lindayani, Lindayani;Wibowo, Dwiprayogo;Salim, La Ode Agus;Aladin, Andi;Nurdin, Muhammad
    • Journal of Electrochemical Science and Technology
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    • v.10 no.4
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    • pp.394-401
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    • 2019
  • The unique study of TiO2 sol-gel modified carbon paste electrode (CPE) nanocomposites have been developed for electrochemical sensor detecting fipronil pesticide compound. We develop the easy synthesized TiO2 via a sol-gel method and modified in CPE which applied electrochemical system as cyclic voltammetry (CV) because the concentration is proportional with current peaks. We discover the TiO2 optimal mass used of 0.1 g which is compared with 0.7 g carbon and 0.3 mL paraffin. It has high-current anodic (Ipa) of 1.13×103 μA and high-current cathodic (Ipc) -0.96×103 μA in scan rate of 0.5 V/s. The limit of detection (LOD) of fipronil has been determined of 34.0×10-5 μM in percent recovery of 0.8%. Its high-stability for lifetime TiO2-CPE nanocomposites was expressed for 13 days which mean that can be used for detecting fipronil pesticide.

Electrogenerated Chemiluminescence Sensor Based on Tris(2,2'-bipyridyl) ruthenium(II) Immobilized in the Composite Film of Multi-walled Carbon Nanotube/Sol-gel Zinc oxide/Nafion

  • Choi, Eun-Jung;Kang, Chang-Hoon;Choi, Han-Nim;Lee, Won-Yong
    • Bulletin of the Korean Chemical Society
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    • v.30 no.10
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    • pp.2387-2392
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    • 2009
  • A composite film of multi-walled carbon nanotube (MWCNT)/sol-gel-derived zinc oxide(ZnO)/Nafion has been utilized as an efficient immobilization matrix for the construction of a highly sensitive and stable tris(2,2'-bipyridyl) ruthenium(II) (Ru(${bpy)_3}^{2+})$ electrogenerated chemiluminescence (ECL) sensor. The electrochemical and ECL behaviors of Ru(${bpy)_3}^{2+})$ ion-exchanged into the composite film were strongly dependent upon the sol-gel preparation condition, the amount of MWCNT incorporated into the ZnO/Nafion composite film, and the buffer solution pH. The synergistic effect of MWCNTs and ZnO in the composite films increased not only the sensitivity but also the long-term stability of the ECL sensor. The present ECL sensor based on the MWCNT/ZnO/Nafion gave a linear response ($R^2$ = 0.999) for tripropylamine concentration from 500 nM to 1.0 mM with a remarkable detection limit (S/N = 3) of 15 nM. The present ECL sensor showed outstanding long-term stability (94% initial signal retained for 5 weeks). Since the present ECL sensor exhibits large response towards NADH, it could be applied as a transduction platform for the ECL biosensor in which the NADH is produced from the dehydrogenase-based enzymatic reaction in the presence of NA$D^+$ cofactor.

A Novel Acid-Base Catalyzed Sol-Gel Synthesis of Highly Active Mesoporous TiO2 Photocatalysts

  • Khan, Romana;Kim, Sun-Woo;Kim, Tae-Jeong;Lee, Hyo-Sun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.1951-1957
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    • 2007
  • A new synthetic strategy based on the acid-base catalyzed sol-gel method was developed for the preparation of a series of mesoporous TiO2 nanoparticles. A key feature of the method involves a gradual change in pH (0.8- 9) during the sol-gel transition, which guarantees easy introduction of mesoporosity without relying on the well-established sonochemical or template approach. In addition, this method leads to the exclusive formation of the anatase phase stable enough to the calcination temperature up to 600 oC. The physicochemical properties of the particles in the series were characterized by various spectroscopic and analytical techniques such as wide-angle XRD, SAXRD, BET surface area, FE-SEM, TEM, FT-IR, TGA, and XPS. The photocatalytic efficiency of these materials was investigated for the oxidation of toluene under UV-irradiation. All but T-ad in the series exhibited high photocatalytic activity pushing the reaction into completion within 3 h. The reaction followed the first order kinetics, and the rate reaches as high as 3.9 × 10?2/min which exceeds the one with the commercially available Degussa P-25 by a factor of 3.2. When comparison is made among the catalysts, the reactivity increases with increase in the calcination temperature which in turn increases the crystallinity of the anatase phase, thus revealing the following rate orders: T-3 < T-4 < T-5 < T-6.

High Tc Superconductor Fiber $YBa_2Cu_3O_{7-{\sigma}}$ Synthesized by the Sol-gel Process (Sol-gel 법에 의한 고온 초전도체 $YBa_2Cu_3O_{7-{\sigma}}$ 선재 합성에 관한 연구)

  • Jin Ho Choy;Jong Seok Yoo;Bae Whan Kim;Seung Tae Hong
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.326-331
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    • 1989
  • Superconducting fiber of high Tc $YBa_2Cu_3O_{7-{\sigma}}$ was successfully prepared by the sol-gel method. The stoichiometric mixture of Y, Ba and Cu nitrates was dissolved in water, to which citric acid solution was added. Then ammonium hydroxide was added to the mixture in order to increase the pH to a value between 5.8 and 6.2. The mixture was heated carefully to form a homogeneous colloid sol at 358 K. The solution was viscous enough to draw a long gel fiber, which was then heated at 1223K for 8 hrs. under oxygen partial pressure of $Po_2$ = 1 atm., cooled slowly and annealed at 723K for 13 hrs.. The reacted superconducting sample maintained a fiber form with some shrinkage of its volume. The superconducting transition temperatures (Tc, onset and Tc, offset) of $YBa_2Cu_3O_{7-{\sigma}}$ have been determined to be approximately 95K and 82K, respectively. The superconducting phase was also confirmed by Meissner effect at liquid nitrogen boiling temperature.

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Sol-Gel Derived Nitrogen-Doped TiO2 Photoanodes for Highly Efficient Dye-Sensitized Solar Cells

  • Kim, Sang Gyun;Ju, Myung Jong;Choi, In Taek;Choi, Won Seok;Kim, Hwan Kyu
    • Rapid Communication in Photoscience
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    • v.3 no.1
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    • pp.20-24
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    • 2014
  • N-doped anatase $TiO_2$ nanoparticles were prepared by the sol-gel process followed by a hydrothermal treatment and successfully used as the photoanodes in organic dye-sensitized solar cells (DSSCs). As expected, the power conversion efficiency (PCE) of 8.44% was obtained for the NKX2677/HC-A-sensitized DSSC based on the 30 mol% N-doped $TiO_2$ photoanode, which was an improvement of 23% relative to that of the DSSC based on the NKX2677/DCA.

SnO2/SiO2 Nanocomposite Catalyzed One-Pot Synthesis of 2-Arylbenzothiazole Derivatives

  • Yelwande, Ajeet A.;Navgire, Madhukar E.;Tayde, Deepak T.;Arbad, Balasaheb R.;Lande, Machhindra K.
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1856-1860
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    • 2012
  • $SnO_2/SiO_2$ nanocomposite has been synthesized by using sol-gel method. Prepared catalytic materials has been well characterized by using X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR), Brunauer-Emmer-Teller (BET) surface area, and temperature-programmed desorption of ammonia ($NH_3$-TPD). $SnO_2/SiO_2$ nanocomposite catalyzed synthesis of 2-arylbenzothiazoles by the cyclocondensation of 2-aminothiophenol and aromatic aldehydes under reflux condition in 1:1 EtOH:$H_2O$. After completion of the reaction, catalyst can be recovered efficiently and reused with consistent activity.

A pH Optosensor Based on Fluoresence from Nile Blue Encapsulated within Silica Sol-Gel Film (실리카 졸-겔막을 이용한 pH 광학센서)

  • Lee, Jung-Min;Li, Ming;Lee, Sang-Hak;Kim, Young-Sun;Kim, Chang-Jin;Lee, Boo-Huyng
    • Journal of Sensor Science and Technology
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    • v.13 no.3
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    • pp.169-174
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    • 2004
  • A fiber optic pH sensor has been fabricated using nile blue entrapped in an ammonia catalyzed silica sol-gel film coated on glass substrate by dip-coating. The sensor was fixed on the end of an optical fiber. The sensor showed pH sensitivity when dipped into liquids at different pHs. Linear and reproducible responses were obtained in standard buffer solutions in the pH range $6.0{\sim}8.5$, which encompasses the clinically-relevant range. The effects of interferences on the determination of pH were also investigated. The sensors were successfully applied to the determination of pH in different commercial ionic drinks.

Structural and Thermal Characteristics of Synthesized SiC by Carbothermal Reaction and Sol-gel Method (Carbothermal 반응법과 졸-겔법에 의해 합성된 SiC의 구조적 특성과 열역학적 특성)

  • Oh, Won-Chun;Kim, Bum-Soo
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.156-160
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    • 1998
  • SiC is synthesized by sol-gel and carbothermal reaction method from various carbon sources and Si source and characterized through the results of DSC and XRD. More SiC has been formed in carbothermal reaction than sol-gel method. From the XRD results, the degree of formation of SiC increases in the order of petroleum cokes, activated carbon, artificial graphite all in two introduced methods. Based on the DSC data, the enthalpy values for the exothermic reaction decrease in the order of activated carbon, petroleum cokes, artificial graphite in carbothermal reaction methods, while those for the endothermic reactions increase in the reverse order. But, the enthalpy values for the exothermic reactions decrease in the order of petroleum cokes, activated carbon, artificial graphite in sol-gel methods.

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Synthesis and Characterization of Nanosized of Spinel LiMn2O4 via Sol-gel and Freeze Drying Methods

  • Seyedahmadian, Masoud;Houshyarazar, Shadi;Amirshaghaghi, Ahmad
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.622-628
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    • 2013
  • Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.

Preparation of Silver-doped Hydroxyapatite Using Sol-gel Method (졸-겔법을 이용한 은 담지 하이드록시아파타이트의 제조)

  • Mun Byung-Bae;Kim Ho-Kun
    • Journal of Powder Materials
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    • v.12 no.6 s.53
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    • pp.428-432
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    • 2005
  • In the present study, silver-doped antibacterial hydroxyapatites were successfully prepared by the sol-gel method. For the starting solution, the molar ratio of $Ca(NO_3)_2{\cdot}4H_2O, P(OC_2H_5)_3,\;C_2H_5OH,\;and\;H_O$ was set to 0.075:0.045:20:0.135; $AgNO_3$ was added to a ratio of Ag to total cation concentration of $0.5-12 mol\%$. The prepared sol was dried at $100^{\circ}C$ for 48h and heat-treated at $1000^{\circ}C$ for 2h to obtain particles in the 200-500nm size range. The product from the synthesis of silver-doped hydroxyapatite was investigated through X-ray diffraction experiments and scanning electron microscopy. The product showed high antibacterial properties, with a disinfection ratio of Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 25922) over $99.9^{\circ}C$ as calculated from an antimicrobial effects evaluation by the shake flask method.