• Title/Summary/Keyword: in-situ reaction synthesis

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The Role of Surface Oxide of Metal Nanoparticles on Catalytic Activity of CO Oxidation Unraveled with Ambient Pressure X-ray Photoelectron Spectroscopy

  • Park, Jeong Young
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.132-132
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    • 2013
  • Colloidal synthesis of nanoparticles with well-controlled size, shape, and composition, together with development of in situ surface science characterization tools, such as ambient pressure X-ray photoelectron spectroscopy (APXPS), has brought new opportunities to unravel the surface structure of working catalysts. Recent studies suggest that surface oxides on transition metal nanoparticles play an important role in determining the catalytic activity of CO oxidation. In this talk, I will outline the recent studies on the influence of surface oxides on Rh, Pt, Ru and Co nanoparticles on the catalytic activity of CO oxidation [1-3]. Transition metal nanoparticle model catalysts were synthesized in the presence of poly(vinyl pyrrolidone) polymer capping agent and deposited onto a flat Si support as two-dimensional arrays using the Langmuir-Blodgett deposition technique. APXPS studies exhibited the reversible formation of surface oxides during oxidizing, reducing, and CO oxidation reaction [4]. General trend is that the smaller nanoparticles exhibit the thicker surface oxides, while the bigger ones have the thin oxide layers. Combined with the nature of surface oxides, this trend leads to the different size dependences of catalytic activity. Such in situ observations of metal nanoparticles are useful in identifying the active state of the catalysts during use and, hence, may allow for rational catalyst designs for practical applications. I will also show that the surface oxide can be engineered by using the simple surface treatment such as UV-ozone techniques, which results in changing the catalytic activity [5]. The results suggest an intriguing way to tune catalytic activity via engineering of the nanoscale surface oxide.

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Synthesis and characterization of polybenzoxazole/graphene oxide composites via in situ polymerization

  • Lim, Jun;Kim, Min-Cheol;Goh, Munju;Yeo, Hyeounk;Shin, Dong Geun;Ku, Bon-Cheol;You, Nam-Ho
    • Carbon letters
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    • v.14 no.4
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    • pp.251-254
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    • 2013
  • In this study, poly(amic acid) was prepared via a polycondensation reaction of 3,3'-dihydroxybenzidine and pyromellitic dianhydride in an N-methyl-2-pyrrolidone solution; reduced graphene oxide/polybenzoxazole (r-GO/PBO) composite films, which significantly increased the electrical conductivity, were successfully fabricated. GO was prepared from graphite using Brodie's method. The GO was used as nanofillers for the preparation of r-GO/PBO composites through an in situ polymerization. The addition of 50 wt% GO led to a significant increase in the electrical conductivity of the composite films by more than sixteen orders of magnitude compared with that of pure PBO films as a result of the electrical percolation networks in the r-GO during the thermal treatment at various temperatures within the films.

Synthesis of Poly(Styrene-co-GMA) and its Application as in situ Reactive Compatabilizer (Poly(Styrene-co-GMA)의 합성과 in situ Reactive Compatabilizer 로서의 응용)

  • Kim, Ju-Young;Suh, Kyung-Do
    • Applied Chemistry for Engineering
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    • v.3 no.3
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    • pp.499-506
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    • 1992
  • Copolymer of Styrene and GMA(glycidyl methachylate), having reactive ratios of $r_1=0.53$, $r_2=0.44$, was synthesized in dioxane using AIBN as free radical initiator. Followed by the reaction of ethylene diamine with copolymer PGS, amine groups were introduced to the PGS(NPGS). The composition of copolymer was determined by elemental analyzer. Poly(glycidyl methacrylate) (PGMA) was obtained in benzene using AIBN as free radical initiator. The NPGS-PGMA blend of 50/50 composition was prepared by mixing these polymers in THF at $65^{\circ}C$. Glass transition temperature (Tg) of NPGS-PGMA blend was measured by DSC. The blend showed a single Tg. Accordingly, it was clear that the NPGS was compatible with PGMA. An intermolecular reaction between amine groups of NPGS and epoxy groups of PGMA imparts compatibility in the NPGS-PGMA blend. When the NPGS-PGMA blend was added to the incompatible PS-PGMA blend, PS-PGMA blend showed Tg change. Scanning Electron Micrograph(SEM) showed a fine morphology in this blend. Consequently, it was apparent that the NPGS-PGMA blend acted as a compatibilizer for the PS-PGMA blend.

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Synthesis of Ceramic Protective Coatings for Chemical Plant Parts Operated in Hi-temperature and Corrosive/Erosive Environment

  • Son, M.C.;Park, J.R.;Hong, K.T.;Seok, H.K.
    • Corrosion Science and Technology
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    • v.4 no.1
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    • pp.33-38
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    • 2005
  • Some feasibility studies are conducted to produce an advanced ceramic coating, which reveals superior chemical and mechanical strength, on metal base structure used in chemical plant. This advanced coating on metallic frame can replace ceramic delivery pipe and reaction chamber used in chemical plant, which are operated in hi-temperature and corrosive/erosive environment. An dual spraying is adopted to reduce the residual stress in order to increase the coating thickness and the residual stress is estimated by in-situ manner. Then new methodology is tried to form special coating of yttrium aluminum garnet(YAG), which reveals hi-strength and low-creep rates at hi-temperature, superior anti-corrosion property, hi-stability against Alkali-Vapor corrosion, and so on, on iron base structure. To verify the formation of YAG during thermal spraying, XRD(X ray diffraction) technique was used.

Synthesis of Ni Silicides by Mechnical Alloying (기계적 합금화에 의한 Ni Silicide 분말의 합성)

  • 변창섭
    • Journal of Powder Materials
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    • v.6 no.2
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    • pp.145-151
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    • 1999
  • Nickel silicides ($Ni_5$Si$_2$, Ni$_2$Si and NiSi) have been synthesized by mechanical alloying (MA) of Ni-27.9at.9at%Si, Ni-33.3at% and Ni-50.0at% powder mixtures, respectively. From in situ thermal analysis, eash citical milling period for the formation of the three phases was observed to be 40.2, 34.9 and 57.5 min, at which there was a rapid increase in temperature. This indicates that rapid, self-propagating high-temperature synthesis (SHS) reactions were observed to produce the three phases during room-temperature high-energy ball milling of elemental powders. Each Ni silicide, Ni and Si, however, coexisted for an extended milling time even after the critical milling period. The powders mechanically alloyed after the critical period showed the rapid increase in microhardness. The Hv values were found to be higher than 1000kgf/mm$^2$. The formation of nickel silicides by mechanical alloying and the relevant reaction rates appeared to be influenced by the critical milling period and the heat of formation of the products involved ($Ni_5$Si$_2$$\rightarrow$-43.1kJ/mol.at., Ni$_2$Si$\rightarrow$-47.6kJ/mol.at., NiSi$\rightarrow$-42.4kJ/mol.at).

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Studies on the Synthesis of Bis-dithiocarbamates as Prodrugs of Isothiocyanates (Isothiocyanate 유도체의 Prodrug를 위한 합성 연구)

  • 심영섭;정오영;김완주;이문희
    • YAKHAK HOEJI
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    • v.26 no.2
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    • pp.91-96
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    • 1982
  • In an attempt to design prodrugs for the Derivatives of the Isothiocyanates R-N=C=S were synthesized eleven novel bis-dithiocarbamates. The best way of preparing the dithiocarbamates was the formation of the dithiocarbonates followed by the reaction of the dithiocarbonates with amines. Thus, the treatment of the diols with carbon disulfide in the presense of potassium hydroxide afforded the potassium salts of the ditniocarbonic acids. The potassium salts were then reacted with alkyl halides to give the dithiocarbonates, which upon treatment with amines produces the dithiocarbamates. In case of vicinal diol (n=o in the above formula), only one of the hydroxy groups was reacted to give the mono-dithiocarbonate. The dithiocarbonates failed to react with amides and aromatic amines. Dithiocarbonates of the different types were obtained when the active double bonds, such as $CH_{2}=CH-Z$ , (Z are electron withdrawing groups), were allowed to react with the free dithiocarbonic acids produced in situ by carefully neutralizing the Potassium salts of the corresponding acids. These compounds are considered to be of some value as prodrugs for the active double bonds.

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Efficient Synthesis of 1,3-Thiazole Derivatives from Arylidenethiosemicarbazones in the Presence of β-Cyclodextrin with Water (수용액과 β-Cyclodextrin 하에서 Arylidenethiosemicarbazone들로부터 1,3-Thiazole 유도체들의 효율적 합성)

  • Park, Kyung-Jin;Bae, Sun Kun
    • Applied Chemistry for Engineering
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    • v.18 no.4
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    • pp.326-329
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    • 2007
  • 2-Arylidenehydrazinyl-4-arylthiazole derivatives (9a-f) were prepared by the in situ formation of ${\beta}$-cyclodextrin complex of 2,4'-dibromoacetophenone (8) in water followed by the addition of arylidenethiosemicarbazones (7a-f) in 70~88% yield. The structures of the compounds 9a-f were elucidated by IR and $^1H-NMR$ spectral data. The role of ${\beta}$-cyclodextrin appears to activate the compound 7 and 8 and promote the reaction to complete in reduced reaction time.

Synthesis of Fe-TiB2 Nanocomposite by a combination of mechanical activation and heat treatment

  • Hyunh, Xuan Khoa;Nguyen, Quoc Tuan;Kim, Ji-Sun;Gang, Tae-Hun;Kim, Jin-Cheon;Gwon, Yeong-Sun
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2012.05a
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    • pp.91.2-91.2
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    • 2012
  • The TiB2-reinforced iron matrix nanocomposite (Fe-TiB2) was in-situ fabricated from titanium hydride (TiH2) and iron boride (FeB) powders by a simple and cost-effective process that combines the mechanical activation (MA) and a subsequent heat treatment (HT). Effect of milling factors and synthesized temperatures on the formation of the nanocomposite were presented and discussed. A differential thermal analyser (DSC-TG) was employed for examination of thermal behavior of MAed powders. Phases of the nanocomposite were confirmed by X-ray diffraction analysis (XRD). The morphologies and microstructure of nanocomposite were investigated by field emission-scanning electron microscopy (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS). Phase composition and distribution were analyzed by electron probe X-ray microanalysis (EPMA). Results showed that TiB2 particles formed in nanoscale were uniformly distributed in alloyed Fe matrix.

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Study on the Development of CVD Precursors II-Synthesis and Properties of New Lathanum β-diketonates

  • 임종태;홍성택;이중철;이익모
    • Bulletin of the Korean Chemical Society
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    • v.17 no.11
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    • pp.1023-1031
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    • 1996
  • A new synthetic route for the lanthanum β-diketonate compounds via in-situ formed lanthanum alkyl complexes was developed in the process for the development of suitable MOCVD (metal-organic chemical vapor deposition) precursors of PLT, one of the promising material for the ferroelectric film. A series of lanthanum β-diketonate compounds were successfully synthesized by this method. This new method is found to have some merits; versatile method for almost every β-diketone, β-hydroxyketone, and β-hydroxyaldehyde, short reaction time, easy purification for high purity, moderate to high yield, and easy access to anhydrous compounds. In some cases, anhydrous oligomeric products fail to show the higher volatility. On the other hand, some lanthanum β-diketonates with aromatic groups such as La(1,3-biphenyl-l,3-propandione)3 are found to have favorable properties for a precursor of lanthanum oxide, one of major components of PLT, such as low melting point, and much higher decomposition temperature. A plausible pyrolysis mechanism is proposed by the TGA, where consecutive dissociation of R, CO, CH, C, and O fragments occurs.

Synthesis and Characterization of Allyl Ester Resin-Layered Silicate Nanocomposite (알릴 에스터 수지-층상 실리케이트 나노복합재료의 합성과 특성)

  • 팽세웅;김장엽;허완수;조길원;이상원
    • Polymer(Korea)
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    • v.28 no.2
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    • pp.177-184
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    • 2004
  • Polymer-clay nanocomposite containing the low amounts of clay shows improved physical, mechanical properties. In this study, allyl ester prepolymer was synthesised by reactions of the diallyl terephthalate monomers and the 1,3-butanediol monomers. Nanocomposites of allyl ester prepolymer and the two kinds of the organically layered silicate were prepared by using the intercalation method as well as the in-situ polymerization method using. By varying the amount of clay content, curing conditions, and feeding conditions. the nanocomposite was studied using X-ray diffraction. From XRD results, allyl ester-Cloisite 30 B nanocomposite made by the in-situ polymerization method shows better exfoliation behavior compared with the intercalation method. It can be said that the transesterification reaction between functional groups (-OH) of intercalant and monomers results in the increased gallery distance. Also mechanical and thermal properties indicate that the dispersity of clay is an important factor for improving physical properties of the nanocomposite.