• Title/Summary/Keyword: Solution-polymerization route

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Characterization of Chemically Stabilized $\beta$-cristobalite Synthesized by Solution-Polymerization Route

  • Lee, Sang-Jin
    • The Korean Journal of Ceramics
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    • v.3 no.2
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    • pp.116-123
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    • 1997
  • A chemically stabilized $\beta$-cristobalite, which is stabilized by stuffing cations of $Ca^{2+}$ and $Al^{3+}$, was prepared by a solution-polymerization route employing Pechini resin or PVA solution as a polymeric carrier. The polymeric carrier affected the crystallization temperature, morphology of calicined powder, and particle size distribution. In case of the polyvinyl alcohol (PVA) solution process, a fine $\beta$-cristobalite powder with a narrow particle size distribution (average particle size : 0.3$\mu\textrm{m}$) and a BET specific surface area of 72 $\m^2$/g was prepared by an attrition-milling for 1 h after calcination at 110$0^{\circ}C$ for 1h. Wider particle size distribution and higher specific surface area were observed for the $\beta$-cristobalite powder derived from Pechini resin. The cubie(P1-to-tetraganalb) phase transformation in polynystalline $\beta$-cristobalite was induced at approximately 18$0^{\circ}C$. Like other materials showing transformation toughening, a critical size effect controlled the $\beta$-to-$\alpha$ transformation. Densifed cristobalite sample had some cracks in its internal texture after annealing. The cracks, occurred spontaneoulsy on cooling, were observed in the sample with an average grain sizes of 4.0 $\mu\textrm{m}$ or above. In case of the sintered cristobalite having a composition of CaO.$2Al_2O_3$.40SiO$_2$, small amount of amorphous phase and slow grain growth during annealing were observed. Shear stress-induced transformation was also observed in ground specimen. Cristobalite having a composition of CaO.2Al2O3.80SiO2 showed a more sensitive response to shear stress than the CaO.$2Al_2O_3$.40SiO$_2$ type cristobalite. Shear-induced transformation resulted in an increase of volume about 13% in $\alpha$-cristobalite phase on annealing for above 10 h in the case of the former composition.

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A preparation of hexacelsian powder by solution-polymerization route and its phase transformation behavior (Solution- polymerization 방법에 의한 hexacelsian 분말의 합성 및 상전이 공정에 의한 celsian 소결체의 제조)

  • Sang-Jin Lee;Young-Soo Yoon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.428-436
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    • 1997
  • Hexacelsian ($BaO{\cdot}Al_2O_3{\cdot}2SiO_2$) powder was prepared by a solution-polymerization route employing PVA solution as a polymeric carrier. A fine amorphous-type hexacelsian powder with an average particle size of 0.8 $\mu \textrm{m}$ and a BET specific surface area of $63 \textrm{m}^2$/g was made by a ball-milling the powder precursor for 12 h after calcination at $800^{\circ}C$ for :1 h. A densified hexacelsian was obtained through sintering at $1550^{\circ}C$ for 2 h under an air atmosphere. The $\alpha\longleftrightarrow\beta$ and $\beta\longleftrightarrow\gamma$ displacive phase transformation in polycrystalline hexacelsia,n was examined by using dilatometry and differential scanning calorimtry. The reconstructive transformation between hexacelsian and celsian was obtained by annealing at $1600^{\circ}C$ for 72h. Volume contraction of 5.6% was accompanied by the reconstructive transformation.

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A Synthesis of Mullite-Cordierite Composite Powders by Solution-Polymerization Route Based on Polyvinyl Alcohol (PVA를 이용한 Solution-Polymerization 합성법에 의한 Mullite-Cordierite 복합분말의 합성)

  • Lee, Yong-Seok;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.41 no.9
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    • pp.663-669
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    • 2004
  • Mullite and cordierite, which were stable oxides having excellent thermal and chemical characteristics, were widely used as an engineering and electronic materials. However, thermal shock resistance of the mullite was detriorated, and strength of the cordierite was also reduced at high temperatures. The mullite-cordierite composite powders were synthesized for solving these problems in this study. The mullite-cordierite composite powders were manufactured by the solution-polymerization method using mixtures of fused silica, aluminium nitrate, magnesium nitrate, and PVA. Crystallinity, phase formation, density, and surface area of the synthesis powders were characteristics. Fine mullite-cordlerite composite powders were successfully synthesized at 1300$^{\circ}C$ and their surface areas were about 20㎡/g after planetary milling for 1h. With increasing the milling time, surface area increased to 23 ㎡/g for 4h ana 24㎡/g for 8h.

Effect of PVA Polymerization on Synthesis of YAG:Ce3+ Phosphor Powders Prepared by a Solid-liquid Hybrid Route (PVA 중합도가 고상-액상 혼합 방식에 의한 YAG:Ce3+ 형광체 분말 합성에 미치는 영향)

  • Kim, A-Reum;Lee, Sang-Jin
    • Journal of the Korean Ceramic Society
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    • v.51 no.5
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    • pp.424-429
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    • 2014
  • YAG:$Ce^{3+}$ phosphor powders were synthesized using $Al(OH)_3$ seeds by means of a PVA-polymer-solution route. Various types of PVA with different molecular weights (different polymerization) were used. All dried precursor gels were calcined at $500^{\circ}C$ and then heated at $1500^{\circ}C$ in a mix of nitrogen and hydrogen gases. The final powders were characterized via XRD, SEM, PSA, PL, and PKG analyses. The phosphor properties and morphologies of the synthesized powders were dependent on the PVA type. As the molecular weight of the PVA was increased, the particle size gradually decreased with agglomeration, and the luminous intensity of the phosphor increased. However, the phosphor powder prepared from the PVA exhibiting very high molecular weight, showed a 531 nm (blue) shift from the 541 nm (yellow) wavelength of the YAG:$Ce^{3+}$ phosphor. Finally, the synthesized YAG:$Ce^{3+}$ phosphor powder prepared from the PVA with 89,000 - 98,000 molecular weight showed phosphor properties similar to those of a commercial phosphor powder, but without a post-treatment process.

Characteristic of Sintering of Mullite-Cordierite Composite by a Solution-Polymerization Route Employing PVA (PVA를 이용한 Solution-Polymerization 합성법에 의하여 제조된 Mullite-Cordierite 복합체의 소결특성)

  • Lee, Yong-Seok;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.42 no.3 s.274
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    • pp.155-164
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    • 2005
  • The characteristics of sintering for Mullite-Cordierite (MC) composites and the effect of $TiO_2$ addition were studied. The MC composites were manufactured by a solution-polymerization method using PVA as a polymer carrier, and $TiO_2$ was used as a sintering agent. They were calcined at $1300^{\circ}C$, planetary milled for 4 h and sintered at $1450^{\circ}C$. As cordierite content increased, relative density of materials was increased up to $98\%$ and sinterability was improved. In case of $50\;wt\%$ mullite/$5\;wt\%$ cordierite composition sintered for 16 h, the flexural strength and thermal expansion coefficient were 190 MPa and $3.07{\times}0^{-6}/^{\circ}C$, respectively. However, mechanical properties were decreased with the cordierite contents higher than $50\;wt\%$ because of the excess liquid-phase amount. As the addition of $TiO_2$ is increased, columnar crystal of mullite and liquid-phase contents were increased. In particular, the flexural strength and thermal expansion coefficient decreased in case of $5\;wt\%\;TiO_2$ addition.

A Novel Synthetic Route to Highly Cross-Linked Poly(alkylvinylether)s. Synthesis and Free Radical Polymerization of a Vinyl Ether Monomer Containing Electron Acceptors in Side Chain

  • 이주연;이현주;김무용
    • Bulletin of the Korean Chemical Society
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    • v.17 no.3
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    • pp.257-262
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    • 1996
  • p-(2-Vinyloxyethoxy)benzylidenemalononitrile 2 and methyl p-(2-vinyloxyethoxy)benzylidenecyanoacetate 3 was prepared by the condensation of p-(2-vinyloxyethoxy)benzaldehyde 1 with malononitrile or methyl cyanoacetate, respectively. Vinyl ether monomers 2 and 3 polymerized quantitatively with radical initiators in γ-butyrolactone solution at 65 ℃. The trisubstituted terminal double bond participated in the vinyl polymerization and radical polymerization of 2 and 3 led to swelling polymers 4 and 5 that were not soluble in common solvents due to cross-linking. Under the same polymerization conditions ethylvinyl ether polymerized well with model compounds of p-methoxybenzylidenemalononitrile 6 and methyl p-methoxybenzylidenecyanoacetate 7, respectively, to give 1:1 alternating copolymers 8 and 9 in high yields. Polymers 4 and 5 showed a thermal stability up to 300 ℃ without any characteristic Tg peaks in DSC thermograms. Alternating copolymers 8 and 9 were soluble in common solvents such as acetone and DMSO, and the inherent viscosities of the polymers were in the range of 0.36-0.74 dL/g. Films cast from acetone solution were cloudy and tough and Tg values obtained from DSC thermograms were in the range of 59-60 ℃.

Synthesis and Photoactivity of SnO2 - Doped Anatase - Type TiO2 Powder Via Polymerization - Complex Route (고분자 첨가법에 의해 SnO2가 도핑된 TiO2 분말의 합성 및 광촉매 특성)

  • Jung, Miewon;Kwak, Yunjung
    • Applied Chemistry for Engineering
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    • v.17 no.5
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    • pp.561-564
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    • 2006
  • $SnO_{2}$-doped anatase type $TiO_{2}$ powder was prepared by the polymerization complex route from tin(IV) bis (acetylacetonate) dichloride, titanium diisopropoxide bis (acetylacetonate) and polyethylene glycol (PEG) as a complexing agent. The structural changes of reaction mixture were monitored by fourier transform infarared (FT-IR) spectroscopy. The microstructure and morphology of gel powder were studied by field-emission scanning electron microscopy (FE-SEM) and X-ray diffractometry (XRD). The photocatalytic activity of these powders with the anatase structure was investigated by using indigo carmine solution.

A Synthesis of Mullite and Cordierite Ceramics by Solution-Polymerzation Route Based on PVA (PVA를 이용한 Solution-Polymerzation 합성법에 의한 Mullite, Cordierite 세라믹스의 합성)

  • 이용석;이병하
    • Journal of the Korean Ceramic Society
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    • v.41 no.2
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    • pp.151-157
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    • 2004
  • Because of the excellent thermal and chemical properties of mullite and cordierite as the stable oxide ceramic materials, they were widely used from engineering materials to electronic materials. Notwithstanding of their high demands, mullite was synthesised because it is not existed in nature. It is also difficult to produce cordierite of fine powder with high purity due to the narrow range of synthetic temperature. Mullite was synthesised by solid state reaction. However, synthesized mullite has been inhomogeneous. Because of the facts, various synthetic methods have been studied so far including sol-gel method. The purpose of this study is to synthesis mullite and cordierite of fine powder with high purity at the lower temperature by solution-polymerization route using PVA as a polymer carrier, which is an economical method by using low cost materials. As a result, mullite and cordierite were produced with mono crystal phase at 1200$^{\circ}C$ and 1250$^{\circ}C$, respectively, and their surface area over 20 ㎡/g.

Synthesis and Characterization of Aliphatic Polyether Dendrons Based on Polystyrene Peripheries

  • Song, Jie;Kim, Hyun-Yu;Cho, Byoung-Ki
    • Bulletin of the Korean Chemical Society
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    • v.28 no.10
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    • pp.1771-1776
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    • 2007
  • The synthesis of well-defined dendrons based on aliphatic polyether dendritic cores and glassy polystyrene peripheries is described. The synthetic route involves a combination of living anionic polymerization and a stepwise convergent method consisting of iterative Williamson etherification and hydroboration/oxidation reactions. On the basis of molecular weight, as characterized by gel permeation chromatography (GPC), the first generation dendron (Generation-1) shows a random coil conformation like a linear polystyrene, while higher generations (Generation-2 and 3) reveal globular forms in solution.

Preparation of Ag/PVP Nanocomposites as a Solid Precursor for Silver Nanocolloids Solution

  • Hong, Hyun-Ki;Park, Chan-Kyo;Gong, Myoung-Seon
    • Bulletin of the Korean Chemical Society
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    • v.31 no.5
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    • pp.1252-1256
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    • 2010
  • A polyvinylpyrrolidone (PVP)/Ag nanocomposites was prepared by the simultaneous thermal reduction and radical polymerization route. The in situ synthesis of the Ag/PVP nanocomposites is based on the finding that the silver n-propylcarbamate (Ag-PCB) complex can be directly dissolved in the NVP monomer, and decomposed by only heat treatment in the range of 110 to $130^{\circ}C$ to form silver metal. Silver nanoparticles with a narrow size distribution (5 - 40 nm) were obtained, which were well dispersed in the PVP matrix. A successful synthesis of Ag/PVP nanocomposites then proceeded upon heat treatment as low as $110^{\circ}C$. Moreover, important advantages of the in situ synthesis of Ag/PVP composites include that no additives (e.g. solvent, surface-active agent, or reductant of metallic ions) are used, and that the stable silver nanocolloid solution can be directly prepared in high concentration simply by dissolving the Ag/PVP nanocomposites in water or organic solvent.