• Title/Summary/Keyword: crystallization kinetics

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Study on the Non-isothermal Crystallization Kinetics of Branched Polypropylene (분지형 폴리프로필렌의 비등온결정화 거동 연구)

  • Yoon, Kyung-Hwa;Shin, Dong-Yup;Kim, Youn-Cheol
    • Polymer(Korea)
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    • v.36 no.2
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    • pp.245-250
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    • 2012
  • Branched polypropylenes (PP) with long chain branch were prepared by solid state reaction with three different branching agent of 0.3 wt% content. The chemical structures, non-isothermal crystallization behavior and complex viscosity of the branched PP were investigated by FTIR, DSC, optical microscope, and dynamic rheological measurement. The chemical structure of the branched PP was confirmed by the existence of =C-H stretching peak of the branching agent at 3100 $cm^{-1}$. There was no distinct change in melting temperature in case of PP-D-0-3 and PP-F-0-3, but PP-H-0-3 indicated a decrease in melting temperature. The decrease in melting temperature was interpreted by the fact that the degradation reaction of PP was more dominant than branched reaction, and confirmed by a decrease in complex viscosity. The non-isothermal crystallization behavior of the branched PP was analyzed using by Avrami equation. The Avrami exponent of PP was 3, and the values of the branched PP with DVB and FS were below 3. The activation energy of PP calculated by Kissinger method was 25 kJ/mol, and there were no big difference in activation energies of the branched PPs compared to PP.

Formation of Layered Bi5Ti3FeO15 Perovskite in Bi2O3-TiO2-Fe2O3 Containing System

  • Borse, Pramod H.;Yoon, Sang-Su;Jang, Jum-Suk;Lee, Jae-Sung;Hong, Tae-Eun;Jeong, Euh-Duck;Won, Mi-Sook;Jung, Ok-Sang;Shim, Yoon-Bo;Kim, Hyun-Gyu
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.3011-3015
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    • 2009
  • Structural and thermo-analytical studies were carried out to understand the phase formation kinetics of the single phase $Bi_5Ti_3FeO_{15}$ (BTFO) nanocrystals in $Bi_2O_3-Fe_2O_3-TiO_2$, during the polymerized complex (PC) synthesis method. The crystallization of Aurivillius phase $Bi_5Ti_3FeO_{15}$ layered perovskite was found to be initiated and achieved under the temperature conditions in the range of ${\sim}$800 to 1050$^{\circ}C$. The activation energy for grain growth of $Bi_5Ti_3FeO_{15}$ nanocrystals (NCs) was very low in case of NCs formed by PC (2.61 kJ/mol) than that formed by the solid state reaction (SSR) method (10.9 kJ/mol). The energy involved in the phase transformation of Aurivillius phase $Bi_5Ti_3FeO_{15}$ from $Bi_2O_3-Fe_2O_3-TiO_2$ system was ${\sim}$ 69.8 kJ/mol. The formation kinetics study of $Bi_5Ti_3FeO_{15}$ synthesized by SSR and PC methods would not only render a large impact in the nanocrystalline material development but also in achieving highly efficient visible photocatalysts.

Study on the characteristics of ALD, ZrO2 thin film for next-generation high-density MOS devices (차세대 고집적 MOS 소자를 위한 ALD ZrO2 박막의 특성 연구)

  • Ahn, Seong-Joon;Ahn, Seung-Joon
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.9 no.1
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    • pp.47-52
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    • 2008
  • As the packing density of IC devices gets ever higher, the thickness of the gate $SiO_2$ layer of the MOS devices is now required to be reduced down to 1 nm. For such a thin $SiO_2$ layer, the MOS device cannot operate properly because of tunneling current and threshold voltage shift. Hence there has been much effort to develop new dielectric materials which have higher dielectric constants than $SiO_2$ and is free from such undesirable effects. In this work, the physical and electrical characteristics of ALD $ZrO_2$ film have been studied. After deposition of a thin ALD $ZrO_2$ film, it went through thermal treatment in the presence of argon gas at $800^{\circ}C$ for 1 hr. The characteristics of morphology, crystallization kinetics, and interfacial layer of $Pt/ZrO_2/Si$ samples have been investigated by using the analyzing instruments like XRD, TEM and C-V plots. It has been found that the characteristics of the $Pt/ZrO_2/Si$ device was enhanced by the thermal treatment.

On the Composites of Poly(ethylene terephthalate) with a Liquid Crystalline Polyester (액정 폴리에스테르와 폴리(에틸렌 테레프탈레이트)의 복합재료 연구)

  • Choi, Jae-Kon;Bang, Moon-Soo;Han, Chul
    • Applied Chemistry for Engineering
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    • v.8 no.1
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    • pp.76-83
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    • 1997
  • Blends of thermotropic liquid crystalline polymer(TLCP) with poly(ethylene terephthalate) (PET) were prepared by the coprecipitation from a common solvent. The blends were processed through a capillary die at $287^{\circ}C$ to produce a monofilament. Morphology and mechanical, thermal properties of blends and composites were examined by differential scanning calorimetry(DSC), tensile test, optical microscopy and scanning electron microscopy. Crystallization kinetics of the blends were investigated by the isothermal DSC method. The Avrami analyses were applied to obtain the information on the crystal growth geometry and factors controlling the rate of crystallization. In the blends, liquid crystalline phase did not reveal any significant macrophase separation and thermal degradation at the processing temperature. From scanning electron micrographs of cryogenic fracture surfaces of extruded fibers, the TLCP domains were found to be more or less finely dispersed with $0.1{\mu}m$ to $0.2{\mu}m$ in size. Interfacial adhesion between the TLCP and matrix polymer was excellent. Tensile strength and modulus of TLCP/PET in-situ fiber composites were enhanced with increasing draw ratio and LCP content.

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Phase Transitions In Nonstoichiometric Titanium Oxide Thin Films (비정량적 산화티타늄 박막의 상변태 특성)

  • Hong, Seong-Min;Lee, Pil-Hong;Go, Gyeong-Hyeon;An, Jae-Hwan;Lee, Sun-Il
    • Korean Journal of Materials Research
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    • v.8 no.3
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    • pp.224-228
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    • 1998
  • Phase transition kinetics of nonstoichiometric amorphous titanium oxide thin films deposited by reactive sputtering was investigated after cooling down with various rate followed by l0min.-3hrs. annealing at $500^{\circ}C$~$600^{\circ}C$ After short duration and fast cooling. Magneli was the only crystalline phase because the oxidation rates of $TiO_{2-x}$, could be relatively slower than that of crystallization. When the films were cooled slowly between $500^{\circ}C$~$300{\circ}C$, Magneli was transformed into an anatase and stabilized, but directly into a rutile under fast cooling. Because the rutile also prevailed after cooling from $600^{\circ}C$, it was concluded that the rutile phase could be formed directly from Magneli as well as converted from the anatase. Changes in volume and surface morphology were observed related to crystallization and oxidation processduring heat treatment.

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Spinodal Phase Separation and Isothermal Crystallization Behavior in Blends of VDF/TrFE(75/25) Copolymer and Poly(1,4-butylene adipate) (I) -Spinodal Phase Separation Behavior-

  • Kim, Kap Jin;Kyu, Thein
    • Fibers and Polymers
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    • v.4 no.4
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    • pp.188-194
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    • 2003
  • Phase behavior and spinodal phase separation kinetics in binary blends of a random copolymer of vinylidene fluoride and trifluoroethylene (75/25) [P(VDF/TrFE)] and poly(l,4-butylene adipate) (PBA) have been investigated by means of optical microscopic observation and time-resolved light scattering. The blends exhibited a typical lower critical solution temperature (LCST)∼${34}^{\circ}C$ above the melting temperature of the P(VDF/TrFE) crystals over the entire blend composition range. P(VDF/TrFE) and PBA were totally miscible in the temperature gap between the melting point of P(VDF/TrFE) and the LCST. Temperature jump experiments of the 3/7 P(VDF/TrFE)/PBA blend were carried out on a light-scattering apparatus from a single-phase melt state (${180}^{\circ}C$) to a two-phase region (205∼${215}^{\circ}C$). Since the late stage of spinodal decomposition (SD) is prevalent in the 3/7 blend, SD was analyzed using a power law scheme. Self-similarity was preserved well in the late stage of SD in the 3/7 blend.

Phase Transition Characteristics in $Ge_xSb_{100-x}$ Film for Optical Storage Media

  • Park Tae-jin;Kang Myung-jin;Choi Se-young
    • 정보저장시스템학회:학술대회논문집
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    • 2005.10a
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    • pp.124-127
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    • 2005
  • Rewritable optical memory devices such as an CD-RW and DVD+RW are data storage media, which take advantage of the different optical properties in the amorphous and crystalline states of phase change materials. The switching property, structural transformation, transformation kinetics and chemical bindings of $Ge_xSb_{100-x}$($6{\le}x{\le}$34) were studied to investigate the feasibility of applying $Ge_xSb_{100-x}$ alloys in optical memory. The $Ge_xSb_{100-x}$ thin film was deposited by RF magnetron co-sputtering system and phase change characteristics were investigated by X-ray diffraction (XRD), static tester, inductively coupled plasma atomic emission spectrometer (ICP-AES) and atomic force microscopy (AEM). Optimum fiim composition of $Ge_xSb_{100-x}$ was studied and its minimum time fur laser induced crystallization and optical contrast fur phase transition was performed. These results might be correlated with the binding energies between Ge and Sb, and indicate that $Ge_xSb_{100-x}$ have an potential far optical memory applications.

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Hydrogen Embrittlement and Surface Properties of Pd-coated Zr-based Amorphous Alloys (Pd 코팅된 Zr기 비정질 합금의 수소취성 및 표면특성)

  • Seok, Song;Lee, Dock-Young;Kim, Ki-Bae
    • Transactions of the Korean hydrogen and new energy society
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    • v.18 no.2
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    • pp.182-188
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    • 2007
  • [ $Zr_{50}-Ni_{27}-Nb_{18}-Co_5$ ] amorphous alloys ribbon was prepared by a single-roller melt-spinning technique. In order to improve the hydrogen kinetics Pd-coating were carried out on each side of the amorphous ribbon. Pd prevents oxidation of Zr and catalyses the dissociation of molecular hydrogen to atomic hydrogen. In this work, the hydrogen embrittlement and surface properties on Zr-based amorphous alloys were investigated. The Zr-based amorphous alloys were characterized by X-ray diffractometry(XRD) and differential scanning calorimetry(DSC). The morphology of surface and roughness was observed by using scanning electron microscopy(SEM) and atomic force microscopy (AFM). A lattice parameter of both Pd and Zr-based amorphous alloy was increased after hydrogen permeation at 473 K. After hydrogen permeation at 473 K, some cracks were observed on the surface of Pd, which was the cause for the hydrogen embrittlement. The crystallization temperature of Zr-based amorphous alloy was decreased due to the permeated hydrogen.

Production of Porous Metallic Glass Granule by Optimizing Chemical Processing

  • Kim, Song-Yi;Guem, Bo-Kyung;Lee, Min-Ha;Kim, Taek-Soo;Eckert, Jurgen;Kim, Bum-Sung
    • Journal of Powder Materials
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    • v.21 no.4
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    • pp.251-255
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    • 2014
  • In this study, we optimized dissolution the dissolution conditions of porous amorphous powder to have high specific surface area. Porous metallic glass(MG) granules were fabricated by selective phase dissolution, in which brass is removed from a composite powder consisting of MG and 40 vol.% brass. Dissolution was achieved through various concentrations of $H_2SO_4$ and $HNO_3$, with $HNO_3$ proving to have the faster reaction kinetics. Porous powders were analyzed by differential scanning calorimetry to observe crystallization behavior. The Microstructure of milled powder and dissolved powder was analyzed by scanning electron microscope. To check for residual in the dissolved powder after dissolution, energy dispersive X-ray spectroscory and elemental mapping was conducted. It was confirmed that the MG/brass composite powder dissolved in 10% $HNO_3$ produced a porous MG granule with a relatively high specific surface area of $19.60m^2/g$. This proved to be the optimum dissolution condition in which both a porous internal granule structure and amorphous phase were maintained. Consequently, porous MG granules were effectively fabricated and applications of such structures can be expanded.

Material Properties of Ni-P-B Electrodeposits for Steam Generator Tube Repair

  • Kim, Dong Jin;Seo, Moo Hong;Kim, Joung Soo
    • Corrosion Science and Technology
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    • v.3 no.3
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    • pp.112-117
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    • 2004
  • This work investigated the material properties of Ni-P-B alloy electrodeposits obtained from a Ni sulfamate bath as a function of the contents of the P and B sources($H_3PO_3$ and dimethyl amine borane complex(DMAB), respectively) with/without additives. Chemical composition, residual stress, microstructure and micro hardness were investigated using ICP(inductively coupled plasma) mass spectrometer, flexible strip, XRD, TEM and micro Vickers hardness tester, respectively. From the results of the compositional analysis, it was observed that P and B are incorporated competitively during the electrodeposition and the sulfur from the additive is codeposited into the electrodeposit. The measured residual stress value increased in the order of Ni, Ni-P, Ni-B and Ni-P-B electrodeposits indicating that boron affects the residual tensile stress greater than phosphorus. As the contents of the alloying element sources of P and B increased, crystallinity and the grain size of the electrodeposit decreased. The effect of boron on crystallinity and grain size was also relatively larger than the phosphorus. It can be explained that the boron with a smaller atomic radius contributes to the increase of residual stress in the tensile direction and the larger restraining force against the grain growth more significantly than the phosphorus with a larger atomic radius. Introduction of an additive into the bath retarded crystallization and grain growth, which may be attributed to the change of the grain growth kinetics induced by the additive adsorbed on the substrate and electrodeposit surfaces during electrodeposition.