• 제목/요약/키워드: Crystallization Kinetics

검색결과 73건 처리시간 0.037초

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

  • 윤경화;신동엽;김연철
    • 폴리머
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    • 제36권2호
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    • pp.245-250
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    • 2012
  • 장쇄분지(long chain branch, LCB)를 가지는 분지화된 폴리프로필렌(polypropylene, PP)이 세 종류의 분지제(branching agent)를 이용하여 고상(solid state)에서 제조하였다. 분지화된 PP의 화학구조, 비등온결정화 거동 및 복합점도를 적외선분광기(FTIR), 시차주사열용량분석기(DSC), 광학현미경 그리고 동적유변측정기(ARES)를 이용하여 관찰하였다. 분지화된 PP의 화학구조는 3100 $cm^{-1}$에서 나타나는 분지제의 =C-H 신축진동을 이용하여 확인하였다. PP-D-0-3과 PP-F-0-3의 경우 순수 PP와 비교하여 용융온도에 큰 변화를 보이지 않은 반면 HQ를 사용한 경우에는 용융온도의 감소를 나타내었다. 이는 분지화 반응보다 분해반응이 우세하여 나타나는 현상으로 해석되고, 복합점도의 감소를 통해 확인하였다. 분지화된 PP의 비등온결정화 거동은 Avrami 방정식을 이용하여 분석하였다. PP의 Avrami 지수는 3의 값을 나타내었고, DVB와 FS로 처리된 분지화 PP의 경우는 3보다 약간 작은 값을 나타내었다. Kissinger 방법에 의해서 계산된 분지화 PP의 활성화에너지는 순수 PP의 25 kJ/mol과 큰 차이를 보이지 않았다.

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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    • 제30권12호
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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.

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

  • 안성준;안승준
    • 한국산학기술학회논문지
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    • 제9권1호
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    • pp.47-52
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    • 2008
  • 소자가 점점 고집적화 됨에 따라, MOS 소자 제조에 있어서 $SiO_2$의 두께가 ${\sim}1nm$로 낮아질 경우 발생하는 터널링전류와 문틱전압 천이를 방지할 수 있는 새로운 게이트용 유전물질을 개발하여 소자의 크기를 줄이는데 주력하고 있다. 본 실험에서는 원자층증착(ALD: atomic layer deposition) 방법으로 증착된 $ZrO_2$ 박막의 물리적, 전기적 특성에 대하여 연구하였다. ALD $ZrO_2$ 박막을 증착한 후 Ar 가스 분위기에서 $800^{\circ}C$, 1 시간동안 열처리한 다음 XRD, TEM, 그리고 C-V plots을 이용하여 $Pt/ZrO_2/Si$ 소자의 형태, 결정화 동역학, 그리고 경계층 특성을 평가한 결과 열처리에 의해 소자의 특성이 크게 향상됨을 알 수 있었다.

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

  • 최재곤;방문수;한철
    • 공업화학
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    • 제8권1호
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    • pp.76-83
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    • 1997
  • 열방성 액정고분자(TLCP)와 폴리(에틸렌 테레프탈레이트)를 혼합용매 중에서 블렌딩하였으며, 이들 블렌드는 capillary rheometer die를 통하여 $287^{\circ}C$에서 섬유상 압출물로 가공되었다. 블렌드와 제조된 복합재료의 열적 성질, 기계적 성질, 모폴로지는 DSC, 편광현미경, SEM 및 인장시험에 의하여 조사되었다. 블렌드의 결정화 동력학은 등온 DSC 방법에 의하여 측정된 데이타로부터 Avrami식을 이용하여 결정화 속도 및 결정성장 메카니즘에 대한 정보를 얻었다. 블렌드내의 액정상은 가공온도조건하에서 거대상분킥나 열분해현상을 보이지 않았으며, 액체질소 속에서 절단된 섬유 단면의 SEM 관찰에 의하면, 섬유내 TLCP domain은 $0.1{\mu}m$에서 $0.2{\mu}m$정도의 크기로 분산되었고, 두 상 계면에서의 접착은 잘 되어있음을 알 수 있었다. TLCP/PET in-situ 섬유상 복합재료의 인장강도와 모듈러스는 TLCP 함량이 많을수록, draw ratio가 높을수록 증가됨을 알 수 있었다.

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

  • 홍성민;이필홍;고경현;안재환;이순일
    • 한국재료학회지
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    • 제8권3호
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    • pp.224-228
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    • 1998
  • 비정량적 조성을 가진 비정질 산화타이타늄 박막을 반응성 스퍼터링으로 제조한후, $500^{\circ}C$~$600^{\circ}C$에서 10분-3시간 열처리후 냉각속도를 달리하였을 때의 상변태과정을 고찰하였다. 10분-30분정도의 단기간의 열처리후 급냉한 경우에는 Mageneli상이 관찰되어 비정상정 상($TiO_{2-x}$)이 산화되는 속도가 결정화속도보다 훨씬 느린 것으로 생각되었다. 그러나 열처리 유지시간이 증가하면 $500^{\circ}C$에서 부터의 느린 냉각과정에서는 Magneil가 anatase로 변화하며 변태한 anatase는 저온에서는 rutile로 변화하지 않았으나 $500^{\circ}C$~$300{\circ}C$의 온도 구간을 비교적 빠르게 냉각하면 Matneli상은 직접 rutile상으로 변화할 수 있는 것으로 고찰되었다. 또한 $600^{\circ}C$에서 냉각시에도 rutile상이 형성됨으로서 rutile상은 $500^{\circ}C$이상의 고온에서도 이 상ㅇ르 거치지 않고 변태할 수 있는 것으로 분석된다. 결정화 및 산화과정은 부피의 변화를 야기하여 박막의 표면 형상의 변화도 가져옴이 관찰되었다.

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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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    • 제4권4호
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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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    • 정보저장시스템학회 2005년도 추계학술대회 논문집
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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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Pd 코팅된 Zr기 비정질 합금의 수소취성 및 표면특성 (Hydrogen Embrittlement and Surface Properties of Pd-coated Zr-based Amorphous Alloys)

  • 석송;이덕영;김기배
    • 한국수소및신에너지학회논문집
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    • 제18권2호
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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
    • 한국분말재료학회지
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    • 제21권4호
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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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    • 제3권3호
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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.