• Title/Summary/Keyword: Small angle X-ray scattering

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Ordering Kinetics of Triblock Copolymer/Low Molecular Weight Homopolymer Mixtures (삼중블록공중합체와 저분자량 단일중합체 혼합물의 미세상분리 동력학)

  • 차국헌
    • The Korean Journal of Rheology
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    • v.10 no.2
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    • pp.65-73
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    • 1998
  • 본연구에서는poystyrene-block-poly (ethlene-co-butylene)-block-polystyrene(SEBS) 삼중블록 공중합체와 저분자량 단일중합체인 Hercotac 1149 (H1149)의 70/30 (w/w) 혼합물 의 미세상분리와 그동력학을 유변물성 측정법과 SAXS 실험을 통하여 연구해 보았다. 먼저 혼합물의 미세상분리 온도를 유변물성 측정법과 SAXS 실험을 통해 각각구한 다음 샘플을 미세상분리 온도보다 높은 온도에서 그이하의 온도로 급냉시킨 후 유변물성과 산란강도의 사간에 따른 변화로부터 미세상분리 동력학에 대한 정보를 구하였다. 이렇게 얻어진 데이터 를 Avrami 형태의 핵생성 성장(NG) 메커니즘으로 해석해 보았는데 최대산란강도 Imax 뿐만 아니라 저장 점탄성계수 G'과 손실 점탄성계수 G"의 시간에 따른 변화를 잘 예측할수 있 었다. 한편 서로다른 두 time-resolved 실험으로부터 Avrami 플롯을 그려서 구해진 Avrami 변수들은 같은 급냉 깊이에서는 서로 잘 일치함을 확인하였다. 반감기는 급냉 깊이가 증가 함에 따라 점차 감소하는 경향을 보였는데 이는 급냉 깊이가 클수록 미세상분리가 더 빨리 진행되고 있음을 보여주는 것이다. 또한 Avrami 지수는 급냉 깊이가 증가함에 따라 3에서 4로 급격히 변했는데 이로부터 급냉 깊이가 작을 때에는 70/30 (w/w) SEBS/H1149 혼합물 의 미세상분리가 불균일 핵생성 성장 메커니즘에 따라 진행되고 급냉 깊이가 더 커지면 미 세상분리가 스피노달 상분리 메커니즘으로 변하고 있음을 예측할수 있었다.

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A novel ceramic GEM used for neutron detection

  • Zhou, Jianrong;Zhou, Xiaojuan;Zhou, Jianjin;Jiang, Xingfen;Yang, Jianqing;Zhu, Lin;Yang, Wenqin;Yang, Tao;Xu, Hong;Xia, Yuanguang;Yang, Gui-an;Xie, Yuguang;Huang, Chaoqiang;Hu, Bitao;Sun, Zhijia;Chen, Yuanbo
    • Nuclear Engineering and Technology
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    • v.52 no.6
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    • pp.1277-1281
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    • 2020
  • A novel ceramic Gas Electron Multiplier (GEM) has been developed to meet the demand of high counting rate for the neutron detection which is an alternative to 3He-based detector at China Spallation Neutron Source (CSNS). An experiment was performed to measure the neutron transmittance of ceramic-GEM and FR4-GEM at the small angle neutron scattering (SANS) instrument. The result showed the ceramic-GEM has higher transmittance and less self-scattering especially for cold neutrons. One single ceramic GEM could give a gain of 102-104 in the mixture gas of Ar and CO2 (90%:10%) and its energy resolution was about 27.7% by using 55Fe X ray of 5.9 keV. A prototype has been developed in order to investigate the performances of the ceramic GEM-based neutron detector. Several neutron beam tests, including detection efficiency, spatial resolution, two-dimensional imaging, and wavelength spectrum, were carried out at CSNS and China Mianyang Research Reactor (CMRR). The results show that the ceramic GEM-based neutron detector is a good candidate to measure the high intensity neutrons.

Preparation and Characterization of Nafion Composite Membranes Containing 1-ethyl-3-methylimidazolium Tetracyanoborate

  • Shin, Mun-Sik;Park, Jin-Soo
    • Journal of the Korean Electrochemical Society
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    • v.15 no.1
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    • pp.35-40
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    • 2012
  • The composite membranes using Nafion as matrix and 1-ethyl-3-methylimidazolium tetracyanoborate (EMITCB) as ion-conducting medium in replacement of water were prepared and characterized. The amount of EMITCB in Nafion varied from 30 to 50wt%. The composite membranes are characterized by ion conductivity, thermogravitational analyses (TGA) and small-angle X-ray scattering (SAXS). The composite membranes containing EMITCB of 40wt% showed the maximum ionic conductivity which was ~0.0146 S $cm^{-1}$ at 423.15 K. It is inferred that the decrease in ionic conductivity of all the composite membranes might be due to the decomposition of a tetracyanoboric acid formed in the composite membranes. The results of SAXS indicated that the ionic clusters to conduct proton in the composite membranes were successfully formed. In accordance with the results of ionic conductivity as a function of a reciprocal temperature, SAXS showed a proportional decrease in scattering maximum $q_{max}$ as the amount of EMITCB increases in the composite membranes, which results in the increase in ionomer cluster size. The TGA showed no significant decomposition of the ionic liquid as well as the composite membranes in the range of operating temperature ($120-150^{\circ}C$) of high temperature proton exchange membrane fuel cells (HTPEMFC). As a result, EMITCB is able to play an important role in transferring proton in the composite membranes at elevated temperatures with no external humidification for proton exchange membrane fuel cells.

Mn 도핑 농도에 따른 ZnO 나노 입자의 구조와 자성 특성 연구

  • Kim, Jeong-Hun;Kim, Seon-Ho;Jeon, Gwang-Deok;Lee, Ji-Eun;Lee, Hui-Su;Jeong, Jin-Cheol;Choe, Pu-Reum;Eo, Jin-Seok;Park, Jun-Ho;Lee, Ji-Un;Choe, Seung-Yeon;Choe, Gyu-Hyeon;Baek, Min;Yang, U-Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.604-604
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    • 2013
  • 차세대 반도체 분야인 스핀트로닉스 소자의 필수적인 물질인 강자성-반도체 하이브리드 물질인 Dilute magnetic semiconductor (DMS)에 관한 연구가 최근 많은 관심을 가지고 있다. 그중에서 넓은 에너지 밴드 갭 에너지(3.37 eV)를 가지고 있고 상온에서 엑시톤 결합 에너지가 ~60 mV로 광전자 소자, 전계 디스플레이 에 응용이 가능한 물질인 ZnO는 최근에 전이금속을 도핑하여 상온에서 강자성 특성을 나타내어 활발한 연구가 이루어지고 있다. 그러나, 이 물질에 대한 특성과 자성의 원인 규명에 관한 연구는 논란이 되고 있다. 본 연구에서는 Mn이 도핑된 ZnO 나노 입자를 만들고, Mn 물질의 도핑 농도에 따른 ZnO 나노 입자의 구조, 크기 및 자기 구조를 측정하여 구조와 자성의 상관관계에 관한 연구하였다. ZnxMn1-xO 나노 입자는 화학적 졸-겔(sol-gel) 방법을 이용하여 준비하였다. ZnxMn1-xO 나노 입자의 크기 및 격자 구조적 특징은 XRD (X-ray diffraction)와 TEM (Transmission Electron Microscope), SEM (Scanning Electron Microscope), SANS (Small Angle Neutron Scattering)를 이용하여 측정하였고 물질의 자기적 특징은 SQUID를 이용하여 조사하였다. Mn 도핑이 증가함에 따라 격자간격이 커지고 나노 입자의 크기는 감소하였으며, Zn와 Mn의 성장 시, 비율이 9:1의 경우에 상온에서 강자성 특성이 나타남을 보았다. 그 이상의 Mn 도핑 비율에서는 상자성 특성이 나타남을 보았다. 본 연구를 통하여 스핀트로닉스 소자 응용을 위한 ZnO 나노 입자에 최적의 Mn 도핑 농도를 제시하고 나노 입자의 자기 특성 형성의 원인 및 모델을 제시하였다.

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Crystallization Behavior of poly(trimethylene terephthalate) in a Confined Geometry (제한공간에서의 폴리(트리메틸렌 테레프탈레이트)의 결정화 거동)

  • 임정은;이종관;이광희
    • Polymer(Korea)
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    • v.27 no.4
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    • pp.293-298
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    • 2003
  • The development of the crystalline structure of poly(trimethylene terephthalate) (PTT) in a confined geometry was investigated with optical microscope, small angle light scattering, and X-ray diffraction. The rejected distance, which was represented in terms of the parameter $\delta$, played an important role in determining the morphological patterns of poly (ethylene terethphalate) (PET/PTT) blend. In case of stepwise crystallization, the crystallization of PTT commenced in the interspherulitic region between the grown PET crystals and proceeded until the interspherulitic space was filled with the PTT crystals. The spherulitic surface of the PET crtstals acted as the nucleation sites where the PTT molecules preferentially crystallized, leading to the formation of transcrystalline structure. As a result, a mixed morphological pattern was observed in the PTT-rich phase: one was a typical spherulitic texture and the other was a transcrystalline texture. Some of the molecular conformations of PTT, which could adopt in the absence of the space limitation, were probably forbidden in the interlamellar and/or interfibrillar regions of the PET spherulite. This constraint was responsible for difference in the crystallization and melting behavior of PTT between the intra and interspheulitic regions of PET.

Microstructure-Sound Absorption Relationships of Polyurethane Foam and Application of Low Monos Polyol (폴리우레탄 폼의 미세구조와 흡음 관계 밑 Low Monos 폴리올의 응용)

  • Lee, Boo-Youn;Kim, So-Yeon;Lee, Kwang-Hee;Jin, Byung-Suk
    • Polymer(Korea)
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    • v.31 no.4
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    • pp.289-296
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    • 2007
  • The material factors influencing the sound absorption of the polyurethane foam were investigated with FT-IR, small-angle X-ray scattering (SAXS), and dynamic mechanical thermal analyzer (DMTA). The measurements were performed using the samples which had a similar cell structure but different absorption coefficients. It was found that the ability of the sound absorption of the polyurethane foams was closely related to the damping behavior over the transition range. In order to confirm the use of the low monol polyol (LMP) in high-performance applications, the polyurethanes based on LMP and polypropylene oxide polyol (PPG) were prepared by the solution polymerization method. The microstructure and the physical properties of these polyurethanes were compared. The PPG-based polyurethane showed a higher level of the phase-separated structure because the considerable amount of monol presented in PPG made a contribution to the increased chain mobility. However the short chains formed due to the monol species deteriorated the damping property. As a result, the LMP-based polyurethane showed the superior damping behavior as compared with the PPG-based one.

Annealing of Co-Cr dental alloy: effects on nanostructure and Rockwell hardness

  • Ayyildiz, Simel;Soylu, Elif Hilal;ide, Semra;Kilic, Selim;Sipahi, Cumhur;Piskin, Bulent;Gokce, Hasan Suat
    • The Journal of Advanced Prosthodontics
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    • v.5 no.4
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    • pp.471-478
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    • 2013
  • PURPOSE. The aim of the study was to evaluate the effect of annealing on the nanostructure and hardness of Co-Cr metal ceramic samples that were fabricated with a direct metal laser sintering (DMLS) technique. MATERIALS AND METHODS. Five groups of Co-Cr dental alloy samples were manufactured in a rectangular form measuring $4{\times}2{\times}2$ mm. Samples fabricated by a conventional casting technique (Group I) and prefabricated milling blanks (Group II) were examined as conventional technique groups. The DMLS samples were randomly divided into three groups as not annealed (Group III), annealed in argon atmosphere (Group IV), or annealed in oxygen atmosphere (Group V). The nanostructure was examined with the small-angle X-ray scattering method. The Rockwell hardness test was used to measure the hardness changes in each group, and the means and standard deviations were statistically analyzed by one-way ANOVA for comparison of continuous variables and Tukey's HSD test was used for post hoc analysis. P values of <.05 were accepted as statistically significant. RESULTS. The general nanostructures of the samples were composed of small spherical entities stacked atop one another in dendritic form. All groups also displayed different hardness values depending on the manufacturing technique. The annealing procedure and environment directly affected both the nanostructure and hardness of the Co-Cr alloy. Group III exhibited a non-homogeneous structure and increased hardness ($48.16{\pm}3.02$ HRC) because the annealing process was incomplete and the inner stress was not relieved. Annealing in argon atmosphere of Group IV not only relieved the inner stresses but also decreased the hardness ($27.40{\pm}3.98$ HRC). The results of fitting function presented that Group IV was the most homogeneous product as the minimum bilayer thickness was measured (7.11 ${\AA}$). CONCLUSION. After the manufacturing with DMLS technique, annealing in argon atmosphere is an essential process for Co-Cr metal ceramic substructures. The dentists should be familiar with the materials that are used in clinic for prosthodontics treatments.

Development of Lamella Morphology in Poly(ethylene terephthalate)/Polycarbonate Blends

  • Lee, Jong-Kwan;Im, Jeong-Eon;Lee, Kwang-Hee
    • Macromolecular Research
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    • v.12 no.2
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    • pp.172-177
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    • 2004
  • We have studied the lamella-level morphology of poly(ethylene terephthalate) (PET)/polycarbonate (PC) blends using small-angle X-ray scattering (SAXS). Measurements were made as a function of the holding time in the melt. We determined the morphological parameters at the lamellar level by correlation function analysis of the SAXS data. An increased amorphous layer thickness was identified in the blend, indicating that some PC was incorporated into the interlamellar regions of PET during crystallization. The blend also exhibits a larger lamella crystalline thickness (l$\sub$c/) than that of pure PET. A possible reason for the increase in l$\sub$c/ is that the inclusion of the PC molecules in the interlamellar regions causes an increase in the surface free energy of folding. At the early stage of isothermal crystallization, we observed a rapid drop in the value of l$\sub$c/ in the blend; this finding indicates that a relatively large fraction of secondary crystals form during the primary crystallization. In contrast, the value of l$\sub$c/ for the sample that underwent a prolonged holding time increased with time in the secondary crystallization-dominant regime; this observation suggests that the disruption of chain periodicity, which results from transesterification between the two polymers, favors the development of fringed micellar crystals that have larger values of l$\sub$c/ rather than the development of normal chain-folded crystals.

Characteristics of composite membranes containing ionic liquid and acid for anhydrous high temperature PEFCs (무가습 고온 PEFC용 이온성 액체 및 산이 함유된 복합막의 특성)

  • Baek, Ji-Suk;Park, Jin-Soo;Park, Seung-Hee;Yang, Tae-Hyun;Park, Gu-Gon;Yim, Sung-Dae;Kim, Chang-Soo;Shul, Young-Gun
    • 한국신재생에너지학회:학술대회논문집
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    • 2009.06a
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    • pp.378-378
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    • 2009
  • The ionic liquid-based sulfonated hydrocarbon composite membranes was prepared for use in anhydrous high temperature-polymer electrolyte fuel cells (HT-PEFCs). Ionic liquid behaves like water in the composite membranes under anhydrous condition. However the composite membranes show a low conductivity and high gas permeability as the content of ionic liquid increases due to its high viscosity and content of ionic liquid, respectively. Hence, in order to enhance the proton conductivity and to reduce the gas permeability of the composite membranes with low content of ionic liquids, the acid containing a common ion of ionic liquid was added to the composite membranes. The characterization of composite membranes was carried out using small-angle X-ray scattering (SAXS), thermogravimetric analyzer (TGA) and impedance spectroscopy. As a result, the composite membranes containing acid showed higher proton conductivity than those with no acid under the un-humidified condition due to a decrease in viscosity. In addition, the proton conductivity of composite membranes increased with increasing mole concentration of acid.

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Synthesis of Mesoporous Silica Using Municipal Solid Waste Incinerator Ash Slag : Influence of NaOH Concentration (생활(生活) 폐기물(廢棄物) 소각재(燒却材) 슬래그를 이용(利用)한 메조포러스 실리카 합성(合成) : NaOH 농도(濃度)의 영향(影響))

  • Han, Yo-Sep;Jung, Jong-Hoon;Park, Jai-Koo
    • Resources Recycling
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    • v.19 no.1
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    • pp.40-48
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    • 2010
  • It was investigated that effects of NaOH concentration on synthesis of mesoporous materials using municipal solid waste incinerator ash slag (MSWI-ash slag). In order to increase the purity and maximize the amount of extracted Si content the raw MSWI-ash slag was mechanically activated. Extraction of Si from the MSWI-ash slag was carried out by alkali treatment using concentrated NaOH solution, which varied from 1M to 4M. Physical properties (i.e., pore size, specific surface area and total pore volume) of the synthesized mesoporous silica were also evaluated as a function of NaOH concentration via BET, SEM, TEM and small-angle X-ray scattering analyses. Over the entire range of NaOH concentration investigated (i.e., 1-4M), the synthesized mesoporous materials were determined to be SBA-15, which exhibited a hexagonal structure with the pore size of approximately 7 nm. On the other hand, specific surface area and total pore volume increased with NaOH concentration up to 3M while the values decreased at 4M, indicating that the optimal NaOH concentration for the synthesized mesoporous silica was approximately 3M. Further comparison analysis between two conditions (3M versus 4M) showed that the decrease in two physical properties at 4M NaOH concentration was likely due to the potential inhibition by excess Na ions on the formation of mesophase and the consequent increase of pore wall thickness by remaining Si ions.