• 제목/요약/키워드: SAXS

검색결과 79건 처리시간 0.03초

진동분광실험을 이용한 n-Paraffin혼합물의 결정화에 관한 연구 (Vibrational Spectroscopic Studies of Crystallization in Mixed n-Paraffins)

  • 김도균;임현주;최선남;김성수;송기국
    • 폴리머
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    • 제26권6호
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    • pp.752-758
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    • 2002
  • 사슬길이가 서로 다른 두 종류의 n-paraffin 혼합물이 결정을 형성할 때 사슬의 움직임과 형성된 라멜라의 구조를 조사하기 위하여 FTIR, FT-Raman, XRD 실험방법을 이용하였다. FTIR crystal field splitting, Raman longitudinal acoustic mode, 그리고 SAXS long period 측정 결과들을 비교하여 사슬길이가 다른 두 n-paraffin 사슬이 혼합되어 하나의 라멜라를 형성하거나 분리되어 각각의 라멜라를 형성하는 과정을 연구하였다.

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

  • Shin, Mun-Sik;Park, Jin-Soo
    • 전기화학회지
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    • 제15권1호
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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.

X선 산란분석법을 이용한 액정에멀젼 구조분석 (Structure Analysis of Liquid Crystal Emulsions Using X-ray Scattering Analysis)

  • 박소현;김수지;노민주;이준배;박수남
    • 대한화장품학회지
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    • 제42권3호
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    • pp.297-302
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    • 2016
  • 본 연구에서는 $C_{12-20}$ 알킬글루코사이드, $C_{14-22}$ 알코올 및 베헤닐알코올로 구성된 액정에멀젼을 제조하고 다양한 분석장비를 이용하여 구조분석을 실시하였다. 먼저 제조한 액정에멀젼을 편광현미경과 cryo-SEM을 이용하여 각각 액정에멀젼의 특징인 maltese cross 무늬와 다층 구조를 확인하였다. 또한, DSC를 이용하여 액정상 형성을 확인하였고, small angle x-ray scattering (SAXS) 분석을 통하여 약 $305{\AA}$의 층간 간격을 갖는 다층 라멜라 구조를 확인하였다. 한편, wide angle x-ray scattering (WAXS) 분석을 통해 제조된 액정에멀젼의 라멜라 구조를 이루고 있는 알킬 사슬 간 배열이 사방정계 구조로 되어 있음을 확인할 수 있었다. 액정에멀젼 구조 연구를 통해 얻어진 다양한 물성 정보는 향후 산업적으로 많이 이용될 것으로 기대된다.

분무열분해 공정을 이용한 메조기공을 가지는 실리카 구형입자의 제조 (Preparation of Mesoporous and Spherical-shaped Silica Particles by Spray Pyrolysis)

  • 백철민;정경열;박균영;박승빈;조성백
    • Korean Chemical Engineering Research
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    • 제46권5호
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    • pp.880-885
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    • 2008
  • 분무열분해 공정을 이용하여 규칙적인 메조기공을 가지는 실리카 분말을 제조하고 고표면적을 얻기 위한 합성조건을 최적화하였다. 주형제로 이용된 CTAB의 양과 액적들의 반응기 내에서 체류시간을 변화시켜주면서 입자를 제조하고 SEM, BET, SAXS, 그리고 DLS를 통해 분말특성을 조사하였다. 기체 유입속도를 고정하고 CTAB/TEOS 몰비를 0.05에서 0.30으로 변화시킴에 따라 비표면적은 200에서 $1,290m^2/g$으로 변화였다. CTAB/TEOS 몰비를 고정했을 때 입자의 비표면적은 기체의 유입속도에 따라 1,062에서 $1,305m^2/g$ 사이에서 변화되었다. 제조된 입자들의 BJH 탈착에 의한 평균 기공 크기는 $21{\sim}23{\AA}$를 가졌으며, CTAB/TEOS 몰비나 기체 유입속도에 크게 영향을 받지 않았다. 최대 표면적은 CTAB/TEOS 비를 0.2, 기체 유속을 20 l/min으로 했을 때 $1,305m^2/g$를 얻었다. 제조된 실리카 분말은 육방형구조의 규칙적인 기공에 기인한 $2{\theta}=2.6^{\circ}$ 강한 피크와 $2{\theta}=4.4$$5.1^{\circ}$ 약한 피크를 가지는 것을 SAXS 분석결과로 확인하였다. 제조된 실리카 분말은 구형의 형상을 가졌으며 $1.0{\mu}m$의 평균크기를 가졌다.

Olefin Separation Performances and Coordination Behaviors of Facilitated Transport Membranes Based on Poly(styrene-b-isoprene-b-styrene)/Silver Salt Complexes

  • Lee, Dong-Hoon;Kang, Yong-Soo;Kim, Jong-Hak
    • Macromolecular Research
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    • 제17권2호
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    • pp.104-109
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    • 2009
  • Solid-state facilitated, olefin transport membranes were prepared by complexation of poly(styrene-b-iso-prene-b-styrene) (SIS) block copolymer and silver salt. Facilitated olefin transport was not observed up to a silver mole fraction of 0.14, representing a threshold concentration, above which transport increased almost linearly with increasing silver salt concentration. This was because firstly the silver ions were selectively coordinated with the C=C bonds of PI blocks up to a silver mole fraction of 0.20, and secondly the coordinative interaction of the silver ions with the aliphatic C=C bond was stronger than that with the aromatic C=C bond, as confirmed by FT-Raman spectroscopy. Small angle X-ray scattering (SAXS) analysis showed that the cylindrical morphology of the neat SIS block copolymer was changed to a disordered structure at low silver concentrations ($0.01{\sim}0.02$). However, at intermediate silver concentrations ($0.15{\sim}0.20$), disordered-ordered structural changes occurred and finally returned to a disordered structure again at higher silver concentrations (>0.33). These results demonstrated that the facilitated olefin transport of SIS/silver salt complex membrancs was significantly affected by their coordinative interactions and nano-structural morphology.

Selective Coordination of Silver Ions to Poly(styrene-b-(ethylene-co-butylene)-b-styrene) and its Influence on Morphology and Facilitated Olefin Transport

  • Lee, Dong-Hoon;Kang, Yong-Soo;Kim, Jong-Hak;Kang, Sang-Wook
    • Macromolecular Research
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    • 제16권8호
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    • pp.676-681
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    • 2008
  • The $\pi$-complex membranes of poly(styrene-b-(ethylene-co-butylene)-b-styrene) (SEBS) of two silver salts of $AgBF_4$ and $AgCF_3SO_3$ were prepared and tested for the separation of the propylene/propane mixtures. The Fourier-transform infrared (FT-IR) spectra of these complexes showed that the silver salts were dissolved in SEBS up to a silver mole fraction of 0.14, due to $\pi$-complexation between the aromatic C=C bonds of styrene blocks and silver ions. Above this solubility limit, ion pairs and high-order ionic aggregates began to form, so that silver salts were distributed unselectively in both the EB and PS blocks. The domain size of the PS blocks was enlarged up to this critical concentration with increasing silver concentration without structural transitions, as confirmed by small angle x-ray scattering (SAXS). These structural properties of the SEBS/silver salt complexes may explain the lower separation properties for propylene/propane mixtures compared to poly(styrene-b-butadiene-b-styrene)(SBS)/silver salt complex membranes.

SAXS와 AFM에 의한 HF-용액내 양극 에칭에 의해 제조된 기공성 실리콘의 구조연구 (SAXS and AFM Study on Porous Silicon Prepared by Anodic Etching in HF-based Solution)

  • 김유진;김화중
    • 한국전기전자재료학회논문지
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    • 제17권11호
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    • pp.1218-1223
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    • 2004
  • Porous silicon materials have been shown to have bright prospects for applications in light emitting, solar cell, as well as light- and chemical-sensing devices. In this report, structures of porous silicon prepared by anodic etching in HF-based solution with various etching times were studied in detail by Atomic Force Microscopy and Small Angle X -ray Scattering technique using the high energy beam line at Pohang Light Source in Korea. The results showed the coexistence of the various pores with nanometer and submicrometer scales. For nanameter size pores, the mixed ones with two different shapes were identified: the larger ones in cylindrical shape and the smaller ones in spherical shape. Volume fractions of the cylindrical and the spherical pores were about equal and remained unchanged at all etching times investigated. On the whole uniform values of the specific surface area and of the size parameters of the pores were observed except for the larger specific surface area for the sample with the short etching time. The results implies that etching process causes the inner surfaces to become smoother while new pores are being generated. In all SAXS data at large Q vectors, Porod slope of -4 was observed, which supports the fact that the pores have smooth surfaces.

Phase Behavior of a PEO-PPO-PEO Triblock Copolymer in Aqueous Solutions: Two Gelation Mechanisms

  • Park, Moon-Jeong;Kookheon Char;Kim, Hong-Doo;Lee, Chang-Hee;Seong, Baek-Seok;Han, Young-Soo
    • Macromolecular Research
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    • 제10권6호
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    • pp.325-331
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    • 2002
  • Phase behavior of a PEO-PPO-PEO (Pluronic P103) triblock copolymer in water is investigated using small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and rheology. Pluronic P103 shows apparent two gel states in different temperature regions. The first sol-to-gel transition at a lower temperature (i.e., the hard gel I state) turns out to be the hexagonal microphase as evidenced by the combined SANS and SAXS and the frequency dependence of both G′ and G" in rheology. In contrast to the hard gel I, the second sol-to-gel transition (i. e., the hard gel II state) at a higher temperature represents the block copolymer micelles in somewhat disordered state rather than the ordered state seen in the hard gel I. Moreover, turbidity change depending only on the temperature with four distinct regions is observed and the large aggregates with size larger than 5,000 nm are detected with DLS in the turbid solution region. Based upon the present study, two different gelation mechanisms for aqueous PEO-PPO-PEO triblock copolymer solutions are proposed.