• 제목/요약/키워드: Small angle X-ray scattering

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Ceramide NP 를 함유한 PLO Gel 에서 형성되는 액정에 관한 연구 (A Study on the Liquid Crystal Formed in PLO Gel Containing Ceramide NP)

  • 허민근;윤경섭
    • 대한화장품학회지
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    • 제47권1호
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    • pp.85-92
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    • 2021
  • 각질층은 각질세포와 세포간지질로 형성되고, 세포간지질의 주성분으로 세라마이드가 있다. 세라마이드는 세포간지질이 라멜라 구조를 형성하는데 중요한 성분 중 하나지만 난용성 물질이기 때문에 피부로의 직접적인 적용은 적합하지 않다. 그래서 약물전달시스템 중 꾸준한 관심을 받는 pluronic lecithin organogel (PLO gel) 제형에 세라마이드를 적용하고자 하였다. 제형에 적합한 오일을 선택하였고, 세라마이드를 함유한 PLO gel을 제조하였다. 편광현미경을 이용하여 액정 형성과 변화를 관찰하였고, 제형의 점탄성 거동을 알아보기 위해 점탄성 분석을 진행하였다. 그리고 제형 내의 구조들을 확인하기 위해 small-angle X-ray scattering (SAXS) 및 wide-angle X-ray scattering (WAXS) 분석을 진행하였다. 결과, 세라마이드를 함유한 PLO gel에서의 세라마이드와 레시틴의 함량비에 따라 액정 형성 여부, 액정의 크기와 안정성에서 차이를 보였다. 또한 점탄성 분석 결과로 제형의 안정성을 알 수 있었고, SAXS/WAXS 분석을 통해 세라마이드를 함유하지 않은 PLO gel은 사방정계 배열의 헥사고날 구조, 세라마이드를 함유한 PLO gel은 사방정계 배열의 라멜라 구조를 갖는 것을 확인하였다.

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.

분무열분해공정에 의한 메조기공 알루미나 제조에 있어 Al 전구체 영향 (Effect of Al Precursor Type on Mesoporous Alumina Particles Prepared by Spray Pyrolysis)

  • 김주현;정경열;박균영
    • 한국분말재료학회지
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    • 제17권3호
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    • pp.209-215
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    • 2010
  • Mesoporous alumina particles were prepared by spray pyrolysis using cetyltrimethyl-ammonium bromide (CTAB) as a structure directing agent and the effect of Al precursor types on the texture properties was studied using $N_2$ adsorption isotherms, small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The surface area and the microstructure of alumina particles were significantly influenced by the Al precursor type. The largest BET surface area was obtained when Al chloride was used, whereas alumina particles prepared from Al acetate had the largest pore volume. According to small-angle X-ray scattering (SAXS) analysis, the alumina powders prepared using nitrate and acetate precursors had a clear single SAXS peak around $2{\theta}=1.0{\sim}1.5^{\circ}$, indicating that regular mesopores with sponge-like structure were produced. On the basis of TEM, SAXS, and $N_2$ isotherm results, the chloride precursor was most profitable to obtain the largest surface area ($265\;m^2/g$), whereas, the nitrate precursor is useful for the preparation of non-hollow mesoporous alumina with regular pore size, maintaining high surface area (${\sim}233\;m^2/g$).

Control of Mechanical Properties of Polyurethane Elastomers Synthesized with Aliphatic Diisocyanate Bearing a Symmetric Structure

  • Kojio, Ken;Nozaki, Shuhei;Takahara, Atsushi;Yamasaki, Satoshi
    • Elastomers and Composites
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    • 제54권4호
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    • pp.271-278
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    • 2019
  • Polyurethane elastomers (PUEs) were synthesized using trans-1,4-bis(isocyanatomethyl) cyclohexane (1,4-H6XDI), poly(oxytetramethylene) glycol, 1,4-butanediol (BD), and 1,1,1-trimethylol propane (TMP). To control the molecular aggregation state and mechanical properties of these PUEs, hard segment contents of 20 and 30 wt% and BD/TMP ratios of 10/0 and 8/2 were chosen. Differential scanning calorimetry and small-angle X-ray scattering measurements revealed that the degree of microphase separation increased with an increase in both hard segment content and BD ratio. The Young's modulus and strain at break of the 1,4-H6XDI-based PUE were 6-20 MPa and 5-15, respectively. Incorporation of 20% TMP as a cross-linking agent into BD increased the melting temperature of the hard segment chains, that is, heat resistance, and decreased the Young's modulus. This could be due to the low density of the physical cross-linking network and the dispersion of hard segment chains in the soft segment matrix in the PUE in the presence of 20% TMP.

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.

Sulfonated Polystyrene Ionomers Containing 4-Aminobenzoic Acid Studied by a Small-Angle X-Ray Scattering Technique

  • Song, Ju-Myung;Hong, Min-Chul;Kim, Joon-Seop;Jikang Yoo;Yu, Jeong-A;Kim, Whangi
    • Macromolecular Research
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    • 제10권6호
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    • pp.304-310
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    • 2002
  • In a recent study by the same authors using a DMTA (Dynamic Mechanical Thermal Analyzer), it was found that the 4-aminobenzoic arid (ABA) molecules acted as either a neutralizing agent, or a plasticizer, or a filler, depending on the order of mixing of poly(styrene-co-styrenesulfonic acid) (PSSA), ABA, and NaOH. Subsequent to that study, we here pursued the same topic, i.e., the effect of the addition of CsOH (instead of NaOH) and ABA on the morphology of PSSA, but this time, by using a small-angle X-ray scattering (SAXS) technique. In line with the previous results, the present study with the SAXS technique verified that the order of mixing has a significant effect on the morphology of ionomers. In addition, with the SAXS data and the density values of the ionomers, we attempted to calculate both the number of sulfonate ionic groups per multiplet and the size of the multiplet of the ionomer.

Lecithin/LiCl 유기젤의 펜탄올 영향에 대한 유변학적 연구 (Effects of Pentanol on the Rheology of Lecithin/LiCl Oranogel)

  • 김민국;추은애;이희영
    • 공업화학
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    • 제32권6호
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    • pp.679-683
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    • 2021
  • 양친매성 인지질의 한 종류인 레시틴은 데케인과 같은 비극성 유기용매상에서 구형의 역마이셀을 형성한다. 염화리튬과 같은 이온이 레시틴용액에 첨가될 때, 유기졸이 역실린더형 마이셀의 얽힘으로 인해 유기젤로 변환하게 된다. 이번 연구에서, 우리는 레시틴과 염화리튬 혼합물의 유변학적 성질에 대한 보조계면활성제로서의 펜탄올 효과를 연구하고자 한다. 유변학 연구를 통해, 유기젤에 펜탄올이 첨가될 때, 유기젤의 점도와 탄성 성질이 감소하였다. 이러한 감소는 역실린더 마이셀의 길이의 감소가 그 원인이며, 엑스선 소각 산란분석기를 통해 이를 확인하였다.

Synthesis and Characterization of Nanocomposite Films Consisting of Vanadium Oxide and Microphase-separated Graft Copolymer

  • Choi, Jin-Kyu;Kim, Yong-Woo;Koh, Joo-Hwan;Kim, Jong-Hak;Mayes, Anne M.
    • Macromolecular Research
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    • 제15권6호
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    • pp.553-559
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    • 2007
  • Nanocomposite films were prepared by sol-gel synthesis from vanadium triisopropoxide with $poly((oxyethylene)_9$ methacrylate)-graft-poly(dimethyl siloxane), POEM-g-PDMS, producing in situ growth of vanadium oxide within the continuous ion-conducting POEM domains of micro phase-separated graft copolymer. The formation of vanadium oxide was confirmed by wide angle x-ray scattering (WAXS) and Fourier transform infrared (FT-IR) spectroscopy. Small angle x-ray scattering (SAXS) revealed the spatially-selective incorporation of vanadium oxide in the POEM domains. Upon the incorporation of vanadium oxide, the domain periodicity of the graft copolymer monotonously increased from 17.2 to 21.0 nm at a vanadium content 14 v%, above which it remained almost invariant. The selective interaction of vanadium oxide with POEM was further verified by differential scanning calorimetry (DSC) and FT-IR spectroscopy. The nanocomposite films exhibited excellent mechanical properties $(l0^{-5}-10^{-7}dyne/cm^2)$, mostly due to the confinement of vanadium oxide in the POEM chains as well as the interfaces created by the microphase separation of the graft copolymer.