• 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.

• Macromolecular Research
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• 제14권1호
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• pp.45-51
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• 2006

We conducted simultaneous, small-angle, X-ray scattering/differential scanning calorimetry (SAXS/DSC) and simultaneous, wide-angle, X-ray scattering (WAXS)/DSC measurements for a polymer blend of poly($\varepsilon$-caprolactone)/poly(ethylene glycol)(PCL/PEG). The time-dependent SAXS/DSC and WAXS/DSC results, measured while the system was quenched below the melting temperature of PCL from a melting state, revealed the competitive behavior between liquid-liquid phase separation and crystallization in the polymer blend. The time-dependent structural evolution extracted from the SAXS/WAXS/DSC results can be characterized by the following four stages in the PCL crystallization process: the induction (I), nucleation (II), growth (III), and late (IV) stages. The influence of the liquid-liquid phase separation on the crystallization of PCL was also observed by phase-contrast microscope and polarized microscope with 1/4$\lambda$ compensator.

• 한국결정학회:학술대회논문집
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• 한국결정학회 2002년도 정기총회 및 추계학술연구발표회
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• pp.51-51
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• 2002

나노기공물질은 특정 기반물질(matrix) 내부에 대략 나노미터크기의 기공을 함유하고 있는 물질이며 나노기공물질의 특성은 기반물질의 특성과 더불어 기공의 형태, 크기, 분포에 의해서 결정된다. 나노기공물질의 기공에 대한 정보를 측정하는 방법으로는 TEM, 흡착법, FE-SEM과 더불어 중성자 또는 X-ray 빔의 산란을 이용하는 소각중성자산란 (Small-Angle Neutron Scatering, SANS), 소각 X-ray 산란 (Small-Angle X-ray Scattering, SAXS), 중성자반사율측정 (Neutron Relfectimetry, NR), X-ray 반사율측정 (X-Ray Reflectometry, XRR) 등이 사용되고 있다. 본 발표는 대략 1 nm - 100 nm 영역의 bulk 구조와 층상구조를 측정할 수 있는 소각 중성자 산란과 중성자 반사율 측정기법을 이용한 나노기공 측정기술을 다룬다.

• Bulletin of the Korean Chemical Society
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• 제24권10호
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• pp.1485-1489
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• 2003

The gelation for di-(2-ethylhexyl) phthalate (DEHP)-plasticized poly(vinyl chloride) was studied by measuring time-resolved small-angle X-ray scattering (SAXS) and a flow of the solutions in test tube. It was found that for the gelation there were three regimes. At Regime I, the solution rapidly changed to a gel, and the SAXS intensity showed a peak and the peak intensity increased, keeping the peak angle constant. Applying the SAXS intensity to the kinetic analysis of the liquid-liquid phase separation, it was revealed that the spinodal decomposition proceeded to develop a periodic length of 29.9 nanometer in size, a hydrogen-bonding-type association in polymer rich phase followed, and then it induced fast gelation rate. At Regime II, the gelation slowly occurred and the SAXS intensity was not observed, suggesting that a homogeneous gel network was formed by a hydrogen-bonding. At regime III, the solution was a homogeneous sol.

• Bulletin of the Korean Chemical Society
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• 제23권4호
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• pp.580-586
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• 2002

We investigated the effect of ionic component on crystalline morphology development during isothermal annealing in a sodium neutralized sulfonated poly(ethylene terephthalate) ionomer (Ion-PET) by time-resolved small-angle x-ray scattering (TR-SAX S) using synchrotron radiation. At early stage in Ion-PET, SAXS intensity at a low annealing temperature (Ta = 120 $^{\circ}C)$ decreased monotonously with scattering angle for a while. Then SAXS profile showed a peak and the peak position progressively moved to wider angles with isothermal annealing time. Finally, the peak intensity decreased, shifting the peak angle to wider angle. It is revealed that ionic aggregates (multiplets structure) of several nm, calculated by Debye-Bueche plot, are formed at early stage. They seem to accelerate the crystallization rate and make fine crystallites without spherulite formation (supported by optical microscopy observation). From decrease of peak intensity in SAXS,it is suggested that new lamellae are inserted between the preformed lamellae so that the concentration of ionic multiplets in amorphous region decreases to lower the electron density difference between lamellar crystal and amorphous region. In addition, analysis on the annealing at a high temperature (Ta = 210 $^{\circ}C)$ by optical microscopy, light scattering and transmission electron microscopy shows a formation of spherulite, no ionic aggregates, the retarded crystallization rate and a high level of lamellar orientation.

• Macromolecular Research
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• 제14권6호
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• pp.588-595
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• 2006

The morphology, structure and melting behaviour of cold-crystallized isotactic polystyrene (iPS) were studied by differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD) and small angle X-ray scattering (SAXS). The polymer was found to crystallize according to the dual-lamellar stack model. The two populations of lamellae, along with a melting-recrystallization phenomenon, determined the appearance of multiple melting peaks in DSC traces. The annealing peak was attributed to the relaxation of a rigid amorphous phase, rather than to the melting of crystalline material.

• 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 (${\sim}233\;m^2/g$).

• 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.

• 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.

• Macromolecular Research
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• 제16권7호
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• pp.575-585
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• 2008

There are two beamlines (BLs), 4C1 and 4C2, at the Pohang Accelerator Laboratory that are dedicated to small angle X-ray scattering (SAXS). The 4C1 BL was constructed in early 2000 and is open to public users, including both domestic and foreign researchers. In 2003, construction of the second SAXS BL, 4C2, was complete and commissioning and user support were started. The 4C2 BL uses the same bending magnet as its light source as the 4C1 BL. The 4C1 BL uses a synthetic double multilayer monochromator, whereas the 4C2 BL uses a Si(111) double crystal monochromator for both small angle and wide angle X-ray scattering. In the 4C2 BL, the collimating mirror is positioned behind the monochromator in order to enhance the beam flux and energy resolution. A toroidal focusing mirror is positioned in front of the monochromator to increase the beam flux and eliminate higher harmonics. The 4C2 BL also contains a digital cooled charge coupled detector, which has a wide dynamic range and good sensitivity to weak scattering, thereby making it suitable for a range of SAXS and wide angle X-ray scattering experiments. The general performance of the 4C2 BL was initially tested using standard samples and further confirmed by the experience of users during three years of operation. In addition, several grazing incidence X-ray scattering measurements were carried out at the 4C2 BL.