• Macromolecular Research
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• v.15 no.7
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• pp.662-670
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• 2007

The crystallization behavior and fine structure of poly(ethylene terephthalate) (PET)/A-zeolite nanocomposites were assessed via differential scanning calorimetry (DSC) and time-resolved small-angle X-ray scattering (TR-SAXS). The Avrami exponent increased from 3.5 to approximately 4.5 with increasing A-zeolite contents, thereby indicating a change in crystal growth formation. The rate constant, k, evidenced an increasing trend with increases in A-zeolite contents. The SAXS data revealed morphological changes occurring during isothermal crystallization. As the zeolite content increased, the long period and amorphous region size also increased. It has been suggested that, since PET molecules passed through the zeolite pores, some of them are rejected into the amorphous region, thereby resulting in increased amorphous region size and increased long period, respectively. In addition, as PET chains piercing into A-zeolite pores cannot precipitate perfect crystal folding, imperfect crystals begin to melt at an earlier temperature, as was revealed by the SAXS profiles obtained during heating. However, the spherulite size was reduced with increasing nanofiller content, because impingement between adjacent spherulites in the nanocomposite occurs earlier than that of homo PET, due to the increase in nucleating sites.

• Proceedings of the Membrane Society of Korea Conference
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• 1991.04a
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• pp.1-4
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• 1991

고분자와 희석제 간의 interaction은 phase diagram의 형태로 결정하고 상분리 mechanism은 phase diagram에 의해 설명된다. Thermodynamic interaction이 TIPS 분리막의 구조에 미치는 영향을 조사하기 위하여 PP/C20alkane, PP/C20acid, PP/TA 3가지 system을 선택하였다. 200$^{\circ}$C에서 25 $^{\circ}$C로의 급냉과 분당 10 $^{\circ}$C의 냉각조건을 적용하였다. 각 phase diagram의 형태와 냉각조건에 따라 상분리 mechanism이 달라져서 서론에서 언급한 바와 같이 각기 특유의 구조를 갖게됨을 확인하였다. 같은 종류의 희석제의 chain length가 분리막의 구조에 미치는 영향을 조사하였다. 희석제의 chain length에 따라 결정화 온도가 달라지며 PP와의 결정화 속도 차이에 의하여 구조가 다양하게 변화되었다. 또한 가 희석제의 확산계수의 차이에 의하여 PP 결정화 시 희석제의 외부 방출 정도가 달라 이에 의한 구조의 차이도 관찰되었다. TIPS 공정에서 용액의 조성이 분리막의 구조에 미치는 영향을 조사하였는데, 조성에 의한 nucleation density의 차이에 따라 PP spherulite의 충돌 (impingment)등이 구조에 영향을 미쳤으며 porosity도 변화하였다. 또한 PP/TA system에서는 조성에 따라 상분리 mechanism이 달라져 현격한 구조의 차이를 보였다. 또한 냉각 속도에 따라 PP spherulitic structure가 변화함을 확인하였고, PP 결정화에 따른 희석제의 방출에 의하여 interspherulitic과 intraspherulitic pore를 갖는 2중 구조를 갖게 됨을 알 수 있다.

• Journal of the Korean Society of Safety
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• v.17 no.4
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• pp.101-109
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• 2002

The electrical properties of polyethylene are changed by the superstructure. Such crystalline polymer as polyethylene or polypropylene changes crystallinity and products spherulite or trans-crystal when it is cooled slowly. In this study, after thermal treatment of LDPE at 100[${circ}C$], in silicone oil for an hour, we made specimens in order of slow cooling, water cooling, quenching according to cooling speed. Also, to study the influence of electrical properties due to the superstructure change, we analyzed physical properties and performed dielectric breakdown experiments using DC and impulse voltage Moreover we measured space charges in bulk using Laser Induced Pressure Pulse(LIPP) method. Trap level of specimen is 0.064[eV] at the low temperature region 0.31[eV] at the high temperature region in DC dielectric strength, 0.03[eV] at the low temperature region 0.0925[eV] at the high temperature region in impulse dielectric strength. As its result shows that the quantity of charges induced from the electrode surface increases with applied voltage time, and the distribution of space charges in samples increases the quantity of charges in proportion to applied voltage.

• 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.

• Membrane Journal
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• v.24 no.2
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• pp.158-166
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• 2014

In this research, microporous and bicontinuous poly vinylidene fluoride(PVDF) hollow fiber membranes were prepared via hybrid process of the thermally induced phase separation (TIPS) and stretching method. The mechanism of the membrane preparation is based on liquid-liquid phase separation. The final membranes have characteristic structures which have both bicontinuous and fibrillar morphology by applying the stretching method. They showed quite different structure when compared with the spherulitic or nodular structure from S/L TIPS and bicontinuous structure from L/L TIPS. At first, PVDF hollow fiber precursors were prepared via TIPS method using various kind of diluent mixtures. We used gamma-butyrolacton, dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP) as diluents. We could make hollow fiber membranes which had porous outer surface or dense outer surface by controling the parameters such as cooling conditions, PVDF concentration and the ratio of diluent mixtures. Finally, these hollow fiber were stretched at room temperature and diluents were extracted by ethanol. Effects of the stretching ratio on the membrane morphology were investigated using scanning electron microscope (SEM), and its effects on water flux, porosity, pore size, roughness and tensile strength were examined.

• Polymer(Korea)
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• v.30 no.2
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• pp.175-181
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• 2006

Hybrid process of thermally-induced phase separation and stretching was developed for the preparation of microporous polypropylene hollow fiber membranes. Precursor for stretching was prepared by using soybean oil as a diluent and benzoic acid as a nucleating agent far the sphenlite control and it was stretched far the micrporous hollow fiber membrane. The effects of stretching ratio and deformation rate for stretching process were investigated. Increase of stretching ratio resulted in the greater pore size with nonuniform size distribution. Higher deformation rate also increaser the pore size with uniform size distribution. Stretching ratio was closely related with the orientation of polymer chain and increased the mechanical strength of the fiber. Increase of deformation rate had little effects on the orientation of crystalline phase, and decreased the orientation of amorphous phase which caused the decrease of tensile strength of the fiber and broke the micro-fibrils connecting spherulites to form a circular pore shape.

• Membrane Journal
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• v.31 no.5
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• pp.363-370
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• 2021

Organic solvent resistant hollow fiber membranes were fabricated via a thermally induced phase separation (TIPS) method using Polyketone polymer, a material with excellent resistance to organic solvents. The PEG300, DMSO₂ and Glycerine called the "green solvents" were used as diluents for TIPS method. The spherulite structure was formed with DMSO₂ by S-L phase separation behavior whereas the bicontinuous structures were formed with PEG300 and Glycerine, respectively. The morphology of the PK hollow fiber membranes was investigated using SEM. The pure water permeability and the durability test were conducted to understand the permeation properties of PK hollow fiber membranes. The tensile strength test was conducted for the property of mechanical strength. In this study, the fabrication of PK hollow fiber membranes with various diluents was discussed to understand the correlation between diluent and polymer in detail.

• Journal of the Korean earth science society
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• v.27 no.3
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• pp.313-327
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• 2006

This study investigated the geochernical characteristics of Mn scale formed in groundwater wells at the Damyang area. The composition of Mn scale consists mainly of MnO and $SiO_2$. The content of Mn ranges from56.61wt.% to 68.69wt.%, and $SiO_2$ content ranges from 1.56wt.% to 10.45wt.%. The contents of Mo and Ba in Mn scale increased with increased depth; whereas, the content of Zn and Pb decreased with increased depth. Birnessite, quartz and feldspars were identified in Mn scales using x-ray powder diffraction studies. The IR absorption bands for Mn scales show major absorption band due to OH stretching, adsorbed molecular water, and birnessite stretching, respectively. In the SEM and EDS analysis, the Mn scale consists of botryoidal, spherical, spherulite, and empty straw structure. Those structure may be precipitated simply due to oversaturation with concentrated Mn content or may be formed through biogenic precipitation by Lepthothrix discophora. Under microanalysis using EDS on those structure surface of Mn scales, the Mn atomic percent range from 28 to 44, and such elements revealed the presence of Si, K, Na, Ca, Cl, Cu, Zn, and Ba.

• Journal of Sericultural and Entomological Science
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• v.35 no.1
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• pp.60-68
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• 1993

It has been known that the silk degumming treated by hot alkali solution is easy to handle but is liable to yield poor-quality silk due to the degree of degumming loss, incomplete-degumming or over-degumming. Therefore, many studies have been carried out on the silk degumming by enzyme in order to improve the quality of silk. However, no attention has been paid to the physicochemical analysis of enzymatic degummed silk. In this paper, two different degumming methods, soap and enzymatic, are compared in aqueous solution state of silk fibroin. The results can be summarized as follows: There was no significant difference between two solutions on the bases of polarizing microscopy, TEM observation and SDS-PAGE. Spherulite of silk fibroin was not observed in polarizing microscopy, however the leaf-shape fibril structure was developed upon solidification. The size of spherulites of silk fibroin in TEM observation were 30~120nm with a wide range of size distribution. The intrinsic viscosity of enzymatic degummed fibroin solution was lower than that of soap degummed solution. This can be explained that the silk fibroin was more degraded by enzymatic degumming method compared with the soap degumming method. SDS-polyacrylamide gel electrophoresis showed that the fibroin molecule was composed of large component of molecule weight above 50 kd and small component of molecule weight about 20 kd. There was no difference in crystallinity between two degumming methods on the bases of results of DSC thermograms and IR spectra.

• The Journal of the Petrological Society of Korea
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• v.22 no.3
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• pp.219-233
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• 2013

Spherulitic rhyolite occur as part of ring dyke which showing a vertical flowage of $60^{\circ}{\sim}90^{\circ}$, of the Jangsan cauldron was studied. The spherulites range in diameter from a few millimeters to 2.8 centimeters or more, and average 5~10 millimeters. It belongs to radiated simple spherulite type. They consist of a core of moderate brown dense material encased by a thin crust, a few millimeters thick at most of white grey material. The spherulites frequently have a radiating fibrous structure, which are thought to have formed as a consequence of rapid mineral growth caused by very fast cooling of the dykes in shallow depth near the surface. EPMA examination of the concentric-zoned core of spherulites show that they are mainly composed of cryptocrystalline-fibrous intergrowth of silica minerals and alkali feldspars which have $SiO_2$ 82% or more, $Al_2O_3$ 7~10%, $Na_2O+K_2O$ less than 8%. The feldspar compositions of the spherulites lie essentially within the sanidine field. XRD examination show that spherulites are mainly composed of quartz, sanidine, albite with minor mica, kaolinite and chlorite. According to X-ray mapping, the spherulites are enriched in $SiO_2$ in the core and partly enriched $Na_2O$ or $K_2O$, $Al_2O_3$ in the shell that reflect in compositional zoning with increasing spherulitic devitrification. The feathery and non-equant crystal shapes of spherulites from rhyolite dyke of Jangsan cauldron suggest that they may have formed during the rapid cooling of dyke under the static state, or faster velocity of devitrification from glassy materials than movement velocity of the magma intrusion. The spherulitic rhyolite originated from high-silica(75.4~75.7 wt.%) rhyolite magma.