• Proceedings of the Membrane Society of Korea Conference
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• 1996.10a
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• pp.75-76
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• 1996

다공성 고분자 분리막을 제조하는 방법으로 기존의 용매교환법을 대신하여 내용매성, 내약품성 및 내열성이 매우 뛰어난 고분자를 소재로하여 다공성 고분자막을 만드는 열유도 상분리법(Thermally Induced Phase Separation, TIPS)이 개발되었다. TIPS공정에서는 주로 고분자/희석제 system의 열역학적인 불안정성에 의하여 polymer-rich phase와 polymer-lean phase로 상이 분리되는 liquid-liquid phase separation과 결정성 고분자의 결정화에 의한 solid-liquid phase separation을 주로 상분리 mechanism으로 사용하고 있다. 따라서 위에 언급된 TIPS 이론에 근거한 melt spinning 공정에 의하여 PP 중공사막을 제조하였는데 wet spinning 공정에 의한 용매 교환법에 비해 비교적 공정이 단순하고 다공도를 조건하기가 용이하며 구조 및 성능면에서도 높은 재현성을 가지고 있다. 또한 우수한 소재임에도 불구하고 절절한 용매의 부재로 용매교환법에서 사용할 수 없었던 폴리올레핀계, 나일론계, 방향족출합계 고분자를 사용할 수 있게 되어 소재의 폭이 넓어졌다는데에 가장 큰 장점이 있다. 본 연구에서는 PP중공사막을 제조하기 위하여 먼저 용융 방사장치를 제작하였고 melt spinning 공정에 의해 막을 제조하는데 적합한 방사조건들을 확립한 후 결정된 방사조건에 의해 얻어진 PP 중공사막의 구조 및 성능에 영향을 미치는 인자들에 관하여 조사하였다.

• Proceedings of the Membrane Society of Korea Conference
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• 2005.11a
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• pp.250-254
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• 2005

• Korean Chemical Engineering Research
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• v.43 no.1
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• pp.16-20
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• 2005

Porous polypropylene membranes were prepared by a thermally induced phase separation method in super-critical $CO_2$, where polypropylene and Camphene were used as raw materials. The porosity of polypropylene membranes with 10 wt% polypropylene concentration was 78, 80, 73% by using methanol, ethanol, and n-buthanol as an analytical solvent, respectively. The tensile strength increased with an increasing polypropylene concentration, where it was $0.17kg_f/mm^2$ at 10 wt% polypropylene concentration. The extraction rate for Camphene increased with time and Camphene was removed 94% in 5 min. It increased with an increasing temperature and was 99% at $45^{\circ}C$, however, decreased with an increasing temperature at higher than $45^{\circ}C$. The extraction rate increased with an increasing pressue up to 150 bar, however, decreased slightly with an increasing pressure over 150 bar. The extraction rate had a relation with the solubility of Camphene in supercritical $CO_2$.

• Fashion & Textile Research Journal
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• v.10 no.2
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• pp.254-259
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• 2008

Poly(ethylene-co-vinylacetate)(EVA) microspheres were prepared by a thermally induced phase separation. The microsphere formation occurred by the nucleation and growth mechanism in the metastable region. The diluents used were toluene. The microsphere formation and growth was followed by the cloud point of the optical microscope measurement. The microsphere size, which was obtained by SEM observation and particle size analyzer, became decreased when the titanium dioxide($TiO_2$) concentration was higher. The deodorizing function of the prepared fabrics was studied by the determination of the decomposing capability for $NH_3$. The deodorant activity of these deodorizing fabrics was measured by chromogenic gas detector tubes. The deodorant activity of $NH_3$ increased with increasing $TiO_2$ concentration of EVA microsphere.

• Fashion & Textile Research Journal
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• v.10 no.3
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• pp.371-376
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• 2008

Poly(ethylene-co-vinylacetate) (EVA) microspheres were prepared by thermally induced phase separation (TIPS) in toluene. The microsphere formation occurred by the nucleation and growth mechanism in metastable region. The effects of the concentration and component of the polymer and cooling rate on microsphere formation were investigated. The microsphere formation and growth were followed by the cloud point of the optical microscope measurement. The microsphere size distribution, which was obtained by particle size analyzer, became broader when the polymer concentration was higher, the content of vinyl acetate in EVA copolymer was higher, the cooling rate of EVA copolymer solution were lower. The content of disperse dye in EVA microsphere was obtained by TGA thermal analysis, the dye content of EVA15 and EVA18 were 3.5 and 2.0 wt% respectively.

• Proceedings of the Membrane Society of Korea Conference
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• 1995.04a
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• pp.1-4
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• 1995

The microstructure of polymer membranes produced via thermally induced phase separation (TIPS) of polymer solutions is a strong function of both the early-stage (by spinodal decomposition or nucleation & growth) and the late-stage phase separation (referred to in general as coarsening). In the case of early stage effects, the membrane morphology resulting from a nucleation & growth mechanism is either a poorly interconnecsed, stringy, beady structure which is mechanically fragile or a well interconnected structure with highly nonuniform pore sizes. In contrast, spinodal decomposition results in a well interconnected, mechanically strong membrane with highly uniform pore sizes. Here I describe recent quantitative studies of the coarsening effects on the microstructure of membranes produced via TIPS process. The dependence of microstructure on coarsening time, quench depth, solution viscosity, and polymer molecular weight was investigated in order to distinguish among three possible coarsening mechanisms, Ostwald ripening, coalescence, and hydrodynamic flow, which may be responsible for structural evolution after the early-stage phase Separation (spinodal decomposition or nucleation & growth).

• 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.

• Membrane Journal
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• v.29 no.6
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• pp.362-376
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• 2019

In this study, hydrophilic coating characteristics of PVDF [poly(vinylidene fluoride)] hollow fiber membranes with flower type cross-section prepared by thermally induced phase separation were studied. The hollow fiber used in this study was provided from PureEnvitech Co. Ltd., and the hydrophilic coating experiment was performed with different concentration and number of coating of PEBAX 1657, 2533 and 3533 block copolymer solution using a dip coating method. The hydrophilic coated hollow fiber membrane was characterized to scanning microscope and contact angle measurements to determine the degree of hydrophilization. As a result of SEM characterization, it was confirmed that the thickness of the coating layer increased as the coating concentration increased and the number of coatings increased. Contact angle of surface of hollow fibers decreased as the concentration of the coating solution increased and the number of coatings increased. Gas permeance of oxygen gas was measured for the application of the hydrophilized hollow fiber to Membrane Areated Biofilm Reactor. As a result of gas permeation test, it was confirmed that gas permeance decreased with increasing coating concentration and number of coatings, and the more hydrophilized hollow fiber coated with PEBAX 1657 showed lower gas permeance than those coated with PEBAX 2533 and 3533.

• Journal of the Korean Applied Science and Technology
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• v.29 no.3
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• pp.370-376
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• 2012

We fabricated linear low density polyethylene (LLDPE) particles via crystallization from decalin solution. In the thermally induced phase separation (TIPS) process, formation of particles occurred during controlled cooling of LLDPE/decalin solution. Despite an increase of nucleation and growth rate for crystals at higher polymer concentrations, which generally results in larger particles than at lower concentration, the average diameter of LLDPE particles increased as LLDPE was more concentrated in decalin solution. In the FE-SEM micrographs, the observed particles from various concentrations were smaller than 10 ${\mu}m$, showing spherical morphologies. In addition to its effect on size, concentration of LLDPE had an broadening effect on the particle size distribution.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.32 no.1
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• pp.64-69
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• 2019

Methylammonium lead triiodide ($MAPbI_3$)-based perovskite solar cells potentially have potential advantages such as high efficiency and low-cost manufacturing procedures. However, $MAPbI_3$ is structurally unstable and has low phase-change temperatures ($30^{\circ}C$ and $130^{\circ}C$); it is necessary to solve these problems. We investigated the crystal structure and phase separation using real-time temperature-change X-ray diffraction, transmission electron microscopy, and electron energy loss spectroscopy. $MAPbI_3$ has a tetragonal structure, and at about $35^{\circ}C$ the c-axis contracts, transforming $MAPbI_3$ into the related cubic crystal structure. In addition, at $130^{\circ}C$, phase separation occurs in which $CH_3NH_2$ and HI at the center of the unit cell of the perovskite structure are extracted by gas, leavingand only $PbI_2$ of the three-component structure, is produced as the final solid product.