• Korean Chemical Engineering Research
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• v.43 no.1
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• pp.66-70
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• 2005

For the application in HI decomposition reaction of thermochemical water-splitting IS process, the carbonized membranes using the polymer material (polyimide) were prepared, and SiC membrane was also prepared by SiO treatment on those carbonized membranes. The weight change by the carbonation of polyimide was about 50%, and the weight decreased with an increase of carbonation temperature. The gas permeance ($H_2$ or $N_2$) of carbonized membrane decreased with an increase of carbonation temperature led to the pore closing. The gas permeance ($H_2$ or $N_2$) of SiC membrane increased with an increase of SiO treatment concentration, and the gas permeation mechanism was changed from the activiation energy flow to Knudsen flow.

• Membrane Journal
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• v.23 no.6
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• pp.450-459
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• 2013

2,3,5,6-Tetramethyl-1,4-phenylenediamine (TMPD) based polyimide (PI) were crosslinked with 1,2-Diaminoethane (DAE) and 1,6-Diaminohexane (DAH) to enhance gas transport properties. Fourier transform infrared (FT-IR) studies show that imide groups were converted into amide groups during crosslinking process. Thermogravimetric analysis (TGA) results indicate that the degradation temperature of crosslinked PI membranes decreased after crosslinking. This is due to degradation of alkyl group in crosslinking agent. The d-space of crosslinked PI membranes decreased with increasing crosslinking time. The ideal permeability for $CH_4$, $N_2$, $O_2$, and $CO_2$ decreased after crosslinking and the ideal permeability of crosslinked PI membranes induced by DAH is larger than that by DAE. In contrast, the permselectivity of $CO_2/CH_4$, $CO_2/N_2$ and $O_2/N_2$ increased during crosslinking. For the gas pair of $CO_2/CH_4$, the maximum increment is about 39.5% after 6 minutes of DAE crosslinking. Also, that of $O_2/N_2$ gas pair is about 20.5% after 6 minutes of DAE crosslinking. According to these result, DAE is more suitable for enhanced permselectivity than DAH. On the contrary, DAE is not useful for $CO_2/N_2$ separation due to reduction in $CO_2/N_2$ permselectivity after 3 minutes DAE crosslinking.

• Applied Chemistry for Engineering
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• v.24 no.3
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• pp.320-326
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• 2013

In this study, various polyimide films were synthesized via low temperature cure in order to understand changes in their physical properties when using 4,4'-oxydianiline (ODA) as a diamine and dianhydride molecules with different backbones on a single diamine such as 4,4'-Oxydiphthalic anhydride (ODPA), 4,4-hexafluoroisopropylidene diphthalic dianhydride (6FDA), and 3,3', 4,4'-benzophenone tetracarboxylic dianhydride (BTDA). After the synthesis of poly(amic acid), polyimide films were fabricated by adding 1,4-diazabicyclo [2.2.2]octane (DABCO), a low-temperature catalyst, at various wt% to poly(amic acid)s. Changes of optical and thermal properties were compared and analyzed between polyimide films without catalyst and polyimide films with catalyst by FT-IR, UV-Vis transmittance, DSC/TGA, and WAXD analysis. Wide-angle X-ray diffraction (WAXD) analysis revealed that the mean intermolecular distance decreased with the use of a catalyst by the type of dianhydride. Thus, while the optical properties of the films improve by a low-temperature cure performed using a catalyst, their thermal properties decrease. These changes can be explained by the changes in the morphological structure of the films triggered by a catalyst-induced reduction in the mean intermolecular distance. Moreover, the results show that the type of dianhydride determines the degree of change in the optical and thermal properties in each types of polyimide, demonstrating that changes in the optical and thermal properties are directly associated with the backbone of the polyimide structure.

• Membrane Journal
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• v.23 no.6
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• pp.393-408
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• 2013

Gas separation processes using polymeric membranes have been greatly developed during the last few decades due to high energy efficiency and economic advantages. To achieve optimum economic performance, gas separation membranes required high permeability and selectivity. So, a number of reports examining the various polymeric materials for gas separation membranes have been published. Among the studied materials, polyimide (PI), which exhibit high permselectivity for various gas pairs, high chemical resistance, thermal stability, and mechanical strength, have attracted much attention. This paper focuses on the basic principle of gas separation, preparation procedure of membrane along with the recent developments and research trends of PI based materials for gas separation.

• Proceedings of the International Microelectronics And Packaging Society Conference
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• 2003.11a
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• pp.181-184
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• 2003

Low Energy High flux Plasma Source인 Stationary Plasma thruster (SPT)를 이용하여 폴리이미드의 표면개질 후 접촉각과 표면에너지의 변화를 조사하고 접착력과의 관계를 조사하였다. 이온에너지는 180 eV - 200 eV, 이온전류 밀도는 수백 ${\mu}A/cm^2$, 이온선량은 $5\times10^{15}/cm^2$부터, $10\times^{18}/cm^2$로 $Ar^+,\;N_2^+,\;O_2^+$를 이온 주입시켰다. 표면 처리된 폴리이미드에 대한 접촉각 변화는 dual contact anglemeter로 증류수와 에틸렌글리콜을 이용하여 측정하였고, 표면에너지의 변화량을 구하였다. 접촉각의 변화는 아르곤 이온의 경우는 최저 $35^{\circ}$, 질소와 산소의 경우 $1\times10^{17}/cm^2$에서 각각 $14^{\circ},\;10^{\circ}$정도의 전촉각을 보였으며, $5\times10^{17}/cm^2$이상에서는 측정하기 불가능하였다. 산소 이온빔으로 처리된 PI의 표면을 x-ray photoelectron spectroscopy를 통하여 측정하여본 결과, 친수성기가 많이 형성되었음을 확인할 수 있었다. 접촉각 측정으르부터 PI의 표변에너지는 42.1 mN/m에서 아르곤 이온빔의 처리 시 65.2 mN/m로 산소 이온빔의 처리 시 81.2 mN/m로 각각 1.5배, 1.9배 정도 증대하였다. 산소 이온빔으로 처리된 PI 표면위에 스퍼터링으로 300 nm 정도의 clad layer 형성 후 $20{\mu}m$ 정도의 구리 전기 도금막을 형성하여, peel 강도를 측정한 결과 0.79 kg/cm의 강도를 얻을 수 있었다.

• Journal of the Microelectronics and Packaging Society
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• v.14 no.1
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• pp.39-47
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• 2007

It is investigated how KOH and Rthylenediamine(EDA) treatment conditions on Polyimide film surface affect the interfacial fracture energy between electroless plated Ni and Polyimide film by $180^{\circ}$ peel test. Estimated values of interfacial fracture energy were 24.5 g/mm and 33.3 g/mm for the KOH treatment times under 1 and 5 minutes, respectively, while, those were 31.6 g/mm and 22.3 g/mm for EDA treatment times under 1 and 5 minutes, respectively. Interfacial bonding between electroless plated Ni and Polyimide seems to be dominated by chemical bonding effect rather than mechanical interlocking effect. It is found that chemical treatment produces carboxyl and mine functional groups which are closely related the interfacial bonding mechanism. Finally, it is speculated that interfacial fracture energy seems to be controlled by O=C-O bonding near cohesive failure region.

• Membrane Journal
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• v.27 no.5
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• pp.389-398
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• 2017

The most important characteristic of the polymer electrolyte membranes (PEMs) for fuel cells, the proton conducting ability is mainly influenced by the distribution and morphology of the water channels inside the PEMs. Non-perfluorinated hydrocarbon PEMs are known to have weaker water channels than perfluorinated PEM, Nafion, and thus relatively low proton conducting ability. In this study, we used a mesoscale simulation technique to observe the water channel formation and phase separation behavior of hydrocarbon PEM, sulfonated polyimides, under the humidification condition. It was observed that the water molecules were distributed evenly through the entire hydrophilic region, and clear water clusters were formed only in the sulfonated polyimide having high sulfonation degree. In addition, it was observed that sulfonated polyimides have a difficulty in forming water channel under the low hydrated condition. These results clearly support the theories of the formation of water channels in non-perfluorinated hydrocarbon PEMs, and also well explain the tendency of proton conducting abilities of sulfonated polyimides. Thus, it is confirmed that mesoscale simulation techniques can be very effective in analyzing phase separation behavior and water channel formation in PEMs for fuel cells and elucidating the ion conducting abilities.

• Membrane Journal
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• v.25 no.3
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• pp.223-230
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• 2015

We synthesized novel polyimides with high gas permeability and selectivity for application of gas separation membrane. 2,2-bis(3,4-carboxylphenyl) hexafluoropropane dianhydride (6FDA) and two kinds of amines with high permeability and solubility were used to prepare the novel polymide. 2,4,6-Trimethyl-1,3-phenylenediamine (DAM) was used to improve gas permeability and 4,4-Methylenedianiline was used to improve the gas selectivity respectively. The polyimide copolymers were synthesized by commercial chemical imidization method using Triethylamine and Acetic anhydride and their average molecular weights were over 100,000 g/mol. The glass temperature (Tg) and the thermal degradation temperature were characterized using differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). The synthesized copolymers showed high Tg over $300^{\circ}C$ and high thermal degradation temperature over $500^{\circ}C$. The gas permeation properties were measured by time-lag equipment. Although general polyimides showed very low gas permeability, synthesized polyimide copolymer showed high $O_2$ permeability of 10.1 barrer with high $O_2/N_2$ selectivity around 5.3. From this result, we confirm that these membranes have possibility to apply to gas separation membrane.

• Polymer(Korea)
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• v.38 no.6
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• pp.752-759
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• 2014

Crosslinked polyimides (PIs) were synthesized by reacting 4,4'-(hexafluoroisopropylidene)-diphthalic anhydride (6FDA) and 2,2'-bis(trifluoromethyl)benzidine (TFDB) with various ratios of the cross-linkable, end-capping agent cis-1,2,3,6-tetrahydrophthalic anhydride (CDBA) via ring-opening metathesis polymerization. Residual stress behaviors were investigated in-situ during thermal imidization of the crosslinked PI precursors using a thin film stress analyzer (TFSA) by wafer bending method. The thermal properties were investigated via differential scanning calorimetry (DSC), thermomechanical analysis (TMA), and thermogravimetric analysis (TGA). The optical properties were measured by ultraviolet-visible spectrophotometer (UV-vis) and spectrophotometry. All properties were interpreted with respect to their morphology of crosslinked networks. With increasing the amounts of the end-capping agent, the residual stress decreased from 27.9 to -1.3 MPa, exhibited ultra-low stress and high thermal properties. The minimized residual stress and enhanced thermal properties of the crosslinked PI makes them potential candidates for versatile high-density multi-layer structure applications.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.08a
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• pp.258-258
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• 2011

최근 유연 기판을 이용한 태양전지 및 TFT 등 전자소자 개발에 관한 연구가 주목받고 있다. 본 연구에서는 공정 시 유리한 유리기판상 전자소자 제작 후 폴리이미드막 박리를 통한 유연전자 소자 구현을 목적으로 한다. 폴리이미드막 박리를 목적으로 희생층으로서 a-Si:H을 사용하였다. 유리기판상에 60 nm 두께의 a-Si : H을 ICP (Induced coupled plasma) 공정으로 증착한 후 a-Si : H층 상부에 30 ${\mu}m$ 두께로 폴리이미드를 코팅하여 Hot plate와 furnace에서 열처리를 거쳤다. 이후 각기 다른 파장을 갖는 레이저의 파워를 가변하며 유리 기판 후면에 조사하였다. 실험 결과 355 nm UV 레이저로 가공한 경우 희생층으로 사용 된 a-Si : H층 내에 존재하는 수소가 레이저 빛 에너지에 의해 결합이 끊어지면서 유리기판과 폴리이미드막이 분리됨을 확인하였다.