• Macromolecular Research
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• v.16 no.8
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• pp.725-733
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• 2008

Polyimide (PI) multilayer thin films were prepared by spin-coating from a poly(amic acid) (PAA) and poly(amic acid) ammonium salt (PAAS). PI was prepared from pyromellitic dianhydride (PMDA) and 4,4'-oxydianiline (ODA) PAA. Different compositions of PAAS were prepared by incorporating triethylamine (TEA) into PMDA-ODA PAA in dimethylacetamide. PI multilayer thin films were spin-coated from PMDA-ODA PAA and PAAS. The PAAS comprising cationic and anionic moieties were spherical with a particle size of $20{\sim}40\;nm$. Some particles showed layers with ammonium salts, despite poor ordering. Too much salt obstructed the interaction between the polymer chains and caused phase separation. A small amount of salt did not affect the interactions of the interlayer structure but did interrupt the stacking between chains. Thermogravimetric analysis (TGA) showed that the average decomposition temperature of the thin films was $611^{\circ}C$. All the films showed almost single-step, thermal decomposition behavior. The nanostructure of the multilayer thin films was confirmed by X -ray reflectivity (XRR). The LF 43 film, which was prepared with a 4:3 molar ratio of PMDA and ODA, was comprised of uniformly spherical PAAS particles that influenced the nanostructure of the interlayer by increasing the interaction forces. This result was supported by the atomic force microscopy (AFM) data. It was concluded that the relationship between the uniformity of the PAAS particle shapes and the interaction between the layers affected the optical and thermal properties of PI layered films.

• Proceedings of the Membrane Society of Korea Conference
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• 1996.10a
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• pp.49-50
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• 1996

비다공성막에서의 기체투과는 분리용막의 재료가 되는 기능성 고분자와 분리하고자 하는 기체 혼합물과의 작용이 투과확산을 지배하며 고분자의 구조에 의하여 결정되는 극성, 수소결합, 응집 에너지 밀도, 고분자 주쇄 유연성, 입체장애, 주쇄간 거리, 측쇄기의 운동성 등의 많은 인자들과 막결정화도 등의 인자들이 복합되어 기체투과에 작용하기 때문에 고분자 구조와 투과 특성과의 관계가 정량적으로 밝혀지지않고 있으나, 실험적 사실을 근거로 정성적 고찰이 이루어지고 있으며 몇가지 고분자막 미세구조를 나타내는 측정가능 물성들과 투과 특성을 상관시킬 수 있다. 폴리이미드막은 합성되는 diahydride와 diamine의 변화에 의해 다양한 화학적 구조를 갖는막을 만들 수 있으며 이들 막의 물성치들과 투과특성들도 서로 다르게 나타난다. 본 연구에서는 PMDA-MDA polyimide를 기본으로하여 다른 종류들의 Phenylene diamine을 첨가시켜 제조한 서로 다른 화학적 구조를 갖는 기체분리막들의 측정 가능한 물성치들과 산소, 질소 투과특성의 연관상을 연구하여 이들 사이의 정성적 상관성이 있음을 고찰한다.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1996.05a
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• pp.154-157
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• 1996

The thin films are fabricated by VDPM and its heat resistant characteristics are investigated using Thermogravimetry. About polyimide, there is a wide difference between 5% weight loss temperature of TG curve and 20,000hr. of life time by methode of ASTM D2307. Therefore, TGI can be obtained by thermogravimetric analysis of NEMA std. pub. NOREI-1974. The TGI was got 670, 674 and 585 at 20$^{\circ}C$, 40$^{\circ}C$ and 70$^{\circ}C$, respectively.

• Proceedings of the Korean Fiber Society Conference
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• 2003.10b
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• pp.130-133
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• 2003

폴리이미드(poly(imide), PI)는 반복 단위 내에 이미드 그룹을 함유하고 있는 고분자로 매우 강한 물리적인 특성을 지니며 열적 및 화학적 안정성이 매우 큰 고분자이다[1-4]. 그러나 이는 대부분이 불용ㆍ불융하기 때문에 프리커서인 poly(amic acid) (PAA) 용액 상태에서 어느 특정한 형태로 가공한 후 열적 혹은 화학적 방법에 의해 이미드 구조로 전환시켜준다. PAA 용액에 사용되는 용매로는 N,N-dimethylacetamide (DMAc), N-methyl-2-pyrrolidone (NMP), N,N-dimethyl-formamide(DMF) 등과 같이 비등점이 높은 극성 용매들이 사용되어진다. (중략)

• Applied Chemistry for Engineering
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• v.10 no.7
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• pp.1041-1045
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• 1999

Three polysiloxaneimide(PSI) as membrane material were prepared by polycondensation of three aromatic dianhydrides(6FDA, BTDA, PMDA) with one siloxane-containing diamine(SIDA, aver. MW. 800). The PSIs were rubbery polymers containing 30~40 wt % of flexible siloxane chains and exhibited low density, high fractional free volume and low surface energy. They were used for pervaporation experiments with 0.05 wt % of four organic aqueous solutions containing ethyl acetate, methylene chloride, trichloroethylene, and toluene, respectively. With increasing hydrophobicity of organic solvents, both pervaporation selectivity and pemeation flux increase.

• Applied Chemistry for Engineering
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• v.27 no.1
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• pp.50-55
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• 2016

Aromatic diamines containing hexafluoroisopropylidene and ester moiety were synthesized from 4,4'-hexafluoroisopropylidene diphenol and nitrobenzoyl chloride. The reaction of aromatic diamines with hexafluoroisopropylidene phthalicdianhydride (6FDA) or pyromellitic dianhydride (PMDA) gave four kinds of poly(amic acid)s. Their inherent viscosities ranged from 0.196 to 0.346 dL/g. Poly(amic acid)s were converted to polyimides by thermal imidization. The glass transition temperatures ($T_g$) of polyimides were between 241 and $289^{\circ}C$. The 5% weight loss temperatures were recorded in the range of $430{\sim}492^{\circ}C$. The tensile strength of polyimide films were measured as 29.84~64.38 MPa.

• Journal of the Korean Chemical Society
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• v.31 no.6
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• pp.590-600
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• 1987

Silicone-containing polyamide-imides were prepared from bis(p-chlorocarbonylphenyl)diphenylsilane (BCCDPS), pyromellitic dianhydride(PMDA) and diamines. The thermal characteristics of the above polymers had been carefully studied using a thermogravimetric analyzer. The thermal stability of polymer was decreased with increasing contents of bis(p-carbonylphenyl)diphenylsilane units(BCDPS). The effect of diamine on thermal stability of polymer led benzidine > m-phenylenediamine> 4,4'-diaminodiphenyl ether > 4,4'-diaminodiphenyl sulfone. The activation energy of degradation of polymer obtained by Friedman method increased as the contents of BCDPS in the polymer decreased. The degradation temperature of polymers generally increased as the activation energy increased. The solubility of polymer increased as the content of BCDPS increased except polymers prepared with benzidine.

• Macromolecular Research
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• v.12 no.3
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• pp.263-268
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• 2004

We have synthesized a water-soluble polyimide precursor, poly(amic acid) amine salt (PAD), from pyromellitic dianhydride (PMDA), 4,4'-oxydianiline, and N,N -dimethylethanolamine (DMEA) and have investigated in detail its properties with respect to the degree of salt formation (D$\_$sf/). The maximum value of D$\_$sf/ we obtained upon precipitation of the precursor solution into acetone was 79%. We synthesized a PAD having a D$\_$sf/ of 100% (PAD100) by the solid state drying of an organic solution. The precursors showed different solubility depending on the D$\_$sf/ to make up to 4 wt% solutions in water containing a small amount of DMEA. PAD100 is completely soluble in pure water. We investigated the imidization behavior of PAD in aqueous solution using various spectroscopic methods, which revealed that PAD 100 has faster imidization kinetics relative to that of the poly(amic acid)-type precursors. The resulting polyimide films prepared from an aqueous precursor solution possess almost similar physical and thermal properties as those prepared from N-methyl-2-pyrrolidone(NMP) solution. Therefore, we have demonstrated that PAD can be used as a water-based precursor of polyimide; this procedure avoids the use of toxic organic solvents, such as NMP.

• Proceedings of the KIEE Conference
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• 1997.07d
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• pp.1216-1218
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• 1997

Hydrolysis of BTDA-ODA: MPDA, PMDA-ODA, PIQ polyimides were investigated by FT-IR. The results showed that hydrolysis depends on structure of polyimide and that polyimide obtains hydrolytic stability by curing. Polyimide-aluminum interfaces were characterized by RAIR. It was concluded that imidization of the polyamic acid to polyimde was inhibited by interaction of acid groups with substrate to form aluminum carboxylate.

• Applied Chemistry for Engineering
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• v.17 no.2
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• pp.217-222
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• 2006

Polyimides have been investigated extensively and used widely over the past three decades because of their high performance properties such as excellent thermal, mechanical, and electrical properties. Polyimides are difficult to be processed because of the aromatic moieties, imide group, and insoluble nature in most organic solvents. The soluble polyimides were synthesized from 2,2,-bis(3-amino-4-hydroxyphenyl) hexafluoropropane (BAPAF) and 3,3,-diamino-4,4-dihydroxybyphenyl (HAB) as aromatic diamines and 4,4-(hexafluoroisopropylidene)diphthalic dianhydride (6FDA), pyromellitic dianhydride (PMDA), 4,4-oxydiphthalic dianhydride (OPDA), 3,3,4,4-benzophenone tetracarboxylic dianhydride (BTDA) and 3,3,4,4-diphenylsulfone tetracarboxylic dianhydride (DSDA) as aromatic dianhydrides. The polyimides were characterized by NMR, FR-IR, TGA and the dielectric constant of the obtained polyimides was calculated from storage of electro-capacity. A novel photosensitive polyimide was synthesized by the reaction of polyimide, containing hydroxyl group and methacryloyl chloride using triethylamine. The good micro-pattern was obtained with photosensitive polyimide from the photolithographic technique.