• 폴리머
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• 제36권4호
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• pp.448-454
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• 2012

폴리아믹산(poly(amic acid), PAA)은 불소치환 단량체인 4,4'-(hexafluoroisopropylidene)diphthalic anhydride(6FDA)와 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluropropane(BAPP)의 조성으로 N,N'-dimethylacetamide(DMAc) 용매에서 반응을 하여 얻어졌으며, 폴리이미드(polyimide, PI) 필름은 PAA을 각각 다른 온도에서 열처리하여 얻었다. 제조된 필름을 얻기 위해 $80-230^{\circ}C$까지 열처리를 하였으며, 용제 증발에 따른 이미드화도 변화를 알아보기 위해서 폴리아믹산 용액을 얻은 후 열중량 분석기(thermogravimetric analysis, TGA)를 통하여 시간과 온도에 따른 용제 증발 정도를 측정하였다. 이에 따른 이미드화 지수는 적외선 분광분석기(fourier transform infrared spectroscopy, FTIR) 스펙트럼을 통해 확인하였다. 시간과 온도에 따른 이미드화도를 통해 용매가 빠르게 증발하지만 용매가 잔류하고 있는 반응의 초기에 이미드화가 빠르게 일어나는 것을 확인하였고, 시간이 흘러 용매의 증발 정도가 줄어들고, 잔류용매가 사라지는 시점에서의 이미드화 지수는 일정하게 나타나는 것을 확인하였다. 이미드화는 온도가 증가함에 따라 진행되나 반응 온도가 $200^{\circ}C$ 이상으로 과도하게 높은 경우에는 용매가 남아 있지 않아 반응시간을 증가시켜도 이미드화 지수가 오히려 감소하는 현상을 보였다.

• Elastomers and Composites
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• 제51권2호
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• pp.138-146
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• 2016

It is an inconvenience for silica nano-particles to dry again when using it in that they cohere each other through moisture in the air. Acrylamide groups were introduced to improve such inconvenience and copolymerized with silica nano-particles and then we copolymerized again with polyamic acid in order to increase thermal characteristic. Amide block copolymers were prepared using silica and (3-mercaptopropyl) trimethoxysilane (MPTMS) with a siloxane group, using 2,6-Lutidine as a catalyst. Amide block polymers and copolymers were synthesized via ATRP after brominating pyromellitic dianhydride (PMDA) and polyamic acid of methylene diphenyl diamine (MDA), using ${\alpha}$-bromo isobutyryl bromide. Characteristic peaks of copolymer with amide and imide groups and patterns of amorphous polymers were researched by FT-IR and XRD analyses and the analysis of surface characteristic groups was conducted via XPS. A change in thermal properties was examined through DSC and TGA and solubility for solvents was also researched.

• 한국막학회:학술대회논문집
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• 한국막학회 1997년도 추계 총회 및 학술발표회
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• pp.83-84
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• 1997

1. INTRODUCTION : Polyimides containing siloxane moiety(poly(imide siloxane), or polysiloxaneimide) have been synthesized because of their some merits over polyimide itseft. Polyimides have excellent thermal and mechanical properties but their poor solubility and processibility in their fullly imidized form give disadvantages in applications. Incorporation of siloxane units make it possible to increase solubility and processibility, and also impart impact resistance, low moisture uptake, low dielectric constant, thermo-oxidative resistance, good adhesion properties to substrate and etc.. Incorporation methods of siloxane groups into the polyimide was mainly copolymerization or terpolymerization between oligomeric dimethylsiloxane and aromatic dianhydride. A few methods of introducing siloxane units in functional groups of polyimide was reported. In our laboratory poly(amideimide siloxane) and poly(imide siloxane) were prepared and the study about their thermal kinetics was performed. In separation membrane area, polysiloxaneimides was utilized in pervaporation and gas separation. Polyimides in gas separation show high selectivity and very low permeability, and introduction of siloxane segments increase permeability with low decrease in selectivity. We aimed to introduce silicone segments into poly(amic acid) state and synthesize polymer partially imidized, and also show the gas separation characteristics of the synthesized polymer.

• Macromolecular Research
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• 제9권6호
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• pp.327-331
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• 2001

A new soluble photosensitive poly(amide-co-imide) containing p-phenylenediacryloyl moiety was synthesized and its photoreactivity was characterized. The copolymer was synthesized fromp-phenylenediacryloyl chloride, 4,4-(hexafluoroisopropylidene)diphthalic anhydride and two equivalents of bis(4-aminophenyl) ether in NMP with a subsequent chemical imidization of the resulting poly[amide$\xi$ο-(amic acid)] by acetic anhydride and pyridine. The structure and thermal properties of the polymer were characterized by spectroscopic methods and thermal analyses. The polymer was stable up to 350$\^{C}$, showed good solubility in polar aprotic solvents, and became insoluble after UV irradiation due to the[2+2] cycloaddition of phenylenediacryloyl moiety. Photoreactivity of the polymer was investigated in solution or as a film with respect to the various exposure conditions by UV/Vis spectroscopy. The photosensitivity was noticeably increased with the irradiation temperature, especially in the presense of photosensitizer. The reason for the increased sensitivity was speculated based on the flexibilization of main chain at elevated temperature. Exposure characteristic curves were obtained from the gel fraction experiments after UV irradiation. The sensitivity and contrast at 160$\^{C}$ were measured to be 293 mJ/㎠ and 1.64, respectively.

• Macromolecular Research
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• 제8권5호
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• pp.215-223
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• 2000

A novel diamine monomer, containing fluorine and phosphine oxide, bis(3-aminophenyl) 3,5-bis(trifluoromethyl)phenyl phosphine oxide (mDA6FPPO), was prepared via Grignard reaction, and utilized to prepare polyimides with dianhydrides such as PMDA, 6FDA, BTDA or ODPA, by the conventional two-step route; preparation of poly(amic acid), followed by solution imidization. The polyimides were characterized by FT-IR, NMR, and DSC with intrinsic viscosity and refractive index also being evaluated. A phosphine oxide containing monomer, bis(3-aminophenyl)phenyl phosphine oxide (mDAPPO) and a commercial 3,3-diaminodiphenyl sulfone (mDDS) were also used for comparison. The polyimides derived from mDA6FPPO exhibited high T$\sub$g/, excellent solubility and low birefringence.

• 한국산학기술학회:학술대회논문집
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• 한국산학기술학회 2008년도 추계학술발표논문집
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• pp.343-346
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• 2008

2,2-BIs (3,4-anhydrodicarboxyphenyl)hexafluoropane(6FDA)와 4-aminophenyl sulfone(4APS), 3-aminophenyl sulfone(3APS)를 사용하여 Polyimide(PI)의 전구체인 Poly(amic acid)(PAA)를 합성하였다. 그 후 PAA의 용해도를 측정 하였다. 그리고 PAA에 열을 가하여 PI로 경화됨을 FT-IR을 이용하여 확인 하였다.

• 한국정보디스플레이학회:학술대회논문집
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• 한국정보디스플레이학회 2000년도 제1회 학술대회 논문집
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• pp.191-192
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• 2000

New copolyimides containing nitrile side group were synthesized from copolymerization of pyromellitic dianhydride, m-phenylene diamine and 3,5-diaminobenzonitrile and subsequent thermal imidization of the resulting poly(amic acid). Crystallinity, glass transition temperature and initial decomposition temperature of copolyimides were almost identical to those of homo polyimide prepared from PMDA and m-PDA. Change of pretilt angle induced by the orientation layer of resulting copolyimide was investigated by using a nitrile-containg nematic liquid crystal cell after rubbing. As the content of polar nitrile group was increased in the copolymer, pretilt angle was increased from $3.65^{\circ}$ to $6.49^{\circ}$. The mechanism of this was speculated as the dipolar interaction between the liquid crystal and nitrile groups in copolyimide.

• Elastomers and Composites
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• 제47권2호
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• pp.168-173
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• 2012

폴리아미드산을 안정제로 사용한 스티렌의 분산중합에 의해 core-shell 구조를 갖는 폴리스티렌-폴리이미드 core-shell 마이크로스피어를 얻었다. Iron pentacarbonyl을 마이크로스피어에 함침시킨 후 열분해하여 산화철 나노 입자를 갖는 자성 폴리스티렌-폴리이미드 마이크로스피어를 제조하였다. 자성 폴리스티렌-폴리이미드 마이크로스피어의 크기와 구조, 열적 특성 및 자성 특성을 조사하였는데, 자성 폴리스티렌-폴리이미드 마이크로스피어는 크기가 약 500 nm 정도로 균일하였으며 40%의 산화철 나노 입자를 가졌다. 산화철은 X선 회절시험에 의해 $Fe_3O_4$임이 확인되었다.

• Macromolecular Research
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• 제12권1호
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• pp.38-45
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• 2004

A highly flexible polyimide (PI) was synthesized successfully from ethylene glycol bis(anhydrotrimellitate) (TMEG) and 1,3-bis(4-aminophenoxy)benzene (TPER) for its application in electronics. To enhance the thermal stability and mechanical properties of this novel PI, we prepared PI nanocomposite films using nanoparticles of clays that had been treated with organic intercalating agents (organoclays). We used two types of organoclays: montmo-rillonite (MMT) treated with hexadecylamine (C$\_$16/) and MMT treated with dimethyl dihydrogenated tallow quaternary ammonium (l5A). PI/organoclay hybrid films were obtained by first preparing poly(amic acid) (PAA)/organoclay films and then converting the PAA to polyimide by thermal conversion. PAA was characterized by FT-IR and $^1$H-NMR spectroscopy and the conversion of PAA to PI was confirmed by FT-IR spectroscopy. We analyzed the dispersion of the organoclays in the PI film by X-ray diffraction. The thermal stability and mechanical properties of the hybrid films were also investigated.

• 한국산학기술학회:학술대회논문집
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• 한국산학기술학회 2006년도 추계학술발표논문집
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• pp.269-271
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• 2006

Pyromellitic anhydride(PMDA)와 4,4-Oxydianiline(ODA)로부터 Polyimide의 전구체인 Poly(amic acid)(PAA)를 합성하고, 이를 열을 가하여 Polyimide되는 반응을 적외선 분광법을 이용하여 추적하였다. 이미드화 반응은 $175^{\circ}C$에서 1시간, $185^{\circ}C$에서 1시간, $195^{\circ}C$에서 1시간, $215^{\circ}C$에서 1시간, $235^{\circ}C$에서 1시간 경화시킴으로 완결됨을 확인하였다.