• Korea-Australia Rheology Journal
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• v.12 no.1
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• pp.69-76
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• 2000

We have derived the translation diffusion coefficient and the intrinsic viscosity formula adopting the Kholodenko's theory using 3＋1 dimensional Dirac propagator in the Kirkwood and Riseman scheme. We also performed static light scattering experiments and intrinsic viscosity measurement of dilute solutions of polyimides with different rigidities. In the framework of Kholodenko's theory, we can easily measure the persistence length of polyimide. We prepared five different polyamic acids and polyimides with different degree of imidization by controlling imidization temperatures. From experimental results, we obtained molecular weights and persistence lengths according to the Kholodenko's plot. The molecular weight and the intrinsic viscosity decreased and then increased with the imidization temperature but the persistence length increased monotonically and then leveled off. The persistence lengths calculated from intrinsic viscosities showed very good agreement with those from light scattering experiments.

• Bulletin of the Korean Chemical Society
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• v.24 no.3
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• pp.357-362
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• 2003

The pathway producing imide ring closure during the thermal imidization of poly(amic acid) (PAA) was investigated in detail using a new analytical method, two-dimensional (2D) Raman correlation spectroscopy. The signs of the cross peaks in synchronous spectra provided evidence of the thermal imidization of PAA into PI as the heating temperature increased. The signs of the cross peaks in asynchronous spectra suggested that the imide-related modes changed prior to the amide or carboxylic mode, which indicates that cyclization occurred before the amide proton was abstracted.

• Macromolecular Research
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• v.14 no.1
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• pp.1-33
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• 2006

Polyimides (PIs) exhibit excellent thermal stability, mechanical, dielectric, and chemical resistance properties due to their heterocyclic imide rings and aromatic rings on the backbone. Due to these advantageous properties, PIs have found diverse applications in industry. Most PIs are insoluble because of the nature of the high chemical resistance. Thus, they are generally used as a soluble precursor polymer, which forms complexes with solvent molecules, and then finally converts to the corresponding polyimides via imidization reaction. This complexation with solvent has caused severe difficulty in the characterization of the precursor polymers. However, significant progress has recently been made on the detailed characterization of PI precursors and their imidization reaction. On the other hand, much research effort has been exerted to reduce the dielectric constant of PIs, as demanded in the microelectronics industry, through chemical modifications, as well as to develop high performance, light-emitting PIs and liquid crystal (LC) alignment layer PIs with both rubbing and rubbing-free processibility, which are desired in the flat-panel display industry. This article reviews this recent research progresses in characterizing PIs and their precursors and in developing low dielectric constant, light-emitting, and LC alignment layer PIs.

• Applied Chemistry for Engineering
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• v.10 no.7
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• pp.979-984
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• 1999

Aromatic soluble polyimides were synthesized from 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane and various dianhydrides such as pyromelltic dianhydride(PMDA), 3,3',4,4'-benzophenone tetracarboxylic dianhydride(BTDA), and 4,4'-(hexafluoroisopropylidene)-bis(phthalic anhydride)(6FDA). Polyimides prepared by thermal imidization were insoluble in common organic solvents (acetone, MNP, DMAc, DMSO, THF, and DMF) but those prepared by chemical imidization were soluble. The difference of solubility was explained by esterification between hydroxyl group and $CH_3COO^-$ from acetic anhydride used as a dehydration agent in chemical imidization. Glass transition temperatures of polyimides by thermal method were higher than those by chemical method. All of the polyimides are stable up to $300^{\circ}C$ regardless of the sample preparation. The x-ray diffraction patterns showed that all polyimides were amorphrous.

• Journal of Adhesion and Interface
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• v.5 no.1
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• pp.29-35
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• 2004

We have prepared polyster/nanQhybridized polyimide films in the range of 1~9 wt% of organophilic synthetic layered silicate (STN). Firstly, poly(amic acid)/STN nanocomposite solutions were prepared via solution blending method in DMAc or THF/MeOH solution, and then cast on the polyester film followed by imidization reaction, thermal and chemical method repestively. XRD and TEM experiment showed that the STN was fully exfoliated through the polyimide matrix. Surface morphologies of nanohybridized polyimide films were characterized by AFM and thermal, mechanical properties were also confirmed by TGA, DMA and UTM each. And also, the water vapor permeabilities highly depended on the content of STN. The sample from chemical imidization route and THF/MeOH solvent system showed better water vapor barrier properties than thermal one and DMAc system.

• Applied Chemistry for Engineering
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• v.3 no.1
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• pp.179-187
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• 1992

Poly(styrene-co-maliec anhydride) was reacted with aromatic amines such as aniline, p-toluidine, and p-chloroaniline in 10% (w/w) DMF solution to convert maleic anhydride units into maleimides. Optimum reaction conditions for cyclodehydration step of imide ring formation were : (a) reaction temp. of $80^{\circ}C$ (b) mole ratios of cyclodehydration agents : anhydride units in SMA/acetic anhydride/sodium acetate/triethyl amine= 1.0/2.0/0.2/1.1. $T_g$of SMI(imide modified SMA) was increased with increasing degree of imidization, but $T_g$leveled off in the early stage of imide content. And $T_g$of SMI was increased with the following order of amines used for imidization reagents : aniline < p-toluidine < p-chloroaniline.

• Electrical & Electronic Materials
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• v.9 no.1
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• pp.59-66
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• 1996

Polyimides containing cyclobutane ring in main chain is known to be thermally stable and able to be developed in organic solvents after photolysis with 254 nm UV light. This type of polyimides can be used as promising positive photoresist in VLSI fabrication process. In the current VLSI process, photoresist films are formed by spin coating. The film thickness is more than several hundred nano meters. It seems that there is room for improvement of film coating process by introducing Langmuir Blodgett technique. Thereby ultra thin film photoresist can be formed, and higher density of integration in VLSI be achieved. In the present work, depositing procedure of LB films of this polyimide was investigated. LB film thickness was measured by ellipsometry to evaluate deposited film status. Chemical imidization procedure was studied to avoid several problems in thermal imidization. The pattern of submicron dimension has successfully formed on LB film of 8nm thick, which found showing good contrast.

• Journal of the Korean Vacuum Society
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• v.1 no.1
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• pp.139-144
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• 1992

Abstract-Polyimide (PI) thin films were deposited by the ionized cluster beam deposition (ICBD) technique. Imidization and crystallization of PI films were investigated using transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FT-IR). PI films deposited under optimum conditions showed a maximum imidization and good crystal structure, which are superior to those of the films fabricated by other techniques.

• Proceedings of the KIEE Conference
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• 1993.11a
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• pp.174-177
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• 1993

The polyimide films were prepared by imidizing the polyamic acid long-chain alkylamine (dimethylhexadecylamine) salt films with a thermal and chemical treatment, where the polyamic acid alkylamine salt film were formed on various substrates by using Langmuir-Blodgett (LB) method. The imidization of polyamic acid alkylamine salt films with various thickness were identified with FT-IR and UV-visible absorption spectroscopies. Atomic Force Microscopy (AFM) have been used to investigate the surface morpology of polyamic acid alkylamine salt and imidized films.

• Macromolecular Research
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• v.10 no.5
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• pp.241-245
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• 2002

A new aromatic diamine monomer containing benzoxazole substituents was prepared by a multi-step synthesis starting from 1,4-dibromo-2,5-difluorobenzene. This bulky and disc-shaped monomer was polymerized with commercial dianhydride monomers to give several different poly(amic acid)s with their inherent viscosities in the range of 0.24-0.35 dL/g. The prepared polymers were soluble in typical polar aprotic solvents. Thermal imidization to the corresponding polyimides were investigated by using FT-IR, DSC and TGA.