• 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.

• Polymer(Korea)
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• v.36 no.4
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• pp.448-454
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• 2012

A poly(amic acid) (PAA) was prepared by reaction of 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluropropane (BAPP) in N,N-dimethylacetamide (DMAc). The cast films of the synthesized PAA were thermally treated at different temperatures to create polyimide (PI) films. The heat treatment temperature varied between 80 and $230^{\circ}C$ to investigate the imidization index in relation with the solvent evaporation rates. The progress of PAA imidization was examined using a thermogravimetric analyzer (TGA) and a Fourier transform infrared spectroscope (FTIR) at various time and temperature. The experimental results showed that the imidization index was fast at the initial stage in the presence of solvent, DMAc, reaching the final imidization. When the imidization temperature is high over $200^{\circ}C$, the imidization index decreased because the solvent was evaporated too fast.

• Macromolecular Research
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• v.9 no.6
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• pp.303-312
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• 2001

The fabrication of liquid crystal display (LCD) panels involves several thermal processes such as imidization of the alignment layer (AL) and annealing of the rubbed polyimide AL. The nature of these processes on the LC alignment, especially on the pretilt angle (Θ$\_$p/) has been systematically studied, employing various types of polyimide structures. The imidization effect depends on the nature of polyimid precursors; Θ$\^$p/ increases with the degree of the imidization for the main-chain type of ALs, due to the decrease in the surface polarity, but this relation is not applicable to the alkylated ones in which the steric effect at the AL surface by the aliphatic side chains is dominant. Annealing of the rubbed polyimide AL deteriorates its rubbing-induced molecular orientation and subsequently the overlying LC alignment, resulting in the decrease in Θ$\_$p/. Especially, annealing of the LC cell affects the LC-AL interaction as well as the AL orientation and thus its effect on LC alignment depends sensitively on the nature of LC-polyimide interface; aromatic moiety in the polyimide structure gives better thermal stability of LC alignment while fluorinated polyimide ALs induce the less stable alignment.

• Macromolecular Research
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• v.11 no.5
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• pp.297-302
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• 2003

The imidization and cure reaction of a thermosetting phenylethynyl-terminated amic acid (LaRC PETI-5) in film form have been monitored as a function of temperature by means of a steady-state fluorescence technique using a front-face illumination method. The variation of the fluorescence emission spectra of LaRC PETI-5 can be divided into four temperature regions; Region I: below 15$0^{\circ}C$, Region II: 150-25$0^{\circ}C$, Region III: 250-35$0^{\circ}C$, and Region IV: above 35$0^{\circ}C$. The fluorescence spectra in Region I are largely influenced by residual N-methyl-2pyrrolidinone in the polymer and also slightly by partial imidization of the polymer. There is a combined effect of imidization and solvent removal on the fluorescence behavior in Region II. The spectra in Regions III and IV are due significantly to the cure reaction of LaRC PETI-5 and to a post-cure effect of the polyimide, respectively. This spectroscopic evidence indicating the transformation of the amic acid imide oligomer into the corresponding polyimide via imidization and cure, agrees well with thermal analysis results obtained previously. The intermediate stage of cure in the range of 250-30$0^{\circ}C$ predominantly influences the change of the fluorescence intensity. The later stage above 30$0^{\circ}C$ significantly influences the position of the spectrum. This fluorescence study also supports the mechanism proposed in earlier work that the crosslinking reaction takes place at the reaction sites in the conjugated polyene and the phenylethynyl end group in the polyimide chain.

• 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 Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1995.05a
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• pp.111-114
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• 1995

This paper describes the imidization of PAAS(polyamic acid alkylamine salts) Langmuir-Blodgett (LB) films and the electrical properties of PAAS and polyimide(PI) LB films, The imidization conditons were investigated by TGA(Thermal Gravi-tational Analysis). FT-IR and UV/ visible absorption spectra. A thermal imidiczation was peformed at 300$^{\circ}C$ for 1 hour. The electrical properties of the PAAS and polymide LB films were measured by current-voltate(L-V) characteristics It shows that the electrical condcutivity of PL LB films is about 10 $\^$-15/S/cm which is two orders of magnetiude lower than that of the PAAS LB films A Schottky effect was also observed in both films.

• Journal of the Korean Graphic Arts Communication Society
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• v.15 no.2
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• pp.117-130
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• 1997

Studies have been conducted to explore thermal imidization of polyamic acid. Aromatic polyimides are well recognized as high temperature linear polymers, and polyimide are used as structural materials, fibers, and adhesive. Two different kinds of polyimide were prepared by theimidization of polyamic acid which were synthesized from 2,2-bis[4-(4-aminophenoxy)phenyl]- hexafluoropropane, 2,2-bis [4-(4-aminophenxy)phenyl] - hexamethylpropane and caprolactam and pyromelliti dianhydride under N-Methly-pyrrolidinone solvent. Polyamic acids were converted to polyimides containing imide bond by thermal imidization. The weight 50% loss temperatures of polyimide by TGA thermogram were recorded in the range of 700 ~ 720$^{\circ}$C in nitrogen gas. According, as a results, we conclued polyamic acid were cycliation after H2O molecule separationed, and this polyimide film could be used for Printed Circuit Boand.

• Proceedings of the Materials Research Society of Korea Conference
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• 2001.05a
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• pp.125-125
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• 2001

• Proceedings of the Korean Fiber Society Conference
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• 2001.04a
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• pp.43-46
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• 2001

• 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.