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

• Polymer(Korea)
• /
• v.34 no.6
• /
• pp.495-500
• /
• 2010

Crosslinked PI films were synthesized from 4,4'-(hexafluoro isopropylidene)diphthalic anhydride (6FDA) and bis[4-(3-aminophenoxy) phenyl] sulfone(BAPS) with various ratios of the reactive monomer cis-4-cyclohexene-1,2-dicarboxylic anhydride(CDBA). We prepared crosslinked poly(amic acid) (PAA) using a 0.1 wt% Grubbs catalyst as a crosslinking agent. The crosslinked PAA was heat-treated at different temperatures to give PI films. The thermo-mechanical properties and optical transparency of the PI films were investigated. The thermal properties of the PI films were examined using Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry(DSC), thermogravimetric analysis(TGA), thermo-mechanical analysis(TMA), and universal tensile machine(UTM), and their optical transparencies were investigated using UV-vis. spectrophotometry. The thermomechanical properties of the PI films improved with increasing CDBA content. However, the optical transparency of the PI films decreased slightly with increasing CDBA content.

• Polymer(Korea)
• /
• v.28 no.6
• /
• pp.494-501
• /
• 2004

A new alkali developable photosensitive poly(amic acid) (PAA-0) with transmittance at 400 nm was synthesized from cyclobutane-1,2,3,4-tetracarboxylic dianhydride, 2-(methacryloyloxy)ethyl-3,5-diamino-benzoate and 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyl disiloxane in N-methyl-2-pyrrolidinone. Photosensitivity of the PAA-0 was investigated at 365-400 nm in the presence of a photoinitiator using a high pressure mercury lamp. The photo-cured poly(amic acid) was insoluble toward aqueous 2.38 wt% tetramethylammonium hydroxide solution. Negative pattern of the PAA-0 with 25 ${\mu}{\textrm}{m}$ resolution was obtained by developing with 2.38 wt% tetramethylammonium hydroxide solution after exposure of 600 mJ/$\textrm{cm}^2$ in the presence of 2,2-dimethoxy-2-phenyl-acetophenone as a photoinitiator. The patterned poly(amic acid) was converted to polyimide by thermal curing at 25$0^{\circ}C$ for 50 min, which showed chemical resistance against photoresist stripper as well as good transmittance at 400 nm.

• Polymer(Korea)
• /
• v.37 no.4
• /
• pp.420-430
• /
• 2013

Polymer blends were prepared by solution blending poly(amic acid) (PAA) and poly(o-hydroxy amide) (PHA) having imide groups in the main chain. The polymers and their blends were characterized by using FTIR, FT NMR, DSC, TGA, SEM, XRD, UTM, and LOI. The solubility study revealed that the blends were readily soluble in aprotic solvents such as DMF, DMAc, DMSO, and NMP. The maximum weight loss of the blends occurred in the range of $578-645^{\circ}C$, and the maximum weight loss temperature increased with increasing the PHA content. The PBO/PI blends showed relatively high char yields (i.e. 56-69 wt%). The LOI values of the blends were in the range of 24.5-28.1% and increased with increasing the PHA content. The initial modulus and tensile strength of the blends increased by 57 to 121% and by 67 to 107%, respectively, compared to the values of PAA. Especially the initial modulus and tensile strength of the PHA/PAA=2/8(wt/wt) showed the highest values of 4.87 GPa and 108 MPa, respectively. The PHA domains of $0.03-0.1{\mu}m$ in their size were more or less uniformly dispersed. The interfacial adhesion between PAA and PHA was found to be good.

• Textile Coloration and Finishing
• /
• v.35 no.4
• /
• pp.221-230
• /
• 2023

Meta-aramid and polyamic acid were separated and the manufactured films were analyzed for their integration and logarithmic properties. The miscibility of meta-aramid and polyamic acid was analyzed by Fourier transform infrared spectroscopy and scanning electron microscopy. Using calorimetric analysis and differential scanning calorimetry, the storage of meta-aramid and polyamic acid, indicated on the right side of the column, was analyzed. It was confirmed that the initial thermal resistance occurs because the polyamic acid is accounted for in the meta-aramid, and the glass transition temperature and persistence phenomenon are explained.

• Elastomers and Composites
• /
• v.42 no.3
• /
• pp.177-185
• /
• 2007

Polyamic acid(PAA)/organoclay nanocomposites containing phosphorous were prepared by solution blending of phosphorylated PAA(PPAA) and organically modified montmorillonite(O-MMT) as a type of layered clays. The nanocomposites were characterized by FT-IR, DSC, TGA, PCFC, SEM, and XRD. The preparation of nanocomposites was confirmed by FT-IR and XRD. SEM pictures showed that the organoclay was dispersed well in the PAA matrix relatively. XRD results indicated that the O-MMT layers were intercalated. The thermal stability and flame retardancy of O-MMT/PPAA nanocomposites were higher than those of pure PAA. PCFC results also showed that the heat release capacity and total heat release values of O-MMT 4 wt%/PPAA-0.2, 0.4, 0.6 composites were decreased with increasing the mole ratio of phosphorous. It was found that the nanocomposite films had the potential to be used as a fire safe material.

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

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

• Journal of Adhesion and Interface
• /
• v.10 no.2
• /
• pp.98-105
• /
• 2009

Poly(amic acid) was synthesized from the reaction of p-PDA/ODA and PMDA/BPDA and silane oligomer containing epoxy group was also synthesized from the reaction of tetramethylorthosilicate (TMOS) and glycidol. After hybridizing poly (amic acid) and silane oligomer, they were effectively converted into polyimide/silica hybrid films by thermal imidization process. As the silica contents in hybrid films increased, CTE values decreased from 17 ppm/K to 10 ppm/K and the tensile modulus increased, in spite of decreasing tensile strength. In addition, the peel test showed that the adhesion strength of hybrid film was enhanced from $0.43kg_f/cm$ to $1.02kg_f/cm$. Therefore, it could be concluded that the polyimide/silica hybrid film is effective to enhance adhesion strength for FCCL films.

• Polymer(Korea)
• /
• v.34 no.5
• /
• pp.480-484
• /
• 2010

A series of poly(amic acid)s(PAAs) was prepared by reacting 4,4'-(4,4'-isopropylidenediphenoxy) bis(phthalic anhydride)(BPADA) as the anhydride monomer and 2,2'-bis(trifluoromethyl) benzidine (TFB), bis(3-aminophenyl)sulfone (APS), 4,4'-methylenebis-(2-methylcyclohexylamine) (MMCA), or bis[4-(3-aminophenoxy) phenyl] sulfone (BAPS) as the amine monomer with 5 mol% melamine in N,N-dimethylacetamide (DMAc). Colorless and transparent polyimide (PI) films were obtained by casting the PAAs at various heat treatment temperatures. The thermo-mechanical properties and optical transparency of the PI films were investigated. The thermal properties of the PI films were examined using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and thermomechanical analysis (TMA), and their optical transparency were measured by spectrophotometry. The coefficient of thermal expansion (CTE) and yellow index (YI) values of all samples were in the range of $48.53-64.24ppm/^{\circ}C$ and < 3.0, respectively.