The 3D orthogonal woven basalt fiber reinforced polyimide (PI) composites were fabricated and characterized in this study. The PI film was firstly prepared to determine PI processing parameters. Fourier transform infr...The 3D orthogonal woven basalt fiber reinforced polyimide (PI) composites were fabricated and characterized in this study. The PI film was firstly prepared to determine PI processing parameters. Fourier transform infrared (FTIR) analysis showed that 300°C was the suitable imidization temperature. Thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) results showed relatively good thermal properties of the PI film. In the fabrication of composites, the multi-step impregnation method was applied. The bending properties of 3 mm-thick composite showed increasing trend in all and the second-time impregnated composite had much higher value than the first-time impregnated composite. Moreover, the bending fracture mode photos showed obvious creases except for the first-time impregnated materials, which agreed well with the bending property values. The dielectric constants for the composites were complex because they had not regular value following the mixing rule of the composites, which was mainly due to the interfacial polarization and other effects in the fabrication processing.展开更多
In order to improve the processibility in thermoplastic polyimides, a new method, termed the'reactive plasticizer' approach, has been proposed. This method uses a small amount (5～15 mol%) of a lessactivated, ...In order to improve the processibility in thermoplastic polyimides, a new method, termed the'reactive plasticizer' approach, has been proposed. This method uses a small amount (5～15 mol%) of a lessactivated, weak nucleophilic diamine co-monomer as a 'reactive plasticizer' to obtain copolyimide resinswhich possess relatively low viscosity at low temperatures and can be readily processed through the autoclavecycle at low pressures. During a high temperature treatment, the reactive plasticizers join the reaction to formhigh molecular weight copolyimides, and the preferred material properties are thus achieved. The mosteffective reactive plasticizer is aromatic heterocyclic diamines, such as 2, 6-diaminopyridine diamine (DAP),and the transimidization involved with a reactive plasticizer has been proposed to play a major role for thesuccess of this approach. In order to understand the transimidization mechanism, three steps have been takenin this research: first, a copolyimide system of 50% of DAP and 50% 1, 4 -bis [4-aminophenoxy] benzenediamine (DODA) with 100% of 2, 2'-bis[4-(3, 4-dicarboxyphenoxy)phenyl] propane dianhydride (Ultem^(R)DA) is prepared. Second, several specifically designed polyimide mixture systems were used, and they consistof two homopolyimides: one is Ultem^(R) DA-DODA, and the other is Ultem^(R) DA-DAP. The third step is toinvestigate two mixture systems in which Ultem^(R) DA-DODA is mixed with DAP monomer solution andUltem^(R) DA-DAP is mixed with DODA monomer solution. For all systems, with increasing degree oftransimidization upon heat-treatment, the chain structures of the mixtures and their thermal and dynamicmechanical transition behaviors are investigated via one-dimensional and two-dimensional nuclear magneticresonance, differential scanning calorimetry, and dynamic mechanical analysis experiments. Experimentalresults indicate that in the mixture of two homopolyimides, transimidization takes place much moreefficiently in solution than in the melt. For the two mixtures with monomer solutions, the transimidizationcan only be found in the mixture of Ultem^(R) DAP/DODA system in p-chlorophenol, and this process does noteffectively occur in the Ultem^(R) DODA/DAP system in p-chlorophenol, indicating that free DODA canefficiently attack the imide linkage of Ultem^(R) DA-DAP. The final product resulting from the transimidizationin the mixtures is a random copolyimide with a major population of DAP as end groups for the copolymersystem.展开更多
文摘The 3D orthogonal woven basalt fiber reinforced polyimide (PI) composites were fabricated and characterized in this study. The PI film was firstly prepared to determine PI processing parameters. Fourier transform infrared (FTIR) analysis showed that 300°C was the suitable imidization temperature. Thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) results showed relatively good thermal properties of the PI film. In the fabrication of composites, the multi-step impregnation method was applied. The bending properties of 3 mm-thick composite showed increasing trend in all and the second-time impregnated composite had much higher value than the first-time impregnated composite. Moreover, the bending fracture mode photos showed obvious creases except for the first-time impregnated materials, which agreed well with the bending property values. The dielectric constants for the composites were complex because they had not regular value following the mixing rule of the composites, which was mainly due to the interfacial polarization and other effects in the fabrication processing.
基金This work was supported by the Center of Molecular and Microstructure Composites(CMMC)of NSF/Ohio State/Industries and the NSF DMR(96-17030)
文摘In order to improve the processibility in thermoplastic polyimides, a new method, termed the'reactive plasticizer' approach, has been proposed. This method uses a small amount (5～15 mol%) of a lessactivated, weak nucleophilic diamine co-monomer as a 'reactive plasticizer' to obtain copolyimide resinswhich possess relatively low viscosity at low temperatures and can be readily processed through the autoclavecycle at low pressures. During a high temperature treatment, the reactive plasticizers join the reaction to formhigh molecular weight copolyimides, and the preferred material properties are thus achieved. The mosteffective reactive plasticizer is aromatic heterocyclic diamines, such as 2, 6-diaminopyridine diamine (DAP),and the transimidization involved with a reactive plasticizer has been proposed to play a major role for thesuccess of this approach. In order to understand the transimidization mechanism, three steps have been takenin this research: first, a copolyimide system of 50% of DAP and 50% 1, 4 -bis [4-aminophenoxy] benzenediamine (DODA) with 100% of 2, 2'-bis[4-(3, 4-dicarboxyphenoxy)phenyl] propane dianhydride (Ultem^(R)DA) is prepared. Second, several specifically designed polyimide mixture systems were used, and they consistof two homopolyimides: one is Ultem^(R) DA-DODA, and the other is Ultem^(R) DA-DAP. The third step is toinvestigate two mixture systems in which Ultem^(R) DA-DODA is mixed with DAP monomer solution andUltem^(R) DA-DAP is mixed with DODA monomer solution. For all systems, with increasing degree oftransimidization upon heat-treatment, the chain structures of the mixtures and their thermal and dynamicmechanical transition behaviors are investigated via one-dimensional and two-dimensional nuclear magneticresonance, differential scanning calorimetry, and dynamic mechanical analysis experiments. Experimentalresults indicate that in the mixture of two homopolyimides, transimidization takes place much moreefficiently in solution than in the melt. For the two mixtures with monomer solutions, the transimidizationcan only be found in the mixture of Ultem^(R) DAP/DODA system in p-chlorophenol, and this process does noteffectively occur in the Ultem^(R) DODA/DAP system in p-chlorophenol, indicating that free DODA canefficiently attack the imide linkage of Ultem^(R) DA-DAP. The final product resulting from the transimidizationin the mixtures is a random copolyimide with a major population of DAP as end groups for the copolymersystem.
