Thermosetting Polyimides with Improved Impact Toughness and Excellent Thermal and Thermo-Oxidative Stability

2001 ◽  
Vol 13 (4) ◽  
pp. 287-299 ◽  
Author(s):  
T J Xiao ◽  
S Q Gao ◽  
A J Hu ◽  
X C Wang ◽  
S Y Yang

Thermoset polyimides were prepared by thermally curing B-staged endcapped polyimide resins that were obtained by thermally baking PMR polyimide matrix resins. The polyimide matrix resins were prepared by incorporating flexible ether-bridged aromatic segments [–Ar–O–Ar–] into PMR polyimide backbone to improve their processability and impact toughness. Experimental results indicated that the B-staged polyimide resins possessed adjustable and easily controllable thermal processability which ensure that thermoset polyimides are produced with improved impact strength and high glass transition temperature compared with PMR-15. Thermal and thermo-oxidative stability as well as hygrothermal resistance of the thermoset polyimides were also systemically investigated.

Author(s):  
M. I. Valueva ◽  
I. V. Zelenina ◽  
M. A. Zharinov ◽  
M. A. Khaskov

The article presents results of studies of experimental carbon plastics based on thermosetting PMRpolyimide binder. Сarbon fiber reinforced plastics (CFRPs) are made from prepregs prepared by melt and mortar technologies, so the rheological properties of the polyimide binder were investigated. The heat resistance of carbon plastics was researched and its elastic-strength characteristics were determined at temperatures up to 320°С. The fundamental possibility of manufacturing carbon fiber from prepregs based on polyimide binder, obtained both by melt and mortar technologies, is shown. CFRPs made from two types of prepregs have a high glass transition temperature: 364°C (melt) and 367°C (solution), with this temperature remaining at the 97% level after boiling, and also at approximately the same (86–97%) level of conservation of elastic strength properties at temperature 300°С.


Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1734
Author(s):  
Erick Franieck ◽  
Martin Fleischmann ◽  
Ole Hölck ◽  
Larysa Kutuzova ◽  
Andreas Kandelbauer

We report on the cure characterization, based on inline monitoring of the dielectric parameters, of a commercially available epoxy phenol resin molding compound with a high glass transition temperature (>195 °C), which is suitable for the direct packaging of electronic components. The resin was cured under isothermal temperatures close to general process conditions (165–185 °C). The material conversion was determined by measuring the ion viscosity. The change of the ion viscosity as a function of time and temperature was used to characterize the cross-linking behavior, following two separate approaches (model based and isoconversional). The determined kinetic parameters are in good agreement with those reported in the literature for EMCs and lead to accurate cure predictions under process-near conditions. Furthermore, the kinetic models based on dielectric analysis (DEA) were compared with standard offline differential scanning calorimetry (DSC) models, which were based on dynamic measurements. Many of the determined kinetic parameters had similar values for the different approaches. Major deviations were found for the parameters linked to the end of the reaction where vitrification phenomena occur under process-related conditions. The glass transition temperature of the inline molded parts was determined via thermomechanical analysis (TMA) to confirm the vitrification effect. The similarities and differences between the resulting kinetics models of the two different measurement techniques are presented and it is shown how dielectric analysis can be of high relevance for the characterization of the curing reaction under conditions close to series production.


2007 ◽  
Vol 15 (5) ◽  
pp. 343-355 ◽  
Author(s):  
S. Lipponen ◽  
P. Pietikäinen ◽  
U. Vainio ◽  
R. Serimaa ◽  
J.V. Seppälä

Ethylene/1,7-octadiene copolymer was polymerised with metallocene catalyst and hydrosilylated to form silane functionalised polyethylenes (PE-co-SiX, X=Cl, OEt, Ph). The functionalised species were tested as modifiers in composites of rubber toughened polypropylene (heterophasic PP, hPP) and microsilica filler (μSi). A metallocene-based functionalised PE (PE-co-SiF) produced earlier in our laboratory and three commercial grades of functionalised polyolefins (one PE- and two PP-based) were used as reference modifiers. Major differences were seen in the toughness of the composites both above and below the glass transition temperature (Tg) of PP. In addition to increasing the stiffness, the microsilica filler enhanced the toughness of the heterophasic polypropylene by over 200% at ambient temperature. Below the Tg of PP (at −20 °C), the influence of μSi was the opposite and the impact strength of the hPP/μSi composite was below that of unfilled hPP. With the addition of just 2 wt% of functionalised polyethylene, the poor cold toughness of hPP/μSi composite was improved by nearly 100%. With the same addition, the toughness of the composites at ambient temperature was improved by 50 to 100% compared with the unfilled hPP. This behaviour was explained by significant changes in the fracture mechanism. Addition of functionalised PE increased the concentration of microsilica in the rubbery phase, allowing the crack to enter that phase. The rubbery phase was also able to absorb a large amount of impact energy below the glass transition temperature of PP.


1998 ◽  
Vol 10 (3) ◽  
pp. 273-283 ◽  
Author(s):  
J W Connell ◽  
J G Smith ◽  
P M Hergenrother

As part of a programme to develop high-performance/high-temperature structural resins for aeronautical applications, imide oligomers containing pendent and terminal phenylethynyl groups were prepared, characterized and the cured resins evaluated as composite matrices. The oligomers were prepared at a calculated number-average molecular weight of 5000 g mol−1 and contained 15–20 mol% pendent phenylethynyl groups. In previous work, an oligomer containing pendent and terminal phenylethynyl groups exhibited a high glass transition temperature (∼313 °C), and laminates therefrom exhibited high compressive properties, but processability, fracture toughness, microcrack resistance and damage tolerance were less than desired. In an attempt to improve these deficiencies, modifications in the oligomeric backbone involving the incorporation of 1,3-bis(3-aminophenoxy)benzene were investigated as a means of improving processability and toughness without detracting from the high glass transition temperature and high compressive properties. The amide acid oligomeric solutions were prepared in N-methyl-2-pyrrolidinone and were subsequently processed into imide powder, thin films, adhesive tape and carbon fibre prepreg. Neat resin plaques were fabricated from imide powder by compression moulding. The maximum processing pressure was 1.4 MPa and the cure temperature ranged from 350 to 371 °C for 1 h for the mouldings, adhesives, films and composites. The properties of the 1,3-bis(3-aminophenoxy)benzene modified cured imide oligomers containing pendent and terminal phenylethynyl groups are compared with those of previously prepared oligomers containing pendent and terminal phenylethynyl groups of similar composition and molecular weight.


2011 ◽  
Vol 2011 (HITEN) ◽  
pp. 000196-000200 ◽  
Author(s):  
Kenji Okamoto ◽  
Yuji Takematsu ◽  
Miyako Hitomi ◽  
Yoshinari Ikeda ◽  
Yoshikazu Takahashi

There is a demand to improve the thermal stability of epoxy molding resins used in the power module of SiC power chips operating at temperatures of 200°C or more. This paper describes a technique for increasing the thermal stability of the resin by decreasing molecular motion through the addition of nanofiller. The experimental results showed that the glass transition temperature (Tg) of the epoxy resin increased by approximately 30°C when the silica nanofiller was added. The epoxy resin added nanofiller was investigated in order to achieve the operation temperature 200°C of power module.


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