scholarly journals Cure Kinetics Modeling of a High Glass Transition Temperature Epoxy Molding Compound (EMC) Based on Inline Dielectric Analysis

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.

Author(s):  
M. Sandor ◽  
S. Agarwal ◽  
D. Peters ◽  
M. S. Cooper

Microcircuit manufacturers of Plastic Encapsulated Microcircuits (PEM’s) have made changes in epoxy molding compound materials and chemistry, which lower Glass Transition Temperature (Tg). PEM users in harsh environments have concerns if either the part in its application, or in evaluation or assembly, is used close to, or above, the Tg. Various Tg measurement techniques are available and discussed. Test results from one technique is reviewed. The implications of the Tg results on usage of these parts in space applications will be presented. Burn-in/ reliability test results of samples with low Tg PEM’s will be presented. The reliability experiments include testing under different temperatures. The issue being addressed is whether outgassing of molding compounds occurs when the temperature of the molding compound exceeds the Tg. This is a caution noted by many vendors. As an example outgassing of flame retardants can degrade parametric performance and wire bond integrity. This would be the case when PEMS are being qualified for Space applications using burn-in or in storage environments. JPL’s past experience has shown that COTS PEMS parametrics can degrade significantly even when the burn-in temperature is well below the Tg. Two different microcircuits exhibiting low Tg were evaluated. Assessment of final electrical test measurements and yield are shown.


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.


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.


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