Isothermal DSC Study of the Curing Kinetics of an Epoxy/Silica Composite for Microelectronics

2017 ◽  
Vol 14 (2) ◽  
pp. 45-50 ◽  
Author(s):  
Lérys Granado ◽  
Stefan Kempa ◽  
Stefanie Bremmert ◽  
Laurence J. Gregoriades ◽  
Frank Brüning ◽  
...  

Abstract Curing kinetics of an industrially important printed-circuit board (PCB) base material (epoxy–phenol/glass fillers) were studied by isothermal differential scanning calorimetry (DSC) measurements between 150 and 190°C, as relevant curing temperatures for the PCB industry. The extent of cure was calculated by integration of the exothermic peak and normalization by the total heat of reaction (obtained by nonisothermal DSC). Although the cross-linking was completed above 180°C, the kinetic profiles show two regimes: one fast and one slow. The kinetic parameters have been elucidated using an isoconversional model-free kinetic method, with the exact method of Friedman, to give to the PCB manufacturers a road map to predict curing behavior of base material. The linearity of Arrhenius plots was satisfactory. The apparent activation energy of curing reaction has been found to increase with the degree of conversion. The elucidation of the kinetic parameters allows us to propose an accurate and predictive description of the curing kinetics within the fast regimen of reaction (i.e., without vitrification). Finally, we discuss how these kinetic measurements and models can be completed and optimized.

2016 ◽  
Vol 2016 (1) ◽  
pp. 000415-000420 ◽  
Author(s):  
Lérys Granado ◽  
Stefan Kempa ◽  
Stefanie Bremmert ◽  
Laurence J. Gregoriades ◽  
Frank Brüning ◽  
...  

Abstract Curing kinetics of an industrially important printed-circuit board (PCB) base material (epoxy-phenol/glass fillers) were studied from isothermal differential scanning calorimetry (DSC) measurements between 150 and 190 °C. The extent of cure was calculated by integration of the exothermic peak and normalization by the total heat of reaction (obtained by non-isothermal DSC). The kinetic profiles show two regimes: one fast, and one slower. The completion was reached above 180 °C. The kinetic parameters have been elucidated using an isoconversional model-free kinetic method. The linearity of Arrhenius plots was satisfactory. The apparent activation energy of curing reaction has been found to increase with the degree of conversion. The elucidation of the kinetic parameters allows us to propose an accurate and predictive description of the curing kinetics of the composite until a degree of conversion of 50%. Finally, we discuss how these kinetic measurements and models can be completed and optimized.


2014 ◽  
Vol 988 ◽  
pp. 31-35
Author(s):  
Jia Le Song ◽  
Chan Chan Li ◽  
Zhi Mi Zhou ◽  
Chao Qiang Ye ◽  
Wei Guang Li

Curing kinetics of MEP-15/593 system and MEP-15/593/660 system is studied by means of differential scanning calorimetry (DSC). Curing kinetic parameters are evaluated and the relationship between diluent 660 and the curing properties is investigated. The results show that the diluent 660 can not only reduce viscosity and activation energy, but also improve the degree of cure and conversion ratio.


2017 ◽  
Vol 30 (3) ◽  
pp. 303-311 ◽  
Author(s):  
Chao Chen ◽  
Yanxia Li ◽  
Yizhuo Gu ◽  
Min Li ◽  
Zuoguang Zhang

The curing kinetics of two different types of commercial epoxy resins were investigated by means of nonisothermal differential scanning calorimetry (DSC) in this work. The complex curve of measured heat flow of CYCOM 970 epoxy resin was simplified with the method of resolution of peak. Two typical autocatalytic curing reaction curves were gained and the kinetic parameters of the curing process were demonstrated by combination of those two reactions. The Kissinger method was adopted to obtain the values of the activation energy. The parameters of curing kinetic model were acquired according to the fitting of Kamal model. Isothermal DSC curve of CYCOM 970 epoxy resin obtained using the experimental data shows a good agreement with that theoretically calculated. Then, 603 epoxy resin was investigated by the simplified method and the kinetic parameters were received through the same procedure. The nonisothermal DSC curve tested according to the recommended cure cycle of 603 epoxy resin is also consistent with the calculated results. This improved simplified approach provides an effective method to analyze the curing kinetics of the epoxy resins with complex DSC curves as similar to this study.


Holzforschung ◽  
2019 ◽  
Vol 73 (9) ◽  
pp. 879-887 ◽  
Author(s):  
Guomin Wu ◽  
Xinhao Feng ◽  
Can Jin ◽  
Zhenwu Kong ◽  
Siqun Wang

Abstract In order to increase the curing rate of polymeric diphenylmethane diisocyanate (PMDI) resin, different contents of lignin-containing cellulose nanofibrils (L-CNFs) were blended into the PMDI. Differential scanning calorimetry (DSC) was used to examine how the addition of L-CNFs influences the curing kinetics of PMDI resin. The activation energy (Ea) of the curing reaction of PMDI/L-CNF systems was calculated using the Kissinger, Friedman and Flynn-Wall-Ozawa model-free methods. The results showed that Ea values calculated by the aforementioned three methods varied in a similar trend with the increase in the L-CNF content. Adding L-CNFs could decrease the Ea value of the curing reaction of PMDI and speed up the curing reaction. The acceleration of the cure rate of the PMDI resin upon the addition of L-CNFs may be attributable to the effective dispersion of the L-CNFs into the PMDI resin as well as the reaction between the hydroxyl (-OH) groups of the L-CNFs and the isocyanate (-NCO) groups of the PMDI.


2018 ◽  
Vol 7 (1) ◽  
pp. 21-30 ◽  
Author(s):  
Norbert Halmen ◽  
Christoph Kugler ◽  
Eduard Kraus ◽  
Benjamin Baudrit ◽  
Thomas Hochrein ◽  
...  

Abstract. The degree of cross-linking and curing is one of the most important values concerning the quality of cross-linked polyethylene (PE-X) and the functionality of adhesives and resin-based components. Up to now, the measurement of this property has mostly been time-consuming and usually destructive. Within the shown work the feasibility of single-sided nuclear magnetic resonance (NMR) for the non-destructive determination of the degree of cross-linking and curing as process monitoring was investigated. First results indicate the possibility of distinguishing between PE-X samples with different degrees of cross-linking. The homogeneity of the samples and the curing kinetics of adhesives can also be monitored. The measurements show good agreement with reference tests (wet chemical analysis, differential scanning calorimetry, dielectric analysis). Furthermore, the influence of sample temperature on the characteristic relaxation times can be observed.


2010 ◽  
Vol 160-162 ◽  
pp. 1712-1715
Author(s):  
Guang Heng Wang

The polymerization reaction kinetics of biodegradable polyurethane extended with soy protein isolate (SPI) with dibutyltin dilaurate (DBTDL) as the curing catalyst was studied by means of non-isothermal differential scanning calorimetry (DSC). Model-free methods, Kissinger method and Ozawa method, were applied for analyzing the DSC data. The Ea and lnA obtained from Kissinger method for catalyzed reaction between toluene diisocyanate (TDI) and Polyoxypropyleneglycol (PPG) are 60.80 kJ•mol-1 and 12.09, and for catalyzed reaction among TDI, PPG, and SPI they were 65.91 kJ•mol-1and 14.04. Similarly the Ea obtained from Ozawa method for catalyzed reaction between TDI and PPG and catalyzed reaction among TDI, PPG, and SPI were 63.49 kJ•mol-1 and 64.78 kJ•mol-1, respectively. The results showed that, the incorporation of a small amount of SPI into polyurethane did not affect the reaction kinetic strongly, but increases the reaction activation energy Ea and lnA.


2011 ◽  
Vol 525 (1-2) ◽  
pp. 31-39 ◽  
Author(s):  
Jintao Wan ◽  
Zhi-Yang Bu ◽  
Cun-Jin Xu ◽  
Hong Fan ◽  
Bo-Geng Li

Energies ◽  
2019 ◽  
Vol 12 (15) ◽  
pp. 2981 ◽  
Author(s):  
Larissa Fedunik-Hofman ◽  
Alicia Bayon ◽  
Scott W. Donne

Reaction kinetics is an important field of study in chemical engineering to translate laboratory-scale studies to large-scale reactor conditions. The procedures used to determine kinetic parameters (activation energy, pre-exponential factor and the reaction model) include model-fitting, model-free and generalized methods, which have been extensively used in published literature to model solid-gas reactions. A comprehensive review of kinetic analysis methods will be presented using the example of carbonate looping, an important process applied to thermochemical energy storage and carbon capture technologies. The kinetic parameters obtained by different methods for both the calcination and carbonation reactions are compared. The experimental conditions, material properties and the kinetic method are found to strongly influence the kinetic parameters and recommendations are provided for the analysis of both reactions. Of the methods, isoconversional techniques are encouraged to arrive at non-mechanistic parameters for calcination, while for carbonation, material characterization is recommended before choosing a specific kinetic analysis method.


Sign in / Sign up

Export Citation Format

Share Document