Estimation of Cure and Thermal Degradation Kinetics of Epoxy/Organoclay Nanocomposite

2010 ◽  
Vol 123-125 ◽  
pp. 667-670 ◽  
Author(s):  
Jae Young Lee ◽  
Bum Choul Choi ◽  
Hong Ki Lee

Polymer nanocomposite was synthesized through the intercalation and exfoliation of organoclay in an epoxy matrix. The epoxy matrix was composed of diglycidyl ether of bisphenol A (DGEBA, epoxy base resin), 4,4'-methylene dianiline (MDA, curing agent) and malononitrile (MN, chain extender) and organoclay was prepared by treating the montmorillonite with octadecyltrimethylammonium bromide (ODTMA). The intercalation of the organoclay was estimated by wide angle X-ray diffraction (WAXD) and transmission electron microscope (TEM) analyses. In order to measure the cure rate of DGEBA/MDA (30 phr)/MN (5 phr)/Organoclay (5 phr), differential scanning calorimetry (DSC) analysis were performed at the heating rates of 5, 10, 15 and 20 oC/min, and the data was interpreted by Kissinger equation. Thermal degradation kinetics of the epoxy nanocomposite was also studied by thermogravimetric analysis (TGA). The epoxy sample was decomposed in the TGA furnace at the heating rates of 5, 10, 15 and 20 oC/min with nitrogen atmosphere of 50 ml/min. The TGA data was introduced to the Ozawa equation and the degradation activation energy was calculated according to the degradation ratio. The activation energy for cure kinetics was 43.3 kJ/mol and that for thermal degradation was 171.5 kJ/mol.

2012 ◽  
Vol 486 ◽  
pp. 27-33 ◽  
Author(s):  
Jae Young Lee ◽  
Sung Wan Hong ◽  
Kyeong Sik Han ◽  
Taeck Hong Lee ◽  
Hong Ki Lee

Palladium (Pd) nanoparticles were incorporated into a nylon 6 film via a dry process which consisted of simultaneous vaporization, penetration and reduction processes of palladium (II) bis (acetylacetonate, Pd (acac)2) at 180°C for various exposure time. The even dispersion of the generated Pd nanoparticles were observed by transmission electron microscope (TEM) and the Pd loading weight of about 15~43 wt% was measured by thermogravimetric analysis (TGA). In order to study the catalytic effect of Pd nanoparticles on the thermal degradation kinetics of nylon 6, TGA data at various heating rates were introduced to Flynn & Wall equation. The thermal degradation activation energy for neat nylon 6 was ca. 162~178 kJ/mol over the thermal degradation fraction of 0.05~0.40 while that of the nylon 6/Pd (26.5 wt%) nanocomposite was ca. 110~169 kJ/mol over the same fraction range. It meant the Pd nanoparticles were acted as a catalyst on the depolymerization of amide group in nylon 6. It was also found that the activation energy decreased slightly with the increasing Pd loading weight.


2018 ◽  
Vol 39 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Dev K. Mandal ◽  
Haripada Bhunia ◽  
Pramod K. Bajpai

AbstractIn this article, the influence of polylactide and pro-oxidant on the thermal stability, degradation kinetics, and lifetime of polypropylene has been investigated using thermogravimetric analysis under nitrogen atmosphere at four different heating rates (i.e. 5, 10, 15, and 20°C/min). The kinetic parameters of degradation were studied over a temperature range of 30–550°C. The derivative thermogravimetric curves have indicated single stage and two stage degradation processes. The activation energy was evaluated by using the Kissinger, Kim-Park, and Flynn-Wall methods under the nitrogen atmosphere. The activation energy value of polypropylene was much higher than that of polylactide. Addition of polylactide and pro-oxidant in polypropylene decreased the activation energy. The lifetime of polypropylene has also decreased with the addition of polylactide and pro-oxidant.


Coatings ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 871
Author(s):  
Maryam Jouyandeh ◽  
Behzad Shirkavand Hadavand ◽  
Farimah Tikhani ◽  
Reza Khalili ◽  
Babak Bagheri ◽  
...  

In the present study, thermal degradation kinetics of polyurethane (PU) powder coatings reinforced with organo-modified montmorillonite (OMMT) was investigated. PU nanocomposites were prepared in different concentrations of 1, 3, and 5 wt.% of OMMT via the extrusion method. The microstructure of the nanocomposites was observed by scanning electron microscope (SEM) illustrating uniform dispersion of OMMT nano-clay platelets in the PU matrix except for the sample containing 5 wt.% nano-palates. Thermal degradation kinetics of the PU nanocomposite was investigated using thermogravimetric analysis (TGA) at different heating rates of 5, 10, and 20 °C/min. The results showed that the initial decomposition temperatures were shifted toward higher values (more than 40 °C for T5% and up to 20 °C for T10%) by introducing the nano-clay to the PU matrix. Friedman, Kissinger–Akahira–Sunose (KAS), Flynn–Wall–Ozawa (FWO), and modified Coats-Redfern iso-conversional methods were applied to model the decomposition reaction and the activation energy of the nanocomposite powder coatings. Overall, the presence of nano-clay increased the activation energy of the PU degradation up to 45 kJ/mol, when compared to the blank PU, which suggests very high thermal stability of nanocomposites. The Sestak-Berggren approach proposed a good approximation for the reaction model, especially at low temperatures. Thus, PU decomposition was detected as an autocatalytic reaction, which was suppressed by the barrier effect of OMMT nano-palates intercalated with polymer chains.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Ali Kuliaei ◽  
Iraj Amiri Amraei ◽  
Seyed Rasoul Mousavi

Abstract The purpose behind this research was to determine the optimum formulation and investigate the cure kinetics of a diglycidyl ether of bisphenol-A (DGEBA)-based epoxy resin cured by dicyandiamide and diuron for use in prepregs. First, all formulations were examined by the tensile test, and then, the specimens with higher mechanical properties were further investigated by viscometry and tack tests. The cure kinetics of the best formulation (based on tack test) in nonisothermal mode was investigated using differential scanning calorimetry at different heating rates. Kissinger and Ozawa method was used for determining the kinetic parameters of the curing process. The activation energy obtained by this method was 71.43 kJ/mol. The heating rate had no significant effect on the reaction order and the total reaction order was approximately constant ( m + n ≅ 2.1 $m+n\cong 2.1$ ). By comparing the experimental data and the theoretical data obtained by Kissinger and Ozawa method, a good agreement was seen between them. By increasing the degree of conversion, the viscosity decreased; as the degree of conversion increased, so did the slope of viscosity. The results of the tack test also indicated that the highest tack could be obtained with 25% progress of curing.


2017 ◽  
Vol 30 (7) ◽  
pp. 787-793 ◽  
Author(s):  
Xu Su ◽  
Yong Xu ◽  
Linshuang Li ◽  
Chaoran Song

Two kinds of thermoplastic polyimides (PIs) were synthesized via a two-step method with 2,2-bis[4-(4-aminophenoxy)phenyl]propane (BAPP), 4,4′-oxydianiline (ODA) diamine, and 3,3′,4,4′-benzophenonetetracarboxylic dianhydride (BTDA), and their thermal degradation kinetics was studied by thermogravimetric analysis at different heating rates under nitrogen. Derivative thermogravimetric analysis curves indicated a simple, single-stage degradation process in PI BTDA-BAPP and a two-stage degradation process in PI BTDA-ODA-BAPP. The activation energies ( Eas) of the thermal degradation reaction were determined by the Flynn–Wall–Ozawa and Kissinger–Akahira–Sunose methods without a knowledge of the kinetic reaction mechanism. By comparing the values of Ea and weight loss temperatures, it was demonstrated that the thermal stability of PI BTDA-ODA-BAPP was superior to that of PI BTDA-BAPP.


e-Polymers ◽  
2017 ◽  
Vol 17 (5) ◽  
pp. 373-381 ◽  
Author(s):  
Xinxin Cao ◽  
Mengqi Wu ◽  
Aiguo Zhou ◽  
You Wang ◽  
Xiaofang He ◽  
...  

AbstractA novel two-dimensional material MXene was used to synthesize nanocomposites with linear low-density polyethylene (LLDPE). The influence of MXene on crystallization and thermal degradation kinetics of LLDPE was investigated. Non-isothermal crystallization kinetics was investigated by using differential scanning calorimetry (DSC). The experimental data was analyzed by Jeziorny theory and the Mo method. It is found that MXene acted as a nucleating agent during the non-isothermal crystallization process, and 2 wt% MXene incorporated in the nanocomposites could accelerate the crystallization rate. Findings from activation energy calculation for non-isothermal crystallization came to the same conclusion. Thermal gravity (TG) analysis of MXene/LLDPE nanocomposites was conducted at different heating rates, and the TG thermograms suggested the nanocomposites showed an improvement in thermal stability. Apparent activation energy (Ea) of thermal degradation was calculated by the Kissinger method, and Ea values of nanocomposites were higher than that of pure LLDPE. The existence of MXene seems to lead to better thermal stability in composites.


Materials ◽  
2019 ◽  
Vol 12 (5) ◽  
pp. 699 ◽  
Author(s):  
Ying Liu ◽  
Liutao Yang ◽  
Chunping Ma ◽  
Yingzhe Zhang

In this study, X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) methods were used to study the structure, the thermal degradation kinetics, and the thermogram of sweet potato starch, respectively. The thermal decomposition kinetics of sweet potato starch was examined within different heating rates in a nitrogen atmosphere. Different models of kinetic analysis were used to calculate the activation energies using the thermogravimetric data of the thermal degradation process. The activation energies got from Kissinger, Flynn–Wall–Ozawa, and Šatava–Šesták models were 173.85, 174.87, and 174.34 kJ·mol−1, respectively. Thermogravimetry–Fourier transform infrared spectroscopy (TG-FTIR) analysis showed that the main pyrolysis products included water, carbon dioxide, and methane.


2019 ◽  
Vol 38 (1) ◽  
pp. 95
Author(s):  
Mirjana Jovicic ◽  
Oskar Bera ◽  
Katalin Meszaros Szecsenyi ◽  
Predrag Kojic ◽  
Jaroslava Budinski-Simendic ◽  
...  

PMMA (poly(methyl methacrylate)) nanocomposites differing in their nature, size, and surface area were prepared containing one volume percent of silica, alumina or titania. These samples and pure PMMA were prepared in order to analyze how the presence of nanooxides affects the thermal stability and degradation kinetics of the materials. A detailed study of thermal degradation and thermal changes was performed by Simultaneous Thermogravimetry and Differential Scanning Calorimetry (SDT). The proposed mathematical model, including all three heating rates in one minimizing function, well fitted all TGA data obtained with a very high coefficient of correlation. This enabled an assessment of four decomposition steps of the PMMA samples and a calculation of their activation energies and individual contributions to total mass loss. The addition of the largest nanoparticles (titania) caused the highest activation energy for each DTG stage of the PMMA/nanooxide systems. The enhancement of head-to-head H–H bonding strength was achieved by addition of alumina and titania. The influence of the size and nature of nanoparticles on the glass transition temperature of prepared PMMA systems was also determined.


Materials ◽  
2018 ◽  
Vol 12 (1) ◽  
pp. 63 ◽  
Author(s):  
Claudia Barile ◽  
Caterina Casavola ◽  
Paramsamy Vimalathithan ◽  
Marco Pugliese ◽  
Vincenzo Maiorano

The present work describes the mechanical characterization combined with the thermal degradation kinetics of Carbon Fiber Reinforced Polymers (CFRP). The thermal degradation kinetics of CFRP have never been studied in the past. In that regard, the present work focuses on studying the thermal degradation kinetics of CFRP tested mechanically at different environmental conditions. Tensile tests were performed on the specimens with different lay-ups at room temperature, elevated temperature (71 °C), and cryogenic conditions (−54 °C), and the same specimens were used for thermal degradation kinetic studies. Mechanical tests show different responses respect to the different environmental conditions and different fibers orientation. On the other hand, the thermogravimetric results, mass loss, and derivative mass loss, show no significant difference in the degradation of CFRP tested at different temperatures. However, the thermal degradation kinetics shows more insight into the degradation pattern of the materials. The activation energy of degradation shows that the degradation of materials subjected to elevated conditions increases rapidly in the later stages of degradation, suggesting the formation of high char yield. The varying activation energy has been related to different degradation mechanisms. Lastly, the morphology of the materials was studied under SEM to understand the structural change in the material after tested in different weather conditions.


2010 ◽  
Vol 96 ◽  
pp. 245-249 ◽  
Author(s):  
Bin Han ◽  
Yu Long Wu ◽  
Guo Rui ◽  
Wei Feng ◽  
Zhen Chen ◽  
...  

The thermal degradation of PVC resin was examined by the thermogravimetric analysis (TGA). The pyrolysis volatile products were analyzed by Fourier transform infrared spectrometer synchronized with TG test (TG-FTIR). Based on the TG results, the kinetics of thermal degradation was studied by Friedman method. The pyrolysis mechanism was discussed also. The results indicate that the pyrolysis process of PVC can be divided into two main stages: 220°C - 380°C and 380°C - 560°C. By the calculation of mass conservation and TG-FTIR results, it can be supposed that not only HCl, but also some unsubstituted aromatics such as benzene were released during the first stage. The comparison of activation energy shows that the second stage exhibited higher activation energy than the first stage. Two activation energy values in the first stage confirm that there arose two reactions in the first stage.


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