Preparation and non-isothermal cure kinetics study of epoxy resin nanocomposites with amine and epoxy functionalized magnetic nanoparticles

2021 ◽  
pp. 095400832110124
Author(s):  
Ali Akbar Keivanloo Shahrestanaki ◽  
Mohammad Mehrshad ◽  
Seyed Hashem Akhlaghi

Amine-functionalized magnetic nanoparticles NiFe2O4@SiO2@Amine (AMNP), and epoxy functionalized magnetic nanoparticles, CuFe2O4@SiO2@Epoxy (EMNP) were synthesized in three steps. Homogeneous stable dispersion of AMNP and EMNP, at concentrations of 1, 5, 10, 15, 20 wt% in epoxy resin were prepared using stoichiometric amounts of 4,4’-diaminodiphenylsulfone (DDS) as a curing. The optimum ratio of AMNP and EMNP were found to be 5%, and these were investigated by the total enthalpy of the curing reaction using differential scanning calorimetry (DSC) thermograms at 10°C/min. The cure kinetics of epoxy resin-functional magnetic nanoparticles-DDS composites were studied using non-isothermal DSC thermograms at different heating rates (5, 10, 15, 20°C/min). The kinetic parameters of the curing process, such as activation energy ( Ea), pre-exponential factor ( A), and rate constant ( k) were determined using several non-isothermal kinetic methods: Kissinger-Akahira-Sunose (KAS), Kissinger, Straink, Flynn-Wall-Ozawa (OFW), and Bosewell. The kinetic curing values obtained with different kinetic methods are well-matched. The Ea values were calculated in the range of 59.80 to 65.94, 57.69 to 63.92, and 45.38 to 52.45 kJ.mol−1 for the DGEBA/DDS, DGEBA/DDS/AMNP, and DGEBA/DDS/EMNP systems respectively. Also, The A values, using the Kissinger method, were calculated to be in the range of 7.0 × 105, 4.0 × 105, and 0.2 × 105 S−1 for the DGEBA/DDS, DGEBA/DDS/AMNP, and DGEBA/DDS/EMNP systems respectively. The glass transition temperatures of cured resins were determined with DSC, and the surface morphology of the nanocomposites and also the dispersion of the nanoparticles were investigated using scanning electron microscopy (SEM).

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.


2021 ◽  
pp. 002199832110015
Author(s):  
Alexander Vedernikov ◽  
Yaroslav Nasonov ◽  
Roman Korotkov ◽  
Sergey Gusev ◽  
Iskander Akhatov ◽  
...  

Pultrusion is a highly efficient composite manufacturing process. To accurately describe pultrusion, an appropriate model of resin cure kinetics is required. In this study, we investigated cure kinetics modeling of a vinyl ester pultrusion resin (Atlac 430) in the presence of aluminum hydroxide (Al(OH)3) and zinc stearate (Zn(C18H35O2)2) as processing additives. Herein, four different resin compositions were studied: neat resin composition, composition with Al(OH)3, composition comprising Zn(C18H35O2)2, and composition containing both Al(OH)3 and Zn(C18H35O2)2. To analyze each composition, we performed differential scanning calorimetry at the heating rates of 5, 7.5, and 10 K/min. To characterize the cure kinetics of Atlac 430, 16 kinetic models were tested, and their performances were compared. The model based on the [Formula: see text]th-order autocatalytic reaction demonstrated the best results, with a 4.5% mean squared error (MSE) between the experimental and predicted data. This study proposes a method to reduce the MSE resulting from the simultaneous melting of Zn(C18H35O2)2. We were able to reduce the MSE by approximately 34%. Numerical simulations conducted at different temperatures and pulling speeds demonstrated a significant influence of resin composition on the pultrusion of a flat laminate profile. Simulation results obtained for the 600 mm long die block at different die temperatures (115, 120, 125, and 130 °C) showed that for a resin with a final degree of cure exceeding 95% at the die exit, the maximum difference between the predicted values of pulling speed for a specified set of compositions may exceed 1.7 times.


Materials ◽  
2019 ◽  
Vol 12 (23) ◽  
pp. 3939 ◽  
Author(s):  
Lucio Fabio Cassiano Nascimento ◽  
Fernanda Santos da Luz ◽  
Ulisses Oliveira Costa ◽  
Fábio de Oliveira Braga ◽  
Édio Pereira Lima Júnior ◽  
...  

Knowledge about the curing behavior of a thermosetting resin and its composites includes the determination of kinetic parameters and constitutes an important scientific and technological tool for industrial process optimization. In the present work, the differential scanning calorimetry (DSC) technique was used to determine several curing parameters for pure epoxy and its composite reinforced with 20 vol % mallow fibers. Analyses were performed with heating rates of 5, 7.5, and 10 °C/min, as per the ASTM E698 standard. The kinetic related parameters, that is, activation energy (E), Avrami’s pre-exponential factor (Z), and mean time to reach 50% cure (t½), were obtained for the materials, at temperatures ranging from 25 to 100 °C. Response surfaces based on the mathematical relationship between reaction time, transformed fraction, and temperature were provided for optimization purposes. The results showed that the average curing time used for the production of diglycidyl ether of bisphenol A/triethylenetetramine (DGEBA/TETA) epoxy systems or their composites reinforced with natural mallow fibers can be considerably reduced as the temperature is increased up to a certain limit.


2006 ◽  
Vol 326-328 ◽  
pp. 1271-1274 ◽  
Author(s):  
Mei Yang ◽  
Shi Lin Yan ◽  
Mei Liu

The cure kinetic properties of 191# resin was studied by means of the differential scanning calorimeter (DSC) data. Dynamic DSC scanning at four different heating rates (5, 10, 15 and 20/min) are employed to investigate the cure kinetics. DSC curves show that there are two exothermal peaks. Kissinger’s method is applied to processing the data. The activation energy E and pre-exponential factor A were gained by linear regress and the cure kinetics model was developed. Based on T − β method, the temperatures of cure reaction beginning, maximum reaction rate and reaction ending were obtained. These will help to process designing of unsaturated polyester resin used in advanced composite materials.


RSC Advances ◽  
2018 ◽  
Vol 8 (52) ◽  
pp. 29830-29839 ◽  
Author(s):  
Li Lu ◽  
Liao Xia ◽  
Hao Zengheng ◽  
Sheng Xingyue ◽  
Zhang Yi ◽  
...  

The cure kinetics of epoxy resin cured by D-EP, D-EP/CNT composites and D-EP/CNTs-H20 were investigated by non-isothermal differential scanning calorimetry (DSC).


2015 ◽  
Vol 60 (2) ◽  
pp. 1357-1359 ◽  
Author(s):  
Y. Hongbo ◽  
C. Meiling ◽  
W. Xu ◽  
G. Hong

Abstract The thermal decomposition of magnesium-aluminum layered double hydroxides (LDHs) was investigated by thermogravimetry analysis and differential scanning calorimetry (DSC) methods in argon environment. The influence of heating rates (including 2.5, 5, 10, 15 and 20K/min) on the thermal behavior of LDHs was revealed. By the methods of Kissinger and Flynn-Wall-Ozawa, the thermal kinetic parameters of activation energy and pre-exponential factor for the exothermic processes under non-isothermal conditions were calculated using the analysis of corresponding DSC curves.


2010 ◽  
Vol 123-125 ◽  
pp. 411-414 ◽  
Author(s):  
Da Hu Yao ◽  
Kyung Bok Sun ◽  
Peng Li ◽  
Joong Hee Lee

The curing reaction of the system bisphenol-A glycidol ether epoxy resin modified by poly (ethylene glycol) (PEO) and flexible amine (D-230) as curing agent has been studied by means of differential scanning calorimetry (DSC) and thermal scanning rheometry. The curing kinetic parameters have been calculated from the non-thermal DSC curve. The kinetic analysis suggests that the two-parameter autocatalytic model is more appropriate to describe the kinetics of the curing reaction of the system. Increasing the PU content leads to an increase in the heat of curing and has a little effect on the kinetic parameters apparent activation energy (Ea), pre-exponential factor (A), and order of the reaction (m and n). The rheological properties were measured by isothermal curing evolution. Introduction of PEO flexible chains delayed the polymerization. It has been confirmed that the introduction of PEO chains in the structure of the epoxy resin increases the mobility of the molecular segment of the epoxy networks and results in the decrease in glass transition temperature.


Author(s):  
Jae-Young Lee ◽  
Bumchoul Choi ◽  
Woo-Kum Lee ◽  
Joong-Pyo Shim ◽  
Hong-Ki Lee

Highly conductive bipolar plate for polymer electrolyte membrane fuel cell (PEMFC) was prepared using phenol novolac-type epoxy/graphite powder (GP)/carbon fiber filament (CFF) composite, and a rubber-modified epoxy resin was introduced to the phenol novolac-type epoxy resin in order to give elasticity to the bipolar plate. The cure condition of the neat epoxy system, differential scanning calorimetry (DSC) was carried out and the DSC data were introduced to Kissinger equation. And tensile and flexural tests were carried out using universal testing machine (UTM) and the surface morphology of the fractured specimen and the interfacial bonding between epoxy matrix and CFF were observed by a scanning electron microscopy (SEM). Kissinger expression showed that the activation energy for the cure kinetics of novolac epoxy (9.3g)/rubber epoxy (1.0g)/curing agent (9.6g)/accelerator (0.1g) system was 76.8 kJ/mol and the pre-exponential factor was 1.73 × 1010 min−1. As was expected, electrical conductivity increased with increasing total carbon content, and the value increased with increasing CFF content at the same carbon content. Tensile strength and flexural strength linearly decreased with increasing epoxy content, however at the same carbon content, these values increased with increasing CFF content. It was because the CFF acted as electrical conductive pass and the good effect on the mechanical properties was due to the strong bonding between CFF and epoxy resin, which was confirmed by the SEM.


2011 ◽  
Vol 236-238 ◽  
pp. 2058-2062
Author(s):  
Hong Jun Zhou ◽  
Guo Qiang Yin ◽  
Miao Hong Zhuang ◽  
Jian Fang Ge ◽  
Xuan Lin

The cure kinetics of epoxy/epoxy-grafted nano-aluminum oxide using 4, 4'-diaminodiphenylsulphone (DDS) as the curing agent was studied by nonisothermal differential scanning calorimetry (DSC) at different heating rates. The activation energy (Ea) was determined by Flynn-Wall-Ozawa method, and kinetic model was predicted by Málek method. TheEa values of epoxy/nano-aluminum oxide/DDS systems are generally higher than those of epoxy /DDS. These imply that the addition of nano-aluminum oxide would inhibit the chain mobility of the epoxy resins. Furthermore, autocatalytic model was found to be appropriate to describe the kinetics of above mentioned reactions. The predicted curves fit well with the experimentally obtained curves.


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