Curing Kinetics of T300 Carbon Fiber/Epoxy Resin Prepregs Investigated by Differential Scanning Calorimetry
XiaobaoZhu1,2Email20230149@kust.edu.cn
LiYang1,2Email20040051@kust.edu.cn
JingChen1
A
KaihuaChen1,2✉A
ShenghuiGuo1,2✉1
A
Faculty of Metallurgical and Energy EngineeringKunming University of Science and Technology650093KunmingChina2State International Joint Research Center of Advanced Technology for Superhard MaterialsKunming University of Science and Technology650093KunmingChina
Xiaobao Zhu1,2, Li Yang1,2, Jing Chen1, Kaihua Chen 1,2*, Shenghui Guo 1,2**
1Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming 650093, China
2State International Joint Research Center of Advanced Technology for Superhard Materials, Kunming University of Science and Technology, Kunming, 650093, China
* Corresponding author: 20230149@kust.edu.cn;
** Corresponding author: 20040051@kust.edu.cn;
Abstract
Understanding and quantifying the curing kinetics of carbon fiber/epoxy prepregs is critical for optimizing manufacturing processes and ensuring structural integrity in high-performance composites. In this work, the non-isothermal and isothermal curing behaviors of T300 carbon fiber/epoxy resin prepregs were systematically studied via differential scanning calorimetry (DSC). Activation energies and kinetic parameters were derived using the Kissinger, Ozawa, and Friedman model-free approaches, revealing both global and conversion-dependent kinetic behavior. The Málek method confirmed that the curing reaction follows an autocatalytic mechanism consistent with the Sestak–Berggren model. Under isothermal conditions, increasing temperature would significantly accelerate the curing rate, and the curing behavior was well captured by a diffusion-modified Kamal model. The combined kinetic modeling provides a comprehensive understanding of the reaction mechanism, enabling more accurate simulation of curing behavior and guiding the design of optimized curing cycles for aerospace-grade thermoset composites.
Keywords:
T300 carbon fiber prepreg
epoxy resin
DSC
kinetic properties
A
1. Introduction
Epoxy resins are among the most widely used thermosetting polymers in the field of fiber-reinforced composites, owing to their excellent thermal stability, high mechanical strength, strong adhesion to fibers, and chemical resistance1. In high-performance applications such as aerospace structures, wind turbine blades, and automotive components, carbon fiber/epoxy prepregs have become indispensable materials due to their superior weight-to-strength ratio and processability. Among these, T300 carbon fiber reinforced epoxy prepregs—particularly those using dicyandiamide (DICY) as the curing agent—are widely adopted in commercial practice due to their well-balanced mechanical properties and storage stability2.
During the manufacturing process of fiber-reinforced composites, the curing behavior of epoxy resin plays a decisive role in determining the final quality and performance of the components. The curing reaction involves an exothermic crosslinking process that transforms the resin matrix from a low-viscosity liquid into a rigid, three-dimensional network3–5. This transformation affects not only the thermal and mechanical properties of the material but also its dimensional stability, void content, and resistance to environmental degradation. An incomplete or sub-optimized curing process can result in under-cured resin, poor fiber-matrix bonding, or residual stresses, leading to inferior structural integrity.
Differential scanning calorimetry (DSC) is a powerful and widely used technique for analyzing the curing characteristics of thermosetting resins6–8. It allows researchers to measure heat flow associated with chemical reactions, enabling the extraction of crucial kinetic parameters such as activation energy, reaction rate constants, and conversion behavior9. Over the years, a variety of model-free (isoconversional) and model-fitting kinetic approaches have been developed, including the Kissinger, Ozawa, and Friedman methods for evaluating apparent activation energy, and the Kamal and Sestak–Berggren models for describing reaction mechanisms. Hwang et al. 9 reported the curing kinetics of vacuum bag only prepregs using DSC and DMA, employing phenomenological and chemical rheological models to predict the curing process. Jouyandeh et al. 8 utilized model-free integral Kissinger and differential Friedman methods to derive the activation energy of epoxy resin/Fe3O4 nanocomposites from DSC data. A. Mousa et al.10 studied the curing kinetics of vinyl ester resin using FTIR and DSC. They monitored double bond reduction in VE and styrene to calculate the degree of cure. Results from both methods correlated well at 120°C, but full curing was not achieved due to vitrification, which limited the reaction by diffusion. Hongfeng Li et al.11 modified bisphthalonitrile (BPh) resin with DP/BMI prepolymer and found it effectively accelerated curing, lowering the peak temperature to 250.6°C. Blending with novolac cyanate ester (NCE) improved thermal stability without greatly affecting viscosity. Zhongjian Ding et al.12 investigated the hydrolytic stability of MUF resin. Results showed that higher melamine content increased branching, reducing stability. MUF resin was less stable than UF resin, and melamine addition stage affected resin structure. Chao Chen et al.13 analyzed the curing kinetics of CYCOM 970 and 603 epoxy resins using nonisothermal DSC. A simplified method revealed two autocatalytic reactions, and kinetic parameters were obtained via the Kamal and Kissinger models. Results matched experimental data well.
Although many studies have applied DSC to investigate epoxy resin systems and their composites, relatively few have focused specifically on the curing kinetics of aerospace-grade T300 carbon fiber/DICY epoxy prepregs under both non-isothermal and isothermal conditions. Moreover, most existing studies treat the curing process as a purely chemically controlled reaction, often neglecting the diffusion-limited behavior that emerges during the later stages of cure, especially near the vitrification point. The lack of comprehensive kinetic modeling limits the ability to accurately simulate and optimize curing cycles in practical processing environments.
The present study systematically investigates the curing kinetics of a commercial T300 carbon fiber/epoxy prepreg using both non-isothermal and isothermal DSC techniques. Apparent activation energies are calculated using Kissinger, Ozawa, and Friedman methods. The Málek method is employed to identify the most appropriate reaction mechanism, while a modified Kamal model incorporating a diffusion control term is developed to describe the full-range curing behavior. The results aim to provide a robust kinetic framework for predicting the cure state and tailoring the curing process of thermoset composites in high-performance structural applications.
2. Materials and Methods
2.1 Materials
The T300 carbon fiber/epoxy resin prepreg employed in this study was designated as model USN10000 and supplied by Weihai Guangwei Composite Materials Co., Ltd.14 The material consists of T300 carbon fibers and a DICY-cured epoxy resin system, with a resin content of approximately 30 wt%. The prepreg was delivered in its uncured form, with a nominal layer thickness of 0.12 mm. Before the DSC testing, the uncured prepreg was stored at -5°C to ensure stability during handling and analysis.
2.2 Experimental procedure
The prepreg samples were subjected to both non-isothermal and isothermal curing protocols. For each non-isothermal experiment, approximately 10 mg of uncured carbon fiber/epoxy resin prepreg was weighed and sealed in an aluminum crucible. Under a nitrogen atmosphere, the samples were heated from − 50°C to 300°C at various rates of 5, 10, 15, and 20°C/min, respectively. After the first heating cycle, the samples were cooled to 30°C at 20°C/min and held for 5 minutes, and then subjected to a second dynamic heating scan under identical conditions to confirm complete curing.
For each isothermal test, sample of similar mass was heated from 30°C to different target temperatures of 120, 130, 140, and 150°C at a heating rate of 50°C/min. Once the sample reached the predetermined temperature, it was maintained at the corresponding temperature for a holding time of 90, 90, 60, and 60 minutes, respectively. After the isothermal curing, the samples were cooled to 0°C at 20°C/min and then analyzed by a final dynamic scan from ambient temperature to 300°C at a heating rate of 10°C/min.
2.3 Characterization
Thermal analyses were carried out using a differential scanning calorimeter (DSC 200F3, Netzsch, Germany). All tests were conducted under a nitrogen purge to prevent oxidation and thermal degradation. Non-isothermal scans were used to evaluate the overall curing behavior, while isothermal measurements provided insight into time-dependent conversion and reaction rates. Second-round dynamic scans were performed after each curing cycle to verify the degree of cure and residual reactivity. The curing enthalpy, glass transition temperature, and kinetic parameters were extracted from the DSC thermograms for further analysis.
3. Results and Discussion
3.1 Non-Isothermal Curing Behavior of T300 Prepreg
To evaluate the curing behavior of the T300 carbon fiber/epoxy resin prepreg, non-isothermal DSC analyses were conducted under four heating rates: 5, 10, 15, and 20°C/min. The DSC thermograms exhibited a single prominent exothermic peak for each heating rate (Fig. 1a), indicating that the curing process follows a one-step dominant reaction. At low temperatures, minor fluctuations in the baseline were observed, corresponding to the glass transition of the uncured resin, where the matrix transitions from a rigid to a viscoelastic state.
After the first dynamic scan, a second scan was performed to confirm reaction completion. As shown in Fig. 1b, no exothermic peak was observed, indicating that the matrix was fully cured during the first cycle. However, a weak endothermic peak appeared near 100°C, which may be attributed to the melting or evaporation of low molecular weight additives or residual volatiles.
The average glass transition temperature of the fully cured matrix (Tg,∞) was determined to be 108.1°C in accordance with ASTM D3418. Curing enthalpies, calculated from the integrated area under the exothermic peaks, varied with heating rate: 115.4 J/g at 5°C/min, 78.85 J/g at 10°C/min, 164.22 J/g at 15°C/min, and 105.0 J/g at 20°C/min. These variations highlight the competition between kinetic and thermal diffusion effects during the curing process.
Fig. 1
(a) Results of the first round of dynamic DSC scanning, (b) Results of the second round of dynamic DSC scanning
3.1.1 Kinetic Model Identification and Reaction Mechanism
In order to clarify the mechanism underlying the curing behavior, phenomenological kinetic models were employed. The curing process of thermosetting epoxy resins can typically be described by two types of models: n-level reaction model and autocatalytic reaction15. In the former, the maximum reaction rate occurs at the onset of the process, while in the latter, a delay is observed due to catalytic accumulation.
Analysis of the DSC curves as shown in Fig. 1 suggested that the T300 system exhibits an autocatalytic curing behavior, as the maximum rate is not observed at the beginning. Accordingly, the reaction model is described by:
1
where α is the degree of cure, A is the pre-exponential factor, Ea is the activation energy, and m and n are empirical reaction orders.
3.1.2 Activation Energy from Kissinger and Ozawa Approaches
To quantitatively determine the apparent activation energy, the Kissinger and Ozawa methods were applied to the non-isothermal DSC data. The Kissinger and Ozawa methods are classic kinetic approaches in thermal analysis, both capable of calculating the activation energy of curing reactions. The Kissinger method assumes:
2
The Kissinger equation is derived through a series of integrations and calculations based on this Eq. 16:
3
In the equation, Tp represents the peak temperature of the DSC curve, β represents the heating rate of the reaction, A represents the pre-exponential factor, Ea represents the activation energy of the reaction, and R = 8.314. Plotting ln(β/Tp2) against 1/Tp and performing linear regression, the intercept of the fitted line can be used to calculate the pre-exponential factor A, while the slope can be used to calculate the activation energy Ea of the curing reaction.
The Kissinger fitting results are depicted by the blue line in Fig. 2. The slope and intercept of the fitting curve are 9.33×103 and 11.82, respectively, indicating a well-established linear relationship. Based on the fitted data, the activation energy and pre-exponential factor are calculated to be 77.57 kJ/mol and 1.27×109 min− 1, respectively.
The Ozawa method can similarly be employed to determine the activation energy of curing kinetics, with its expression as follows17–19:
4
During the temperature rise of the material, the transformation from temperature to time is obtained:
5
In the equation, β represents the heating rate. By performing variable integration of this equation and then substituting it into the conversion rate function integral, the Ozawa equation can be derived based on the approximate solution of the Boltzmann factor integral and the Doyle approximation:
6
Based on the above equation, plotting ln(β) against 1/Tp and performing linear regression yields the fitting results shown by the red line in Fig. 2, with a slope of 1.02×104. The activation energy of the reaction is calculated to be 80.61 kJ/mol. As the Ozawa equation involves the kinetic model f(α), it is not possible to calculate the pre-exponential factor A using the slope of the fitted curve in the absence of a clear kinetic model.
These close results, obtained from both the Kissinger and Ozawa approaches, confirm the reliability of the model-fitting methods for capturing the global curing kinetics of this system.
Fig. 2
Comparison of the fitting results of Kissinger and Ozawa
3.1.3 Conversion-Dependent Activation Energy from Friedman Analysis
Both the Kissinger and Ozawa methods can only yield a single value for the activation energy. However, during the curing reaction, chemical reactions proceed continuously, and the activation energy of the reaction varies at different degrees of cure. Therefore, the Friedman method can be further employed to calculate the activation energy at different degrees of cure in the reaction process. The expression for this method is as follows 20,21:
7
Figure 3 depicts the curves of the degree of cure as a function of temperature at different heating rates. It can be observed that with higher heating rates, the temperature required to reach the same degree of cure is higher.
Fig. 3
Curve of curing degree of carbon fiber/epoxy resin prepreg as a function of temperature at different heating rates
A
The data from Fig. 3 corresponding to various heating rates were analyzed by extracting ln(dα/dt) values at fixed conversion levels ranging from 0.1 to 0.9, and plotting them against the reciprocal of the corresponding temperatures (1/Tα). Linear regression was then applied to these plots to determine the apparent activation energy as a function of the degree of cure. The results, presented in Fig. 4, reveal a continuous decline in activation energy throughout the curing process. Initially, the activation energy is 75.03 kJ/mol at α = 0.1. As the curing process proceeds, the resin matrix gradually transfers from a rigid state to a viscoelastic gel, leading to the enhanced molecular mobility and improved collisions between epoxy groups and curing agents. As a result, the activation energy steadily decreases with increasing conversion, reaching the minimum value of 35.66 kJ/mol at α = 0.9.Fig. 4
Fitting curve of ln(dα/dt) to 1/Tα at different warming rates for equal conversion points
3.1.4 Model Validation via Málek and Sestak–Berggren Approach
Although the Kissinger, Ozawa, and Friedman methods provide key kinetic parameters such as the activation energy (Ea) and pre-exponential factor (A), they are insufficient for identifying the specific reaction model f(α) governing the curing process of T300 carbon fiber prepreg. To determine the type of curing reaction in the resin system, given the activation energy (Ea), the Málek method can be employed to determine which kinetic equation is suitable for describing the reaction process in the resin system. The Málek method primarily relies on two functions, y(α) and z(α) 22,23:
8
9
A
where x represents Ea/RT, where Ea is the activation energy, R is the gas constant, T represents the absolute temperature of the reaction, β represents the heating rate of the reaction, and π(x) denotes the expression for temperature integral. Senum and Yang proposed that π(x) can be approximated using the following fourth-order function 24,25:10
The average activation energy obtained from the Friedman method was substituted into the functions y(α) and z(α) for calculation and normalization. The relationship among y(α), z(α) and α is shown in Fig. 5.
Fig. 5
Variation trend of the two functions y(α) and z(α) as a function of curing degree α
The values of αp∞, αM, and αp at various heating rates β, as calculated using the Málek method, are summarized in Table 1. The respective degrees of cure corresponding to the maximum values of the functions y(α) and z(α) are denoted as αM and αp∞. Based on Málek 's research 26, when αp∞ ≠ 0.632 and αM∈(0, αp), the curing reaction conforms to the self-catalytic Sestak-Berggren model. According to these criteria, it is observed that the curing kinetics of the epoxy resin system studied in this paper can be described by the self-catalytic Sestak-Berggren model.
Heating rates β (°C/min) | αp∞ | αM | αp |
|---|---|---|---|
5 | 0.380 | 0.367 | 0.372 |
10 | 0.377 | 0.374 | 0.381 |
15 | 0.353 | 0.346 | 0.350 |
20 | 0.360 | 0.348 | 0.353 |
The values of αp∞, αM, and αp calculated using the Málek method at different heating rates β can be utilized to establish dynamic kinetic analysis on the fundamental reaction rate equation.
11
Sestak and Berggren described the reaction mechanism function.
12
According to Arrhenius law:
13
Substituting Eqs. (12) and (13) into the Eq. (11) yields the dynamic kinetic calculation formula:
14
After simplification, the equation can be derived as follows:
15
In the equation, m and n represent two reaction orders. The reaction order n can be calculated by plotting ln[(dα/dt)ex] against ln[αp(1-α)] and fitting the slope, while the relationship between reaction orders m and n is given by m = pn, where p = αM/(1-αM) 27. The fitting calculation results of A, reaction orders m and n under different heating rates are summarized in Table 2.
Heating rate (°C/min) | A | m | n |
|---|---|---|---|
5 | 0.7036 | 0.8533 | 1.361 |
10 | 1.043 | 0.8104 | 1.292 |
15 | 1.592 | 0.8053 | 1.433 |
20 | 1.908 | 0.7936 | 1.441 |
Figure 6 presents a comparison between the experimental DSC data and the kinetic simulation results. The fitted curves based on the Sestak–Berggren model exhibit good agreement with the experimental data across different temperatures, indicating that this model accurately captures the curing behavior of the epoxy resin system studied. The consistency between the calculated and measured reaction rates further validates the applicability of the Sestak–Berggren model to describe the curing kinetics.
Fig. 6
Comparison of DSC test results with kinetic fit results
3.2 Isothermal Curing and Diffusion-Controlled Mechanism
3.2.1 Isothermal DSC Analysis of Prepreg
To further examine the cure behavior under practical manufacturing conditions, isothermal DSC experiments were conducted at 120°C, 130°C, 140°C, and 150°C-all above the Tg,∞.
The results of the first round of isothermal DSC scans are shown in Fig. 7. The initial scans reveal that the prepreg system requires an induction period at the beginning of isothermal curing, followed by a gradual increase in the rate of exothermic curing until the reaction is complete. It is evident from the graph that the curing reaction is exothermic, as evidenced by the appearance of an exothermic peak in all DSC curves.
Fig. 7
Variation of heat flow measured by DSC with time
Figure 8 illustrates the variation of curing degree over time. It can be observed that the curing rate increases with the increase of isothermal curing temperatures. At 120°C, 130°C, 140°C, and 150°C, the time required to reach 90% curing degree is 33.4 min, 22.3 min, 18.5 min, and 14.4 min, respectively.
Fig. 8
Relationship between reaction curing degree and time at different temperatures
3.2.2 Application of the Diffusion-Controlled Kamal Model
Kamal et al. investigated the curing kinetics of epoxy resins and proposed the Kamal model as follows28:
16
The variables m and n represent the reaction orders, while k1 and k2 denote the rate constants for uncatalyzed and catalyzed reactions, respectively.
To further examine the influence of diffusion control on the curing system during the later stages of the reaction, researchers introduced a diffusion factor based on the free volume theory29:
17
In the equation, C represents the restriction constant, and αc represents the critical degree of cure. By incorporating this diffusion factor into the Kamal model, the diffusion-controlled Kamal equation can be expressed as follows:
18
The relationship between the degree of curing and time at 120°C, as shown in Fig. 9, was obtained by fitting the experimental data using the diffusion-controlled Kamal equation (Eq. (18)). The model was successfully fitted to isothermal experimental data, as shown in Fig. 9. Table 2 presents the fitted data for the relationship between cure rate and degree of cure. The simulation accurately reproduced the transition from chemically controlled to diffusion-limited regimes, demonstrating that the modified Kamal model can effectively describe the complete curing behavior of the prepreg under isothermal conditions.
Temperature (°C) | K1 | K2 | m | n | C | |
|---|---|---|---|---|---|---|
120 | -0.00105 | 0.218 | 0.4325 | 0.7578 | 1.393 | 0.3815 |
130 | 0.02884 | 0.6018 | 0.6495 | 0.7393 | 2.824 | 0.1263 |
140 | -0.04209 | 0.4739 | 0.2813 | 0.5526 | 4.636 | 0.431 |
150 | -0.08672 | 0.8402 | 0.291 | 0.7765 | 4.377 | 0.4327 |
Fig. 9
Comparison of DSC test results and kinetic fitting results
5. Conclusion
This study presents a comprehensive kinetic analysis of T300 carbon fiber/epoxy prepregs by using non-isothermal and isothermal DSC scans. The key findings are included:
1.
The fully cured system exhibits an ultimate glass transition temperature (Tg,∞) of 108.1°C, and non-isothermal enthalpy data revealed heating rate–dependent behavior indicating the competing thermal and kinetic effects.
2.
The activation energy derived using Kissinger and Ozawa methods ranged from 77.57 to 80.61 kJ/mol, while the Friedman method revealed a significant reduction in activation energy with the increase of curing degree. The lowest activation energy is 35.66 kJ/mol which is obtained at 90% conversion.
3.
Model discrimination using the Málek approach confirmed that the Sestak–Berggren autocatalytic model best describes the curing behavior under dynamic conditions.
4.
Isothermal experiments showed a strong temperature dependence of the cure rate, and the curing process was accurately reproduced by a diffusion-controlled Kamal model, which accounts for vitrification effects in later stages.
These findings contribute to a deeper understanding of the curing mechanisms in epoxy-based prepregs and provide a robust theoretical framework for simulation-based process design and cycle optimization in advanced composite manufacturing.
A
Acknowledgements
This research was supported by Yunnan Fundamental Research Projects (grant NO. 202401BE070001-021, NO. 202501AU070116, and NO. 202401BE070001-005), Natural Science Foundation of China (52364051), and Central guidance local scientific and technological development funds (202407AB110022). The authors (Shenghui Guo, Yunling Scholar; Li Yang, Industrial Innovation Scholar) would like to acknowledge Yunnan Province Xingdian Talent Support Plan Project.
A
Availability of Data and Materials
The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.
A
Conflict of InterestOn behalf of all authors, the corresponding author states that there is no conflict of interest.
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