Curing Kinetics and Thermal Stability of Epoxy Composites Containing Newly Obtained Nano-Scale Aluminum Hypophosphite (AlPO2)
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. AHP Nanoparticles Preparation
2.3. Preparation of Epoxy/AHP Nanocomposites
2.4. Characterization Methods
2.4.1. Electron Microscopy (SEM and TEM)
2.4.2. Nonisothermal Differential Scanning Calorimetry (DSC)
2.4.3. Thermogravimetric Analysis (TGA)
3. Results and Discussion
3.1. Characterization of AHP Nanoparticles
3.2. Qualitative Cure Analysis
3.3. Quantitative Cure Analysis
3.4. Glass Transition Analysis
3.5. Thermal Stability
4. Conclusions
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
Appendix A. Isoconversional Kinetic Methods
Appendix A.1. Friedman Model
Appendix A.2. Kissinger Method
Appendix B. Curing Reaction Model Determination
Appendix B.1. Friedman Model
Appendix B.2. Malek Method
Appendix C. Determination of Degree of Reaction
References
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Designation | β (°C/min) | Tonset | Tp (°C) | Tendset | ΔT (°C) | ΔH∞ (J/g) | ΔT* | ΔH* | CI | Quality |
---|---|---|---|---|---|---|---|---|---|---|
5 | 26.8 | 86.9 | 143.7 | 116.8 | 179.9 | n.a. | n.a. | n.a. | n.a. | |
Epoxy | 10 | 27.7 | 98.8 | 139.9 | 112.1 | 192.5 | n.a. | n.a. | n.a. | n.a. |
15 | 35.1 | 111.7 | 147.3 | 112.2 | 132.5 | n.a. | n.a. | n.a. | n.a. | |
20 | 40.6 | 118.42 | 150.5 | 110.0 | 145.9 | n.a. | n.a. | n.a. | n.a. | |
E-0.1 AHP | 5 | 19.0 | 86.5 | 134.5 | 115.4 | 232.8 | 0.99 | 1.29 | 1.28 | Excellent |
10 | 26.9 | 102.3 | 143.9 | 117.0 | 201.2 | 1.04 | 1.05 | 1.02 | Good | |
15 | 36.4 | 115.6 | 149.6 | 113.2 | 181.7 | 1.01 | 1.37 | 1.38 | Good | |
20 | 41.2 | 123.4 | 156.2 | 115.0 | 165.2 | 1.05 | 1.13 | 1.19 | Good | |
E-0.3 AHP | 5 | 22.8 | 91.1 | 135.2 | 112.4 | 196.5 | 0.96 | 1.09 | 1.05 | Excellent |
10 | 30.3 | 102.3 | 142.5 | 112.2 | 195.0 | 1.01 | 1.01 | 0.95 | Good | |
15 | 34.1 | 110.0 | 147.6 | 113.5 | 192.8 | 1.01 | 1.46 | 1.47 | Good | |
20 | 37.2 | 115.7 | 152.1 | 115.0 | 190.7 | 1.05 | 1.31 | 1.38 | Good | |
E-0.5 AHP | 5 | 22.3 | 90.6 | 137.0 | 114.8 | 250.5 | 0.98 | 1.39 | 1.36 | Excellent |
10 | 28.1 | 101.0 | 145.8 | 117.7 | 213.5 | 1.05 | 1.10 | 1.09 | Good | |
15 | 34.3 | 109.3 | 149.0 | 114.7 | 199.7 | 1.02 | 1.51 | 1.54 | Good | |
20 | 35.5 | 113.3 | 152.8 | 117.3 | 172.2 | 1.07 | 1.18 | 1.26 | Good |
Designation | Heating Rate (°C/min) | αp∞ | αm | αp |
---|---|---|---|---|
Epoxy | 5 | 0.47 | 0.14 | 0.51 |
10 | 0.70 | 0.15 | 0.55 | |
15 | 0.79 | 0.15 | 0.70 | |
20 | 0.83 | 0.17 | 0.79 | |
E-0.1AHP | 5 | 0.47 | 0.19 | 0.51 |
10 | 0.59 | 0.18 | 0.59 | |
15 | 0.70 | 0.17 | 0.72 | |
20 | 0.72 | 0.18 | 0.72 | |
E-0.3AHP | 5 | 0.50 | 0.06 | 0.59 |
10 | 0.57 | 0.07 | 0.60 | |
15 | 0.62 | 0.08 | 0.62 | |
20 | 0.65 | 0.08 | 0.64 | |
E-0.5AHP | 5 | 0.50 | 0.04 | 0.55 |
10 | 0.54 | 0.05 | 0.58 | |
15 | 0.60 | 0.06 | 0.59 | |
20 | 0.62 | 0.06 | 0.57 |
Designation | β (°C/min) | Ēa (kJ/mol) | ln A (s−1) | Mean (s−1) | m | Mean | n | Mean |
---|---|---|---|---|---|---|---|---|
Friedman | ||||||||
Epoxy | 5 | 72.5 | 22.2 | 22.0 | 0.40 | 0.39 | 1.17 | 0.94 |
10 | 22.1 | 0.39 | 1.00 | |||||
15 | 21.9 | 0.41 | 0.83 | |||||
20 | 21.9 | 0.37 | 0.78 | |||||
E-0.1AHP | 5 | 64.4 | 19.6 | 19.3 | 0.27 | 0.29 | 1.12 | 0.89 |
10 | 19.3 | 0.31 | 0.91 | |||||
15 | 19.2 | 0.31 | 0.77 | |||||
20 | 19.2 | 0.26 | 0.74 | |||||
E-0.3AHP | 5 | 77.2 | 23.4 | 23.3 | 0.53 | 0.49 | 1.03 | 0.93 |
10 | 23.4 | 0.51 | 0.94 | |||||
15 | 23.3 | 0.47 | 0.90 | |||||
20 | 23.3 | 0.44 | 0.85 | |||||
E-0.5AHP | 5 | 80.7 | 24.6 | 24.5 | 0.56 | 0.52 | 1.19 | 1.06 |
10 | 24.6 | 0.54 | 1.09 | |||||
15 | 24.5 | 0.53 | 0.98 | |||||
20 | 24.5 | 0.46 | 0.97 | |||||
Kissinger | ||||||||
Epoxy | 5 | 62.4 | 18.9 | 18.8 | 0.26 | 0.25 | 1.08 | 0.87 |
10 | 18.9 | 0.25 | 0.92 | |||||
15 | 18.7 | 0.27 | 0.77 | |||||
20 | 18.8 | 0.24 | 0.71 | |||||
E-0.1AHP | 5 | 54.9 | 16.5 | 16.4 | 0.14 | 0.16 | 1.04 | 0.82 |
10 | 16.4 | 0.18 | 0.83 | |||||
15 | 16.3 | 0.18 | 0.71 | |||||
20 | 16.4 | 0.13 | 0.69 | |||||
E-0.3AHP | 5 | 69.3 | 21.0 | 21.0 | 0.43 | 0.39 | 0.97 | 0.88 |
10 | 21.0 | 0.41 | 0.89 | |||||
15 | 21.1 | 0.371 | 0.85 | |||||
20 | 21.0 | 0.34 | 0.80 | |||||
E-0.5AHP | 5 | 72.5 | 21.9 | 21.9 | 0.44 | 0.41 | 1.11 | 0.99 |
10 | 21.9 | 0.42 | 1.03 | |||||
15 | 21.9 | 0.41 | 0.92 | |||||
20 | 22.0 | 0.34 | 0.91 |
Sample | Tg (°C) |
---|---|
Epoxy | 73.2 |
E-0.1AHP | 79.5 |
E-0.3AHP | 73.1 |
E-0.5AHP | 69.5 |
Samples | T5%(°C) | T10%(°C) | Residue Weight Ratio at 550 °C |
---|---|---|---|
Epoxy | 319 | 351 | 9.8% |
E-0.1AHP | 320 | 348 | 9.0% |
E-0.3AHP | 295 | 343 | 9.4% |
E-0.5AHP | 299 | 337 | 10.7% |
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Tikhani, F.; Moghari, S.; Jouyandeh, M.; Laoutid, F.; Vahabi, H.; Saeb, M.R.; Dubois, P. Curing Kinetics and Thermal Stability of Epoxy Composites Containing Newly Obtained Nano-Scale Aluminum Hypophosphite (AlPO2). Polymers 2020, 12, 644. https://doi.org/10.3390/polym12030644
Tikhani F, Moghari S, Jouyandeh M, Laoutid F, Vahabi H, Saeb MR, Dubois P. Curing Kinetics and Thermal Stability of Epoxy Composites Containing Newly Obtained Nano-Scale Aluminum Hypophosphite (AlPO2). Polymers. 2020; 12(3):644. https://doi.org/10.3390/polym12030644
Chicago/Turabian StyleTikhani, Farimah, Shahab Moghari, Maryam Jouyandeh, Fouad Laoutid, Henri Vahabi, Mohammad Reza Saeb, and Philippe Dubois. 2020. "Curing Kinetics and Thermal Stability of Epoxy Composites Containing Newly Obtained Nano-Scale Aluminum Hypophosphite (AlPO2)" Polymers 12, no. 3: 644. https://doi.org/10.3390/polym12030644