Title: Investigating the Thermal Decomposition and Char Formation in a Furan-Based Epoxy Thermoset for Carbon/Carbon Composites

Authors: Amy E. Honnig, Giuseppe R. Palmese

DOI: 10.33599/nasampe/s.22.0677

Abstract: Carbon/carbon composites (CCC) contain an ablation resistant carbonaceous matrix reinforced with high strength carbon fibers. This combination leads to high thermal stability allowing CCC to be used as thermal protection systems. CCC are manufactured through time intensive and costly densification processes called chemical vapor deposition (CVD) and polymer infiltration and pyrolysis (PIP). Therefore, there is a need to reduce processing costs for CCC. PIP has potential to reduce costs by using a polymer with a high carbon content and a carbon with an open pore structure when pyrolyzed. In order to meet these demands, the pyrolysis conditions must be tuned. However, the polymer’s thermal decomposition needs to first be understood. In this study, the char and pore structure formation of a high char yielding furan-based epoxy resin was investigated from 200-1000 °C. Thermogravimetric analysis with mass spectrometry (TGA-MS), Fourier-Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, and Scanning Electron Microscopy (SEM) were used. Three major decomposition regions were identified showing how the carbon and pores formed. The first region showed the beginnings of porosity and polyaromatic carbon domains. The second region resulted in an increase in volatiles and the growth of carbon domains. The final pore structure was achieved in the second region. The third region resulted in carbon domains increasing through the release of gases with heteroatoms. Keywords: Thermal decomposition, char formation, carbon/carbon composite

References: . Savage, G., Carbon-Carbon Composites. First ed.; New York: Chapman & Hall, 1993. 2. Wampler, T. P., Analytical Pyrolysis: An Overview. In Applied Pyrolysis Handbook, Second ed.; Wampler, T. P., Ed. CRC Press: Boca Raton, FL, 2007. 3. Gandini, A.; Belgacem, M. N., ""Furans in Polymer Chemistry"". Prog. Polym. Sci. 22 (1997): 1203-1379. 4. Organ, P. P.; Mackie, J. C., ""Kinetics of Pyrolysis of Furan"". J. Chem. Sco. Faraday Trans. 87 (1991): 815-523. 5. Liu, R.; Zhou, X.; Zuo, T., ""The Pyrolysis Mechanism of Furan Revisted"". Chem. Phys. Letters 325 (2000): 457-464. 6. Fitzer, E.; Schäfer, W., ""The Effect of Crosslinking on the Formation of Glasslike Carbons from Thermosetting Resins"". Carbon 8 (1970): 353-364. 7. Shindo, A.; Izumino, K., ""Structural Variation During Pyrolysis of Furfuryl Alcohol and Furfural-Furfuryl Alcohol Resins"". Carbon 32 (1994): 1233-1243. 8. Burket, C. L.; Rajagopalan, R.; Marencic, A. P.; Dronvajjala, K.; Foley, H. C., ""Genesis of porosity in polyfurfuryl alcohol derived nanoporous carbon"". Carbon 44 (2006): 2957-2963. 9. Guo, Y.; Bustin, R. M., ""FTIR Spectroscopy and Reflectance of Modern Charcoals and Fungal Decayed Woods: Implications for Studies of Inertinite in Coals"". Int. J. Coal Geo. 37 (1998): 29-53. 10. Alakhras, F.; Holze, R., ""In situ UV-vis and FT-IR Spectroscopy of Electrochemically Synhtesized Furan-Thiophene Copolymers"". Synthetic Metals 157 (2007): 109-119. 11. Ferrari, A. C.; Robertson, J., ""Interpretation of Raman spectra of disordered and amorphous carbon"". Physical Review B 61 (2000): 14095. 12. McDonald-Wharry, J.; Manley-Harris, M.; Pickering, K., ""Carbonisation of Biomass-Derived Chars and the Thermal Reduction of a Graphene Oxide Sample Studied using Raman Spectroscopy"". Carbon 59 (2013): 383-405. 13. Smith, M. W.; Dallmeyer, I.; Johnson, T. J.; Brauer, C. S.; McEwen, J.-S.; Espinal, J. F.; Garcia-Perez, M., ""Structural Analysis of Char by Raman Spectroscopy: Improving Band Assignments through Computational Calculations from First Principles"". Carbon 100 (2016): 678-692. 14. Smith, M. W.; Pecha, B.; Helms, G.; Scudiero, L.; Garcia-Perez, M., ""Chemical and Morphological Evaluation of Chars Produced from Primary Biomass Constituents: Cellulose, xylan, and lignin"". Biomass and Bioenergy 104 (2017): 17-35. 15. Ayiania, M.; Weiss-Hortala, E.; Smith, M.; McEwen, J. S.; Garcia-Perez, M., ""Microstructural Analysis of Nitrogen-Doped Char by Raman Spectroscopy: Raman Shift Analysis from First Principles"". Carbon 167 (2020): 559-574. 16. Inagaki, M., ""Pores in Carbon Materials- Importance of Their Control"". New Carbon Materials 24 (2009): 193-232. 17. Zdravkov, B. D.; Cermak, J. J.; Sefara, M.; Janku, J., "Pore Classification in the Characterization of Porous Materials: A Perspective". Central European Journal of Chemistry 5 (2007): 385-395.

Conference: SAMPE 2022

Publication Date: 2022/05/23

SKU: TP22-0000000677

Pages: 9

Price: $18.00