<p>Cured phenolic resins with distinct microstructures were prepared by varying the formaldehyde to phenol molar ratio from 1.1 to 1.4 to investigate the influence of microstructure on char integrity during pyrolysis. Scanning electron microscopy and dynamic contact angle analysis confirmed that increasing the formaldehyde content led to the formation of a more porous microstructure. Simultaneous thermal analysis revealed that the cured resin with a formaldehyde to phenol molar ratio of 1.3 exhibited the highest char yield of 67% at 1000&#xa0;°C. Interestingly, the cured resins with higher initial porosity formed a more solid char after pyrolysis, suggesting that the porous microstructure facilitated the escape of pyrolysis gases, thereby reducing internal pressure buildup and mitigating pressure induced microstructural damage. In addition, Fourier transform infrared spectroscopy revealed that the cured resin with a formaldehyde to phenol molar ratio of 1.3 also possessed the highest total methylene index of 2.046, indicating the highest crosslink density. Correspondingly, this cured resin exhibited the highest compressive strength of 76.8&#xa0;MPa and a modulus of 1.31 GPa, despite being more porous than the formulations with lower molar ratios. These results highlight that microstructural porosity primarily controls char integrity, whereas crosslink density dominantly governs mechanical performance, providing a framework for optimizing cured phenolic resins for thermal protection applications.</p>

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Microstructure-Controlled Char Integrity During the Pyrolysis of Cured Phenolic Resins

  • Ahmedi Asraf,
  • Ariadne Lakshmidevi Juwono,
  • Bagus Hayatul Jihad,
  • Yudi Nugraha Thaha,
  • Joko Triwardono

摘要

Cured phenolic resins with distinct microstructures were prepared by varying the formaldehyde to phenol molar ratio from 1.1 to 1.4 to investigate the influence of microstructure on char integrity during pyrolysis. Scanning electron microscopy and dynamic contact angle analysis confirmed that increasing the formaldehyde content led to the formation of a more porous microstructure. Simultaneous thermal analysis revealed that the cured resin with a formaldehyde to phenol molar ratio of 1.3 exhibited the highest char yield of 67% at 1000 °C. Interestingly, the cured resins with higher initial porosity formed a more solid char after pyrolysis, suggesting that the porous microstructure facilitated the escape of pyrolysis gases, thereby reducing internal pressure buildup and mitigating pressure induced microstructural damage. In addition, Fourier transform infrared spectroscopy revealed that the cured resin with a formaldehyde to phenol molar ratio of 1.3 also possessed the highest total methylene index of 2.046, indicating the highest crosslink density. Correspondingly, this cured resin exhibited the highest compressive strength of 76.8 MPa and a modulus of 1.31 GPa, despite being more porous than the formulations with lower molar ratios. These results highlight that microstructural porosity primarily controls char integrity, whereas crosslink density dominantly governs mechanical performance, providing a framework for optimizing cured phenolic resins for thermal protection applications.