The effect of pyrolysis heating rate on the mesoporosity of Pluronic F-127 templated carbon xerogels

This study explored the impact of pyrolysis heating rates ranging from 1 to 20 K min⁻¹ (final temperature 500 °C) on the porosity of resorcinol-formaldehyde based carbonaceous xerogels soft-templated with Pluronic F-127. We primarily utilized thermoporometry (differential scanning calorimetry technique) and, to a lesser extent, conventional nitrogen adsorption at −196 °C to analyze the porosity of the resulting carbons. Additionally, we examined the effects of particle size and the scale of the pyrolysis experiment, comparing a laboratory furnace with a thermal analyzer. At lower heating rates, particularly in a thermal analyzer, mesopores approximately 7–8 nm in size were observed. An increase in the heating rate resulted in larger mesopores, from 7 to 17 nm, widened pore size distribution (PSD), and a rise in mesopore volume from 0.21 to 0.53 cm³ g⁻¹. Higher heating rates (> 5 K min^-1) also accelerated the decomposition of the Pluronic F-127, leading to fast gas release, which subsequently caused cracking of the carbon skeleton and widening of the pores. Pyrolysis heating rate had no significant effect on the degree of graphitization in the pyrolyzed samples. Particle size showed minimal influence on porosity when xerogels were pyrolyzed at either the minimal or maximal heating rates in the thermal analyzer. However, experiments conducted in a laboratory furnace at the lowest heating rate demonstrated that imprecise temperature control and fluctuations can lead to the formation of larger mesopores.