The hydrolysis and polymerization of a non-catalyzed silica sol was investigated by Fourier Transform Infrared Spectroscopy (FT-IR) and deconvolution of the infrared spectra. The hydrolysis was followed by the 1168 and 812 cm⁻¹ bands which have been observed that decrease continously with the reaction time, and they dissapear showing the complete hydrolysis. The bands located at 1200 and 1147 cm⁻¹ are assigned to polymerization of Si-OH groups forming Si-O-Si bonds in cyclic or linear structures respectively. Both bands increase with time and are present simultaneously in the spectra showing that both kind of cross-linking of Si-OH groups are taking place in the sol to form the gel. In the gel the presence of Si-OH groups and Si-O⁻ free broken bonds have been detected by means of the bonds located at 960 and 920 cm⁻¹ respectively.

Three dimensional (3D) hierarchical porous (micro-, meso- and macro-porous) carbon monoliths (HCMs) have recently been proposed as promising supercapacitor electrodes. In this work, we have further explored the use of block-copolymers as templates for the preparation of HCMs via condensation of resorcinol and formaldehyde (RF) and subsequent carbonization. The resulting HCMs exhibited a textured morphology consisting of a bicontinuous macroporous carbon network built of interconnected microporous carbon colloids, as demonstrated by nitrogen adsorption/desorption isotherms, mercury porosimetry and electron microscopy, in both scanning and transmission mode. Such a texture favored the performance of HCMs as supercapacitor electrodes, reaching remarkable values of capacitance of up to 198 F g⁻¹ (normalized by mass) and 34.5 μF cm⁻² (normalized by BET surface area). The first electrolyte infiltration into the micropore (prior capacitance measurements) was demonstrated to play a crucial role in the achievement of large capacitance values.