AbstractPorous silica was synthesized from cornhusk using the sol–gel polymeric route and compared with ash obtained from the direct combustion process under laboratory conditions. The unmodified ash from the direct combustion process was dissolved in NaOH for 1 h to form sodium silicate, which was subsequently hydrolyzed with citric acid to yield a silica xerogel. The obtained xerogel was characterized using inductively coupled plasma–optical emission spectrometry (ICP-OES), Fourier transforms infrared (FTIR) spectroscopy, X-ray diffraction (XRD), simultaneous thermal analysis (STA), gas sorption techniques to determine their elemental constituents, functional groups, crystalline phases, thermal stability, and porosity, respectively. The results showed that the synthesized silica xerogel exhibited porous network structures with a high-specific surface area and mesopore volume of 384 m2/g and 0.35 cm3/g, respectively. The pore size distribution revealed a complete transformation of the pore network structures of the unmodified ash from a monomodal to a bimodal pore system, with micro- and mesopore peaks centered around 1.5 and 3.8 nm, respectively. The ICP-OES results showed that the silica content significantly increased from 52.93 to 91.96 wt.% db after the sol–gel treatment. XRD diffraction confirmed the amorphicity of the silica particles obtained from the sol–gel extraction method. In addition, the STA data showed that the silica xerogel has high thermal stability compared to the unmodified ash, as the latter exhibited poor thermal stability and low textural properties. The high surface area and narrow pore cavity size distribution of the porous silica xerogel make it an ideal substrate for catalysts and an excellent template for growing other nanoparticles within the pores.