Carbon microsphere with high porosity and surface area were synthesized via the sol-gel polycondensation of resorcinol with formaldehyde in a slightly basic medium and followed by drying and pyrolysis. The effects of different parameters during synthesis were investigated. The porous properties of carbon microsphere were evaluated by nitrogen adsorption method and scanning electron microscopy (SEM). By changing both the catalyst species and resorcinol to catalyst ratio (R/C), it was possible to prepare ultramicroporous carbon sphere with pore size about 1.8 nm. The samples evolve from micro-mesoporous solid (RF-Na2CO3: combination of types I and IV isotherms) with 24.2% micropore to an exclusively microporous material (RF-NH4HCO3: type I isotherm) with 98.7% micropore. The results show that it is possible to tailor the morphology of these materials by varying the initial pH of the precursor’s solution in a narrow range and that the micropore surface area and micropore volume are independent from the initial pH, while the BET surface area vary from 582 m2/g (pH = 3.2) to 680 m2/g (pH = 6). However, as the pH increases over pH = 6 the surface area is decreases. These materials can be used as packing for separation columns or as catalysts supports.
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