The goal of this study is the completion of the parameter field of resorcinol-formaldehyde solutions towards the regime of non-monolithic phases. For low sodium carbonate concentration and low mass content of resorcinol and formaldehyde in the starting solution the formation of spherical particles rather than monolithic gels is observed. The organic precursors were converted into carbon powders by pyrolysis. The resulting carbon particles were characterized by scanning electron microscopy (SEM), nitrogen sorption and small-angle X-ray scattering (SAXS). The study shows that carbonization of the organic particles results in spherical carbon particles with a micropore volume of about 0.28 cm~3/g. The composition of the starting solution, however, strongly affects the external surface area as determined from sorption data for the organic as well as for the corresponding carbon particles; the values derived can be converted into average diameters of spherical particles ranging from 30 nm to 5 μm. Complementary SEM and SAXS measurements confirm these findings. A diameter of 5 nm appears to be the upper size limit in particle size forming, while 30 nm spheres develop near the formation of a continuous gel at relatively high sodium carbonate concentrations.
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