This paper reports the preparation of microporous carbon (MC) nanoparticles (25-90 nm) and spheres (260-320 nm) by carbonization of poly(furfuryl alcohol) (PFA) particles from furfuryl alcohol. Two synthetic routes were developed for forming "nonstick" PFA particles, which include (1) using silica as temporary barrier to isolate surface-reactive PFA nanoparticles and (2) a two-step polymerization of furfuryl alcohol (FA) involving slow polymerization (1 st step) and sphere formation (2 nd step). The high dispersibility of the MC spheres was realized by removing surface functional groups of the PFA spheres with the evaporation-induced concentrated sulfuric acid (2 nd step). Both routes were effective in preventing irreversible aggregation of nanoparticles and spheres. Scanning electron microscopy, transmission electron microscopy, photon correlation spectroscopy and nitrogen adsorption were used to characterize the nanoparticles and spheres. The MC nanoparticles and spheres obtained showed good dispersibility in water and various organic solvents. They had a micropore volume of 0.13-0.14 cm 3/g, and a pore size of 0.49-0.56 nm. This synthetic routes presented here are very efficient for large-scale synthesis of MC nanoparticles and spheres.