Abstract: Organic aerogels were fabricated by sol-gel polymerization of melamine and formaldehyde monomers. The porous morphology, structure and thermal stability of the aerogels were characterized by nitrogen adsorption, Fourier transform infrared spectroscopy(FTIR) and thermogravimetry-mass spectrometry(TG-MS). The results show that melamine(M)-formaldehyde(F) aerogel is a material of continuous, interpenetrant, three-dimensional network structure with a high surface area, whose corresponding specific surface is roughly 842 m2/g, and average pore size is 16.04 nm. The pyrolysis process releases several gaseous products, including NO, H2O, NH3, NO2, CO2 and CH4, which is conformed with TG curves, and nearly 97% of MF is decomposed in all. The aerogel is expected to be employed as the template to obtain three-dimensional nanoporous materials.