New highly porous aerogel materials based on the coordination of metal ions and organic ligands are developed and characterized by PXRD, BET and TEM analysis. The new metal-organic aerogels (MOAs) have typical specific BET surface area above 1000m2/g with the thermal stability up to 250oC, which is generally larger than the normal silica based or carbon aerogels. The intrinsic chemical compositions of meal-organic aerogel provide itself the advantages of easy synthesis, feasible modification and functionalization on the properties and structures. One example of using such aerogel as reaction matrix to synthesis metal-organic frameworks, such as HKUST-1, is discussed. It generates size-homogenized crystals of HKUST-1 around 20ìm. This new kind of porous materials gives great potentials in the catalysis, adsorption/separation and sensors applications.