A new processing method, ice-templating method, for the preparation of ordered macroporous materials using sol-gel transformation is developed. When precursor hydrogels are unidirectionally frozen, pseudosteady state growth of ice crystals occurred inside their matrices. Such ice crystals were regularly aligned parallel to the freezing direction, and played the role of a template. A microhoneycomb morphology was formed at this freezing stage. After removal of the ice crystals by thawing and drying, organic/inorganic gel microhoneycombs with micro/mesopores inside their honeycomb walls could be obtained. Carbon cryogel microhoneycombs (CMH) preparation succeeded by applying this new method to resorcinol-formaldehyde (RF) hydrogels. The relationship between the preparation conditions and the morphology of the resulting RF cryogels is compared, and the preparation of fine CMH is presented. This is an abstract of a paper presented at the 229th ACS National Meeting (San Diego, CA 3/13-17/2005).