Cellulose aerogels are the latest generation of aerogels and have also received extensive attention due to their renewable and biocompatible properties. Herein, cellulose aerogel was facilely prepared by using NaOH/urea solution as solvent, raising the temperature to control gelation and drying wet gel sequentially. With NaOH/urea solution as solvent, the cellulose concentration has an important impact on the micromorphology of cellulose aerogels, while the aging time rarely affects the micromorphology. The appropriate solvent and drying method allow the formation of different cellulose crystalline structures. Different from the Cellulose Ⅰ crystalline structure of raw cellulose powder, the cellulose phase of as-prepared cellulose aerogels belongs to the Cellulose Ⅱ crystalline structure, and to some extent the pyrolysis temperature is also lower than that of raw cellulose powder. The resultant cellulose aerogel prepared by using NaOH/urea solution as solvent and freeze-drying has a uniform macroporous structure with a macropore size of 1~3 µm.

Hierarchically porous carbon aerogels (CAs) were prepared by organic condensation gelation method combined with atmospheric drying and pore-formation technology, followed by a carbonization process. With as-prepared CAs as substrate, the transition metal oxide nanoparticles loaded CAs composites (MnO2/Mn2O3@CA and Ni/NiO@CA) were achieved by means of liquid etching method combined with heat treatment, respectively. The catalyst, pore-forming agent and etching have important roles on the apparent density and pore structure of CAs. The hydrochloric acid (catalyst) significantly accelerates the gelation process and influences the size and distribution of macropores, whereas the addition of PEG2000 (pore-forming agent) and the etching of liquid solution leads to the formation of mesopore structure in CAs. Appropriate amounts of hydrochloric acid and PEG2000 allow the formation of hierarchically porous CAs with a BET surface area of 482.9 m2·g−1 and a macropore size of 11.3 μm. After etching and loading, the framework of CAs is etched to become a mesoporous structure, and the transition metal oxide nanoparticles can be uniformly loaded in CAs. These resultant composites have promising application in super capacitor, electrocatalysis, batteries and other fields.