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In the field of thermal energy storage, organic phase change materials (PCMs) are widely used as functional materials to boost thermal applications. However, there is often a tradeoff between constructing shape-stable composite PCMs with high enthalpy value and those with low leakage rates. Here, we proposed a promising scheme to address this issue. A novel hydrogel consisting of reduced graphene oxide (rGO) and covalent organic framework (COF) was prepared via hydrothermal methods, and the rGO–COF ultralight aerogel with a hierarchical porous structure was formed after freeze-drying. The rGO–COF aerogel shows excellent absorption ability and affinity for organic solvents. It can sufficiently adsorb the molten organic PCMs, such as polyethylene glycol (PEG), and synthesize shape-stable composite PCMs with excellent leak resistance. The COF grown on the surface of rGO has a superior affinity for PEG, so rGO–COF aerogel shows an outstanding PEG loading rate of up to 96.1 wt %, which is 1.7 wt % higher than that of rGO aerogel. In addition, the COF effectively reduces the subcooling of PEG/rGO–COF with 20.3%, compared to PEG/rGO. Meanwhile, the prepared PEG/rGO–COF exhibits extremely high enthalpy and relative enthalpy efficiency (164.6 J/g, 97.4%). This demonstrates that a promising direction was highlighte for the preparation of high-enthalpy shape-stable composite organic PCMs in this work.

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