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Two-dimensional (2D) nanostructures, though promising in energy storage, suffer from aggregation and subsequent deterioration of performance in practical applications. Hence, assembly of 2D nanostructures into three-dimensional (3D) architectures is highly desirable. Here, we report a microwave-assisted approach to the controllable synthesis of 2D materials with tunable 3D structures simply by adjusting the ratio of water/ethylene glycol (H₂O/EG). Novel flower-on-sheet 3D hierarchical structures of nickel cobalt double hydroxide (NiCo LDHs) are obtained at EG content of 40%, while microspheres and 2D nanosheets are obtained when the EG content is 0% and 75%, respectively. We propose that under microwave irradiation, EG molecules disperse the nuclei and facilitate the initial formation of 2D sheets. Subsequently, the dominating hydrophobicity of the assembling results in the formation of nanoflowers …