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Hierarchical self-assembly nanomaterials with high spatial/angular precision have attracted intensive attention in the urgent research focus in industrial and environmental fields, such as the efficient removal of heavy metal ions from aqueous solution. Herein, we developed an facile microwave-induced ultrasonic hydrolysis approach for the fine synthesis of the hierarchical CuO/Cu(OH)2 urchin-like nanoparticles, which is comprised by Cu-based substructure nanowires with an average diameter of ~5 nm. Benefiting from the high specific surface area of 230.67 m2/g, the urchin-like CuO/Cu(OH)2 hierarchical nanoparticles demonstrated a high maximum adsorption capacity of 357.25 mg/g at pH = 6.0 and T = 298 K for Cr(VI). Furthermore, the corresponding removed approximately 95% can be achieved after the adsorption process for 30 min, suggesting the fast adsorption for Cr(VI). Thermodynamic and kinetic investigations revealed that the Cr(VI) adsorption on the urchin-like CuO/Cu(OH)2 hierarchical nanoparticles was an endothermic and spontaneous process, which could be well fitted by the pseudo-second-order kinetic model. This approach provides new prospects for curbing heavy metal pollution in the environment based on the hierarchical self-assembly nanomaterials.