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Multishelled NiO hollow microspheres for high-performance supercapacitors have been prepared and the formation mechanism has been investigated. By using resin microspheres to absorb Ni 2+  and subsequent proper calcinations, the shell numbers, shell spacing and exterior shell structure were facilely controlled via varying synthetic parameters. Particularly, the exterior shell structure that accurately associated with the ion transfer is finely controlled by forming a single shell or closed exterior double-shells. Among multishelled NiO hollow microspheres, the triple-shelled NiO with an outer single-shelled microspheres show a remarkable capacity of 1280 F g −1  at 1 A g −1 , and still keep a high value of 704 F g −1  even at 20 A g −1 . The outstanding performances are attributed to its fast ion/electron transfer, high specific surface area and large shell space. The specific capacitance gradually increases to 108% of its initial value after 2500 cycles, demonstrating its high stability. Importantly, the 3S-NiO-HMS//RGO@Fe 3 O 4  asymmetric supercapacitor shows an ultrahigh energy density of 51.0 Wh kg −1  at a power density of 800 W kg −1 , and 78.8% capacitance retention after 10,000 cycles. Furthermore, multishelled NiO can be transferred into multishelled Ni microspheres with high-efficient H 2  generation rate of 598.5 mL H 2  min −1  g −1  Ni  for catalytic hydrolysis of NH 3 BH 3  (AB).

Multishelled NiO Hollow Microspheres for High-performance Supercapacitors with Ultrahigh Energy Density and Robust Cycle Life