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The metal–organic-framework (MOF) approach is demonstrated as an effective strategy for the morphology evolution control of MIL-53(Fe) with assistance of microwave irradiation. Owing to the homogeneous nucleation offered by microwave irradiation and confined porosity and skeleton by MOF templates, various porous Fe2O3nanostructures including spindle, concave octahedron, solid octahedron, yolk–shell octahedron, and nanorod with porosity control are derived by simply adjusting the irradiation time. The formation mechanism for the MOF precursors and their derived iron oxides with morphology control is investigated. The main product of the mesoporous yolk–shell octahedron-in-octahedron Fe2O3nanostructure is also found to be a promising anode material for lithium-ion batteries due to its excellent Li-storage performance. It can deliver a reversible larger-than-theoretical capacity of 1176 mAh g–1after 200 cycles at 100 mA g–1and good high-rate performance (744 mAh g–1after 500 cycles at 1 A g–1).

A unique CuO@NiO microsphere with three-layer ball-in-ball hollow morphology is successfully synthesized by Cu–Ni bimetallic organic frameworks. The beforehand facile microwave-assisted production of the Ni organic framework sphere is used as the template to induce the morphology control of bimetallic oxides. Designed by the controlled surface cationic exchange reactions between Cu and Ni ions, there is an elemental gradient (decreased amount of CuO but increased amount of NiO) from the shell to the core of the microsphere product. This ternary metal oxide hollow structure is found to be very suitable for solving the critical volume expansion problem, which is critical for all high-capacity metal oxide electrodes for lithium ion batteries. A reversible larger-than-theoretical capacity of 1061 mAh·g–1can be retained after a repetitive 200 cycles without capacity fading compared to the initial cycle. These excellent electrochemical properties are ascribed to the step-by-step lithium insertion reactions induced by the matched CuO@NiO composition from the shell to the core and facilitated lithium/electron diffusion and accommodated volume change in the porous bimetallic oxides microsphere with a multiple-layer yolk–shell nanostructure.