Hollow carbon spheres are potential candidates for lightweight microwave absorbers. However, the skin effect of pure carbon‐based materials frequently induces a terrible impedance mismatching issue. Herein, small‐sized NiO/Ni particles with heterojunctions on the N‐doped hollow carbon spheres (NHCS@NiO/Ni) are constructed using SiO2 as a sacrificing template. The fabricated NHCS@NiO/Ni displayed excellent microwave absorbability with a minimum reflection loss of −44.04 dB with the matching thickness of 2 mm and a wider efficient absorption bandwidth of 4.38 GHz with the thickness of 1.7 mm, superior to most previously reported hollow absorbers. Experimental results demonstrated that the excellent microwave absorption property of the NHCS@NiO/Ni are attributed to balanced dielectric loss and optimized impedance matching characteristic due to the presence of NiO/Ni heterojunctions. Theoretical calculations suggested that the redistribution of charge at the interfaces and formation of dipoles induced by N dopants and defects are responsible for the enhanced conduction and polarization losses of NHCS@NiO/Ni. The simulations for the surface current and power loss densities reveal that the NHCS@NiO/Ni has‑ applicable attenuation ability toward microwave under the practical application scenario. This work paves an efficient way for the reasonable design of small‐sized particles with well‐defined heterojunctions on hollow nanostructures for high‐efficiency microwave absorption.

The rational design of lightweight, broad‐band, and high‐performance microwave absorbers is urgently required for addressing electromagnetic pollution issue. Metal single atoms (M–SAs) absorbers receive considerable interest in the field of microwave absorption due to the unique electronic structures of M–SAs. However, the simultaneous engineering of the morphology and electronic structure of M–SAs based absorbers remains challenging. Herein, a template‐assisted method is utilized to fabricate isolated Co–SAs on N‐doped hollow carbon spheres (NHCS@Co–SAs) for high‐performance microwave absorption. The combination of atomically dispersed Co sites and hollow supports endows NHCS@Co–SAs with excellent microwave absorption properties. Typically, at an ultralow filler content of 8 wt%, the minimum reflection loss and effective absorption bandwidth of the NHCS@Co–SAs are up to −44.96 dB and 5.25 GHz, respectively, while the absorbing thickness is only 2 mm. Theoretical calculations and experimental results indicate that the impedance matching characteristic and dielectric loss of the NHCSs can be tuned via the introduction of M–SAs, which are responsible for the excellent microwave absorption properties of NHCS@Co–SAs. This work provides an atomic‐level insight into the relationship between the electronic states of absorbers and their microwave absorption properties for developing advanced microwave absorbers.

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