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Microwave-absorbing materials have attracted increased research interest in recent years because of their core roles in the fields of electromagnetic (EM) pollution precaution and information security. In this paper, microwave-absorbing material NiFe-layered double hydroxide (NiFe-LDH) was synthesized by a simple co-precipitation method and calcined for the fabrication of NiFe-mixed metal oxide (NiFe-MMO). The phase structure and micromorphology of the NiFe-LDH and NiFe-MMO were analyzed, and their microwave-absorbing properties were investigated with a vec