Dual‐Step Redox Engineering of 2D CoNi‐Alloy Embedded B, N‐Doped Carbon Layers Toward Tunable Electromagnetic Wave Absorption and Light‐Weight Infrared Stealth Heat Insulation Devices

Abstract 2D layered metallic graphite composites are promising electromagnetic wave absorption materials (EWAMs) for their combined properties of abundant interlayer free spaces, rich metallic polarized sites, and high conductivity, but the controllable synthesis remains rather challenging. Herein, a dual‐step redox engineering strategy is developed by employing cobalt boron imidazolate framework (Co‐BIF) to construct 2D CoNi‐alloy embedded B, N‐doped carbon layers (2D‐CNC) as a promising EWAM. In the first step, a chemical etching oxidation process on Co‐BIF is used to obtain an optimized 2D‐CoNi‐layered double hydroxide (2D‐CoNi‐LDH) intermediate and in the second, high‐temperature calcination reduction is implemented to modify graphitization of the degree of the 2D‐CNC. The obtained sample delivers superior reflection loss (RL min ) of −60.1 dB and wide effective absorption bandwidth (EAB) of 6.24 GHz. The synergy mechanisms of interfacial/dipole polarization and magnetic coupling are in‐depth evidenced by the hologram and Lorentz electron microscopy, revealing its significant contribution on multireflection and impedance matching. Further theoretical evaluation by COMSOL simulation in different fields based on the dynamic loss process toward the test ring reveals the in situ EW attenuation process. This work presents a strategy to develop multifunctional light‐weight infrared stealthy aerogel with superior pressure‐resistant, anti‐corrosion, and heat‐insulating properties for future applications.