In situ regulation of microstructure and microwave-absorbing properties of FeSiAl through HNO3 oxidation

Wrapping insulation of coatings is effective for enhancing the microwave-absorbing properties (MAPs) of ferromagnetic absorbents (FMAs). However, the process is still limited by the low bonding strength with the matrix. Herein, an in situ regulation strategy based on the preparation of thin thickness and strong adhesion insulating layers through HNO3 oxidation was developed to address the limitations. The oxidation process of FeSiAl (FSA) powders was carried out by HNO3 following three main steps. First, the original oxide layer first reacted with HNO3 to form Fe3+ and Al3+. Second, the oxide layer composed of Al2O3 and Fe3O4 was preferentially formed due to the negative change in Gibbs free energy. Finally, the oxide and pigment-deposition layers were subjected to competitive growth and dissolution accompanied by the dissolution of Fe and Al atoms. Oxidation time up to 10 min resulted in the formation of a bilayer structure with a thickness of ∼50 nm on the FSA surface, as well as an outer layer crammed of Al(OH)3 and Fe(OH)3, and an inner layer containing mixed Fe2O3, Fe3O4, Al2O3, and SiO2. The MAPs of as-treated FSA achieved minimum reflection loss (RL) of −25.90 dB at 13.36 GHz, as well as absorption bandwidth of 5.61 GHz (RL < −10 dB) at 10.13–15.74 GHz and thickness of 2.5 mm. In sum, the developed route looks promising for the preparation of high-performance FMAs.