Influence of Hydrogen Reduction Stage Conditions on the Microwave Properties of Fine Iron Powders Obtained via a Spray-Pyrolysis Technique

The relationship between the chemical purity of one-size particles and microwave properties in ferromagnetic materials is not clearly studied. Ferromagnetic nanostructured iron powders were synthesized from iron nitrate solution using ultrasonic spray-pyrolysis and then reduced in H₂ flow at 350, 400, 450, and 500 °C. A rise in the concentration of solutions of a precursor from 10 to 20 wt. % led to an increase in mean particle size. The interrelationship was studied between chemical composition and the microwave dispersion of the powders obtained. An increase in the temperature of reduction changes the chemical composition and increases the amplitude of complex microwave permeability, which was studied using solid-state physics methods (XRD, STA, SEM, and VNA). It was found that annealing at 400 °C is the optimal treatment that allows the production of iron powders, consisting of about 90% of α-Fe phase, possessing a particle surface with low roughness and porosity, and demonstrating intense microwave absorption. Annealing at a higher temperature (500 °C) causes an even higher increase in permeability but leads to the destruction of nanostructured spheres into smaller particles due to grain growth. This destruction causes an abrupt increase in permittivity and therefore significantly reduces potential applications of the product. The insight into chemical–magnetic relationships of these materials enhances the data for design applications in magnetic field sensing.