Hollow ferromagnetic powders of iron were obtained by means of ultrasonic spray pyrolysis. A variation in the conditions of the synthesis allows for the adjustment of the mean size of the hollow iron particles. Iron powders were obtained by this technique, starting from the aqueous solution of iron nitrate of two different concentrations: 10 and 20 wt.%. This was followed by a reduction in hydrogen. An increase in the concentration of the solution increased the mean particle size from 0.6 to 1.0 microns and widened particle size distribution, but still produced hollow particles. Larger particles appeared problematic for the reduction, although admixture of iron oxides did not decrease the microwave permeability of the material. The paraffin wax-based composites filled with obtained powders demonstrated broadband magnetic loss with a complex structure for lesser particles, and single-peak absorption for particles of 1 micron. Potential applications are 5G technology, electromagnetic compatibility designs, and magnetic field sensing.

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.

Thick dielectric SiO2 shells on the surface of iron particles enhance the thermal and electrodynamic parameters of the iron. A technique to deposit thick, 500-nm, SiO2 shell to the surface of carbonyl iron (CI) particles was developed. The method consists of repeated deposition of SiO2 particles with air drying between iterations. This method allows to obtain thick dielectric shells up to 475 nm on individual CI particles. The paper shows that a thick SiO2 protective layer reduces the permittivity of the ‘Fe-SiO2—paraffin’ composite in accordance with the Maxwell Garnett medium theory. The protective shell increases the thermal stability of iron, when heated in air, by shifting the transition temperature to the higher oxide. The particle size, the thickness of the SiO2 shells, and the elemental analysis of the samples were studied using a scanning electron microscope. A coaxial waveguide and the Nicholson–Ross technique were used to measure microwave permeability and permittivity of the samples. A vibrating-sample magnetometer (VSM) was used to measure the magnetostatic data. A synchronous thermal analysis was applied to measure the thermal stability of the coated iron particles. The developed samples can be applied for electromagnetic compatibility problems, as well as the active material for various types of sensors.

Composite materials filled with ferromagnetic inclusions are useful in the development of various microwave devices. The performance of such devices is determined both by material properties (such as the saturation magnetization and the permeability) and by the demagnetization effects. The paper is devoted to the study of the demagnetization effect on the permeability measurements of composites under external magnetic bias. The microwave permeability of composites filled with flake sendust (Fe-Si-Al alloy) particles is measured as a function of frequency and the external magnetic field. The measurements are carried out by the Nicolson–Ross–Weir technique in a 7/3 coaxial line in the frequency range of 0.1 to 20 GHz by a vector network analyzer. It is found that the magnetic loss peak is split under external fields of more than 1.5 kOe. The main aim of this paper is to study the causes of this splitting and to interpret the observed magnetic loss peaks. To study this effect, the samples of various thicknesses and the samples with isotropic and anisotropic orientations of particles are measured. The particles in the anisotropic samples are oriented by a strong uniform magnetic field. At a small fraction of inclusions, the permanent magnetic field is demagnetized on the individual particles rather than the whole sample. The splitting of the magnetic loss peak of the isotropic sample is caused by different orientations of particles in the sample. At a high fraction of inclusions, the permanent magnetic field is demagnetized on the whole sample and the magnetic loss peak of the isotropic sample is not split. The saturation magnetization of the material is found by measurements under the external magnetic field of the anisotropic sample.

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