Protective SiO2 coating deposited to iron microparticles is highly demanded both for the chemical and magnetic performance of the latter. Hydrolysis of tetraethoxysilane is the crucial method for SiO2 deposition from a solution. The capabilities of this technique have not been thoroughly studied yet. Here, two factors were tested to affect the chemical composition and the thickness of the SiO2 shell. It was found that an increase in the hydrolysis reaction time thickened the SiO2 shell from 100 to 200 nm. Moreover, a decrease in the acidity of the reaction mixture not only thickened the shell but also varied the chemical composition from SiO3.0 to SiO8.6. The thickness and composition of the dielectric layer were studied by scanning electron microscopy and energy-dispersive X-ray analysis. Microwave permeability and permittivity of the SiO2-coated iron particles mixed with a paraffin wax matrix were measured by the coaxial line technique. An increase in thickness of the silica layer decreased the real quasi-static permittivity. The changes observed were shown to agree with the Maxwell Garnett effective medium theory. The new method developed to fine-tune the chemical properties of the protective SiO2 shell may be helpful for new magnetic biosensor designs as it allows for biocompatibility adjustment.
Frequency dependencies of permittivity and permeability of composites filled with Permalloy powder with various concentrations and shapes of particles have been measured and discussed. The powder particles of various shapes were obtained by mechanical milling of industrial Permalloy powder in organic media. Paraffin wax was used as a matrix for producing the composites. A shape data of the particles was obtained with an electron microscope. The permittivity and permeability were measured in the frequency range of 0.13 to 10 GHz. The shape of the particles changes from sphere to platelet with increase of milling time. The change leads to a shift of the ferromagnetic resonance (FMR) frequency and magnetic loss peak. It is shown that for larger particles, a decrease of the Q-factor of the ferromagnetic resonance is observed, which is explained by the strong influence of the skin effect. With increase of the concentration of the Permalloy particles in composite, the magnetic loss peak shifts to low frequencies. When the spherical particles are flattened, the resonance frequency shifts to high frequencies, which indicates that the shift to high frequencies due to the decrease of the skin effect and the change in the magnetic structure is stronger than the shift to the low frequencies by changing the shape and reducing the demagnetization.
Spray pyrolysis of an aqueous solution of iron nitrate, proceeded with reduction of the product in hydrogen, gave iron powder with micron-sized hollow particles. Coating these iron particles with SiO2 through tetraethyl orthosilicate hydrolysis prevented interparticle electrical contacts and suppressed DC percolation. This material shows a high ferromagnetic resonance frequency of 18 GHz, low permittivity, and weighs 20% less than common carbonyl iron. Potential microwave applications are for inductors and electromagnetic interference shielding designs.
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