Magnetic nanoparticles (Ni, CoNiFe) with diameters ranging from 30 to 200 nm were synthesized by electrode position using carbon nanowalls as templates. A series of experiments have been carried out to study the formation mechanism of nanoparticles. It was found that the formation of nanoparticles instead of continuous films was attributed to two key factors, i.e., the uneven current density distribution on the nanowall surfaces and the pulsed current supply with alternate polarities. The as-grown nanocomposite structures were characterized using energy-dispersive X-ray analysis, scanning electron microscopy, and magnetic measurement using a vibrating sample magnetometer. These types of nanostructures may have potential applications in batteries, supercapacitors, catalysts, and biomedical devices.
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