Abstract
Recently, magnetic nanoparticles and nanocomposite microspheres have attracted great interest for biomedical and technical application. Magnetic metal nanoparticles are of special interest due to their beneficial, size‐dependent magnetic properties. Superparamagnetic metal nanoparticles and mesoscale nanocomposite particles (viz. Co nanoparticles, Co@SiO2, and Co@SiO2@TiO2 particles) were obtained by a three‐step synthesis, involving consecutive steps of thermolysis and sol–gel procedures. A high‐resolution Schottky‐type field emission scanning electron microscope (FESEM) equipped with an energy dispersive X‐ray spectrometer was used to characterize intermediate and final products at the successive stages of synthesis. The samples were deposited on carbon‐coated transmission electron microscopy (TEM) grids (thin film technique) which afforded enhanced specimen contrast and reduced X‐ray background contribution in microanalysis. The FESEM was equipped with a special mounting device for these grids with an appropriate detector beneath. By this method, the samples, covering sizes from the nanometer to micron scale, could be characterized and analyzed by several imaging modes, viz. with standard SE and BSE detection mode and supplementary with low‐voltage scanning transmission mode (STEM‐in‐SEM) and fundamental information about particle size, morphology, and elemental distribution was obtained. Copyright © 2012 John Wiley & Sons, Ltd.
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