Cross-sectional analysis of W-cored Ni nanoparticle via focused ion beam milling with impregnation

Tungsten and nickel bimetallic nanoparticle is synthesized by radio frequency thermal plasma process which belongs to the vapor phase condensation technology. The morphology and chemical composition of the synthesized particle were investigated using the conventional nanoparticle transmission electron microscopy (TEM) sample. A few part of them looked like core/shell structured particle, but ambiguities were caused by either TEM sample preparation or TEM analysis. In order to clarify whether a core/shell structure is developed for the particle, various methodologies were tried to prepare a cross-sectional TEM sample. Focused ion beam (FIB) milling was conducted for cold-compacted particles, dispersed particles on silicon wafer, and impregnated particles with epoxy which is compatible with electron beam. A sound cross-sectional sample was just obtained from cyanoacrylate impregnation and FIB milling procedure. A tungsten-cored nickel shell structure was precisely confirmed with aid of cross-sectional sample preparation method.