Scanning electron microscopy with energy-dispersive X-ray spectroscopy
(SEM–EDX; Hitachi TM3030) was used for the microstructural
analysis of the starting powders and reaction products at a 15 kV
voltage and working distance of approximately 9 ± 0.2 mm. This
was fitted with the Bruker Quantax Energy Dispersive X-ray Spectrometer
for compositional analysis through BSE detectors. The reaction products
were mounted, in powder form, in epoxy resin without crushing and
left to harden for 72 h. The analysis surface was ground manually
with progressively finer abrasives, up to a 1 μm finish,33 (link) and further polished by using diamond pastes
of 6, 3, 2, 1, and 0.25 μm (MetPrep). The samples then underwent
a three-step carbon coating and were back-loaded to a metallic holder.
Electrically conductive silver paint (RS Components) was applied at
the interface between the metallic base epoxy resin to ensure the
sufficient conductivity and, therefore, good quality of the SEM micrographs.
(SEM–EDX; Hitachi TM3030) was used for the microstructural
analysis of the starting powders and reaction products at a 15 kV
voltage and working distance of approximately 9 ± 0.2 mm. This
was fitted with the Bruker Quantax Energy Dispersive X-ray Spectrometer
for compositional analysis through BSE detectors. The reaction products
were mounted, in powder form, in epoxy resin without crushing and
left to harden for 72 h. The analysis surface was ground manually
with progressively finer abrasives, up to a 1 μm finish,33 (link) and further polished by using diamond pastes
of 6, 3, 2, 1, and 0.25 μm (MetPrep). The samples then underwent
a three-step carbon coating and were back-loaded to a metallic holder.
Electrically conductive silver paint (RS Components) was applied at
the interface between the metallic base epoxy resin to ensure the
sufficient conductivity and, therefore, good quality of the SEM micrographs.