We report an enhanced
thermal insulation of Fe3O4 nanoparticle by
nanoporous char layer formed during thermal
decomposition of Fe3O4@carboxymethyl cellulose.
The role of char layer properties, decomposition pathways at different
Fe3+/Fe2+ ratio, and the initial core size on
thermal stability are evaluated using XRD, HRTEM, SAXS, TGA, FTIR,
XPS, and laser Raman scattering. In situ high temperature XRD results
show that the Fe3O4 core is stable up to 1000
°C due to the presence of a porous char shell. The presence of
nanopores in the char layer of thickness ∼7 nm was evident
in HRTEM images. The percentage of magnetite increases from 82 to
100% as the temperature is increased from 30 to 1000 °C. The
XPS results show that the relative concentration of Fe2+:Fe3+ is increased from 1:4 to 1:2 on increasing the annealing
temperature from 550 to 1000 °C. For smaller particle size, a
slower growth rate of magnetite core is observed, due to the effective
blocking of the active growth sites. The mechanism of thermal protection
of iron oxide core is explained using existing theoretical models.
The increase in saturation magnetization of the nanocomposites after
high temperature annealing has great significance for practical applications.