During
the past decade, CoFe2O4 (hard)/Co–Fe
alloy (soft) magnetic nanocomposites have been routinely prepared
by partial reduction of CoFe2O4 nanoparticles.
Monoxide (i.e., FeO or CoO) has often been detected as a byproduct
of the reduction, although it remains unclear whether the formation
of this phase occurs during the reduction itself or at a later stage.
Here, a novel reaction cell was designed to monitor the reduction in situ using synchrotron powder X-ray diffraction (PXRD).
Sequential Rietveld refinements of the in situ data
yielded time-resolved information on the sample composition and confirmed
that the monoxide is generated as an intermediate phase. The macroscopic
magnetic properties of samples at different reduction stages were
measured by means of vibrating sample magnetometry (VSM), revealing
a magnetic softening with increasing soft phase content, which was
too pronounced to be exclusively explained by the introduction of
soft material in the system. The elemental compositions of the constituent
phases were obtained from joint Rietveld refinements of ex
situ high-resolution PXRD and neutron powder diffraction
(NPD) data. It was found that the alloy has a tendency to emerge in
a Co-rich form, inducing a Co deficiency on the remaining spinel phase,
which can explain the early softening of the magnetic material.