The sol–gel
synthesis of iron carbide (Fe
3
C)
nanoparticles proceeds through multiple intermediate crystalline phases,
including iron oxide (FeO
x
) and iron nitride
(Fe
3
N). The control of particle size is challenging, and
most methods produce polydisperse Fe
3
C nanoparticles of
20–100 nm in diameter. Given the wide range of applications
of Fe
3
C nanoparticles, it is essential that we understand
the evolution of the system during the synthesis. Here, we report
an
in situ
synchrotron total scattering study of
the formation of Fe
3
C from gelatin and iron nitrate sol–gel
precursors. A pair distribution function analysis reveals a dramatic
increase in local ordering between 300 and 350 °C, indicating
rapid nucleation and growth of iron oxide nanoparticles. The oxide
intermediate remains stable until the emergence of Fe
3
N
at 600 °C. Structural refinement of the high-temperature data
revealed local distortion of the NFe
6
octahedra, resulting
in a change in the twist angle suggestive of a carbonitride intermediate.
This work demonstrates the importance of intermediate phases in controlling
the particle size of a sol–gel product. It is also, to the
best of our knowledge, the first example of
in situ
total scattering analysis of a sol–gel system.