Abstract

Nanometer-size iron-rich particles in carbon nanotubes have been studied by transmission electron microscopy with and without in situ and ex situ heating. Several remarkable results were found; a high temperature phase (γ-Fe) of iron stable at low temperatures and preferential presence of iron and iron carbide in carbon nanotubes. Based upon these experimental results, thermodynamics of the Fe–C phase diagram and its kinetics were used to explain the non-uniform distribution of iron and iron carbide, which also yielded a deeper insight into the formation of carbon nanotubes. Some of the results also allowed describing the role of the graphitic structure in retaining the high temperature phase (γ-Fe) of iron at low temperatures. Furthermore, methods have been demonstrated with which γ-Fe can be produced in carbon nanotubes intentionally or in a large quantity. Selected area electron diffraction patterns of iron inside nanotubes demonstrated the crystallographic relationship of the iron to the nanotube axis along with phase changes of the iron. This paper summarizes the findings and draws further conclusions on the particle shape inside multiwalled carbon nanotubes.

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