The effect of hydrogen plasma treatment of iron oxide films on the growth and microstructure of carbon nanotubes (CNTs) by microwave plasma enhanced chemical vapor deposition process has been investigated. Microwave plasma was characterized in-situ using optical emission spectrometer. Morphology of the films was examined by scanning electron microscopy. Structural analysis was carried out by high resolution transmission electron microscopy (HRTEM) equipped with energy dispersive X-ray spectroscopy (EDS) and micro-diffraction attachments. It is found that oxide films without H 2 plasma pretreatment or treated for lesser time resulted in CNT films with high percentage of carbonaceous particles and with embedded particles/nanorods distributed discontinuously in the cavity of the nanotubes. The embedded particles were found to be of iron carbide (Fe-C) as confirmed by HRTEM, EDS and micro-diffraction analysis. Experimental observations suggested that the iron oxide particles had poor catalytic action for CNT growth and in-situ reduction of oxide clusters to Fe by hydrogen plasma plays a key role in discontinuous filling of the nanotubes by the catalytic particles. [12][13][14] have been used to synthesize CNTs. CVD methods (both thermal and plasma enhanced) are reliable in producing multiwalled CNTs (MWNTs) with proper control over the process parameters. Plasma enhanced CVD, however, can produce CNTs with a higher growth rate, at low temperature, and with better reproducibility. The plasma not only ionizes the gas but also causes a local surface heating [15]. Consequently, growth temperature could be significantly decreased compared to non-plasma CVD processes. In addition, the plasma atmosphere may also influence the detailed catalyst surface kinetics in many ways [16] and hence the growth of carbon nanostructures.Growth of CNTs and their microstructures depend on several parameters such as growth technique, feed gases, growth temperature, catalyst, and catalyst preparation method as well as their state (solid, liquid or vapor). In plasma assisted CVD processes, dilution gases play a critical role in the growth of CNTs and the structure of CNTs can be tailored by judicious control over gas composition [17]. In our earlier report, we investigated the effect of different dilution gases such as H 2 , NH 3 and N 2 and their different composition on the growth and microstructure of CNTs by microwave plasma enhanced CVD (MPECVD) process on Fe coated Si substrates using C 2 H 2 as feed gas [17]. Plasma pretreatment of catalyst film can also affect the growth and structure of CNTs significantly especially in a high frequency plasma process such as MPECVD. To the best of our knowledge, effect of H 2 plasma pretreatment of iron oxide films on the growth and structure of CNTs by MPECVD process have not been reported. Therefore, the motivation for the present