Iron-Multiwalled Carbon Nanotubes (iron-MWCNT) were synthesized using varied durations of optimized high-energy ball milling (HEBM) of powder mix. Characterization and furthermore structural stability of these nano tubes were ascertained using state-of-the-art techniques such as Scanning and high resolution Transmission Electron Microscopy, X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, and Differential Scanning Calorimetry (DSC). Additionally, magnetic properties were measured by Vibrating Sample Magnetometer (VSM). Our results indicate that structural integrity and therefore characteristic properties of MWCNTs such as (magnetic, electrical and mechanical properties) are retained up to 60 min post ball milling. Expectedly, HEBM led to partial destruction of C-C bonds, however, the amount of carbon atoms released by bond disruption is insignificant and heavy super saturation of iron with carbon and extensive precipitation of carbides during heating is untenable. Optimal ball milling ensures the formation of smooth and continuous interfaces between the matrix therefore reinforcing the MWCNTs. The excellent interfacial structure so achieved has significantly improved the magnetic properties of iron-MWCNT nanocomposites synthesized in this study. (C) 2018 Elsevier B.V. All rights reserved.