Nano-structured powders of intermetallic compound FeTi were prepared by ball milling process in the presence of NaBH4. FeTi is considered as one of promising reversible hydrogen storage, however, the difficulty in initial activation of FeTi demands a high temperature vacuum heat treatment, followed by repeated exposure to H2 gas at elevated pressure, before use as a reversible H2 gas absorption/desorption. The demand for such activation process is reported to be mitigated by preparing the FeTi into nanostructured form by mechanical milling. In this work, NaBH4 was added as a hydrogen-source while the mechanical synthesis process was undertaken, aiming at further reducing the demand for the initial activation process for the nano-structured FeTi hydrogen storage alloy. X-ray crystallographic characteristics of the FeTi powders prepared as such are reported in this work