Characterization of crystallite size, dislocation characteristics and stacking faults in nanostructured mechanically alloyed Cu–Fe system using an advanced X-ray diffraction analysis method

• Various microstructural features of mechanically alloyed Cu–Fe are investigated simultaneously.
• The crystallite size and size distribution are calculated via refinement of XRD profiles.
• Using the eCMWP method, characteristics of dislocations are studied as a function of milling time and composition.
• The probability of stacking faults are calculated.

Developments in the synthesis of nanostructured materials have expanded the need for appropriate characterization methods. The aim of this work is to apply new X-ray diffraction analysis methods for simultaneous investigation of various microstructural characteristics. For this purpose, the structure of mechanically alloyed Cu–Fe system with three compositions of 30 wt%, 50% and 70% of iron was studied. By applying the modified Williamson-Hall method, the type of dislocations in the FCC phase is distinguished. Afterwards by modification of previous XRD analysis methods, the proportion of edge/screw dislocations was characterized. Moreover, the outer cut-off radius, the density and energy of dislocations were calculated as a function of the composition and the milling time. On the other hand, using the extended convolutional multiple whole profile fitting procedure, the variations in the crystallite size and size distribution of FCC and BCC phases were studied. Finally, the stacking fault probability was calculated in different milled samples. It is revealed that smaller steady state crystallite size of samples with higher Fe content, is relevant to reduction of the outer cut-off radius of dislocation. On the other hand, the density of dislocations and stacking faults increased continuously up to 96 h of milling.