Two kinds of iron alloys have been prepared: one set with 6.67wt.% C and second one with 0.4 wt% C. The alloys have been mechanically alloyed in argon atmosphere, using 8000 SPEX CertiPrep Mixer/Mill. The ratio of ball mass to powder mass (BPR) has been 2:1. X-ray powder diffraction has been used to control, up to 150 hours, the results of mechanical alloying, during the process of milling. The measurements have been performed using Philips PW 1140 diffractometer with Co radiation and diffracted beam graphite monochromator. A formation of cementite Fe₃C has been detected in the first group of alloys (Fe-6.67wt.%C) and some fraction of α-Fe has been present up to 150 hours of milling. In alloys of the second group (Fe-0.4wt.% C) only α-Fe has been observed together with amorphous component. Quantitative phase analysis has been applied to follow the changes in powders' constitution after different times of milling. The internal standard procedure has been used to detect and to calculate the fractions of amorphous component in the powders. Corundum α-Al₂O₃ has been added as internal standard. The Rietveld method has been used to determine the fractions of components of the powders, including the amorphous phase. SIROQUANT^TM software has been used in calculations.

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