Iron-based products account the main volume of powder metallurgy production. Nevertheless its strength and reliability are not enough in comparison with classical cast materials. So that is why making nanostructural powder materials allows to increase strength and extend the range of products. A principally new way of nanostructure production is possible by means of iron mechanical alloying with nitride-forming and nitrogen both at the same time. Unlike classical technology of internal nitrogenation, nitrogen saturation, in our case, occurs by whole volume at plastic deformation conditions. A review of experimental results of phase forming alloys in the Fe-Ni, Fe-Ni-Cr, Fe-Ni-N, Fe-Ni-Cr-N, Fe-Cr-Ni systems prepared by mechanical alloying are given. The influence of the technological parameters of mechanical alloying, atmosphere of mechanical activation on nitrogen content and phase composition of examined alloys has been studied. Experimental results of the influence of mechanical alloying technological parameters on degree of ammonia dissociation and nitrogen content in examined alloys are presented. Heat treatment influence of mechanically alloyed, nitrogen-containing alloys on their phase composition and structure are investigated. It was shown that using mechanical alloying, it’s possible to prepare high-alloyed iron-based alloys containing more than 1% of nitrogen. It was established that technology of mechanical alloying in ammonia atmosphere allows to prepare austenitic steels with nanocrystalline structure, which affords high value of yield stress. Physico-chemical patterns of interaction between the nitrogen-containing atmosphere and nitride-forming elements under their mutual mechanical activation conditions were established in consequence of theoretical and experimental researches. Some scientific principles of nanocrystalline materials were gained by quantitative description of correlation between the mechanical dose, nitrogen potential, nitrogen content in alloy and morphology of hardening phase. Iron-based products account the main volume of powder metallurgy production. Nevertheless its strength and reliability are not enough in comparison with classical cast materials. So that is why making nanostructural powder materials allows to increase strength and extend the range of products. A principally new way of nanostructure production is possible by means of iron mechanical alloying with nitride-forming and nitrogen both at the same time. A classical of internal nitrogenation, nitrogen saturation, in our case, occurs by whole volume at plastic deformation conditions. A review of experimental results of phase forming alloys in the Fe-Ni, Fe-Ni-Cr, Fe-Ni-N, Fe-Ni-Cr-N, Fe-Cr-Ni systems prepared by mechanical alloying are given. The influence of the technological parameters of mechanical alloying, atmosphere of mechanical activation on nitrogen content and phase composition of examined alloys has been studied. Experimental results of the influence of mechanical all oying technological parameters on degree of ammonia dissociation and nitrogen content in examined alloys are presented. Heat treatment influence of mechanically alloyed, nitrogen-containing alloys on their phase composition and structure are investigated. It was shown that using mechanical alloying, it’s possible to prepare high It was established that mechanical alloying in ammonia atmosphere allows to prepare austenitic steels with nanocrystalline structure, which affords high value of yield stress. Physico-chemical patterns of interaction between the nitrogen-containing atmosphere and nitride-forming elements under their mutual mechanical activation conditions were established consequence of theoretical and experimental researches. Some scientific principles of nanocrystalline materials were gained by quantitative description of correlation between the mechanical dose, nitrogen potential, nitrogen content in alloy and morphology of hardening phase.