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• Although the nano-dispersed precipitation of G-phase within the grain hardens the alloy remarkably, its large amount of precipitation at the grain boundary leads to serious alloy embrittlement. • For the first time, the crystal structure transition of nano-dispersed precipitates from the Fe 2 TiSi-L2 1 to the Ni 16 Ti 6 Si 7 -G phase is observed within the ferrite at the early stage of aging. • Guided by current TEM and DFT results, the interfacial energy is predicted to play a leading role in forming the cube-on-cube orientation relationship between α-Fe and G-phase. • Adopting the "cold-rolling and aging" process to effectively avoid its precipitation at grain boundaries, a class of high-performance ferroalloys with both high strength and good ductility is realized. A typical G-phase strengthened ferritic model alloy (1Ti:Fe-20Cr-3Ni-1Ti-3Si, wt.%) has been carefully studied using both advanced experimental (EBSD, TEM and APT) and theoretical (DFT) techniques. During the classic "solid solution and aging" process, the superfine (Fe, Ni) 2 TiSi-L2 1 particles densely precipitate within the ferritic grain and subsequently transform into the (Ni, Fe) 16 Ti 6 Si 7 -G phase. In the meanwhile, the elemental segregation at grain boundaries and the resulting precipitation of a large amount of the (Ni, Fe) 16 Ti 6 Si 7 -G phase are also observed. These nanoscale microstructural evolutions result in a remarkable increase in hardness (100–300 HV) and severe embrittlement. When the "cold rolling and aging" process is used, the brittle fracture is effectively suppressed without loss of nano-precipitation strengthening effect. Superhigh yield strength of 1700 MPa with 4% elongation at break is achieved. This key improvement in mechanical properties is mainly attributed to the pre-cold rolling process which effectively avoids the dense precipitation of the G-phase at the grain boundary. These findings could shed light on the further exploration of the precipitation site via optimal processing strategies. [Display omitted] [ABSTRACT FROM AUTHOR]