| Summary: | Within the grain boundary engineering (GBE) of alloys, a mixed grain boundary network with random grain boundaries interrupted by twin boundaries, contributes to enhancing the overall grain boundary-related properties. The higher density of twin boundaries is pursued herein. Furthermore, a two-stage deformation method, i.e., prior cold deformation followed by thermal deformation, was proposed for improving the mixed grain boundary network in the thermal deformation of Ni80A superalloy. The influence of prior cold deformation on the mixed grain boundary network was investigated through a series of two-stage deformation experiments. The analysis of the stress–strain curves shows that the critical strain for dynamic recrystallization (DRX) and peak strains decrease significantly under the effect of prior cold deformation. In comparison to the necklace-like microstructures that occur after a single thermal deformation, the microstructures apparent after a two-stage deformation are characterized by finer DRX grains with abundant Σ3<sup>n</sup> twin boundaries, with a significantly improved density of the Σ3<sup>n</sup> twin boundaries (BLD<sub>Σ3</sub><sup>n</sup>) by a factor of around nine. With increasing prior cold strain, the grain size, after a two-stage deformation, decreases continuously, while the BLD<sub>Σ3</sub><sup>n</sup> increases firstly and then decreases. The mechanisms for improving the mixed grain boundary network via two-stage deformation were uncovered. The sub-grain boundaries formed in prior cold deformation stimulate the nucleation of DRX grains and twins; meanwhile, the driving force for grain boundary migration is enhanced due to prior stored energy. Then, DRX is activated in advance and occurs more completely, thereby promoting the formation of Σ3<sup>n</sup> twin boundaries.
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