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Because there is not enough time to form the new grain and the stress exceeds the expected value, the shear stress suddenly dropped at nearly Planck’s constant. According to the proposed model of microscopic bulging in Fig. 3(b,c), the shear stress was reduced via the prism of SDGBM, which can be seen by the gradual decrease of prism size and by the noticeable increase of dislocation density. The field emission microscopy observation in Fig. 2 confirmed this bulging region.
The above analysis demonstrated that the drive of the sub-grain rotation and twinning was associated with the stress dislocation nucleation from the dislocations trapped in the disclination quadrupole. Therefore, the question that emerges is: Is there a dislocation reservoir present in the GB region?
The answer to this question is provided by the TB specimen fabricated from the same microfreeze-milled Mg-6.4wt%Y (treated with MgY and electroless plating with Ag) substrate. The details of the microprocessing method and experimental setups can be found in the previous study23. The TEM specimen was first mechanically thinned and finally thinned using the focused ion beam.
Figure 6 shows the XRD pattern for the TB specimen. Although the as-fabricated Mg-Y-rich amorphous matrix in the TB substrate is semi-crystalline and has crystal structures similar to those of the bulk Mg (space group: Pm3m), no sharp peak was observed in the XRD diffractogram owing to its high density of dislocations and vacancies. This is a clear indication that the bulk crystalline Mg phase was disrupted by the microfreeze-milled amorphous Mg-Y matrix42. Figure 7 shows the TEM images of the TB specimen. The observed aging GB and the dislocation field suggest that a dislocation-based amorphization process was occurring in the TB specimen. Considering that the as-fabricated state of the TB specimen was semi-crystalline, the amorphous matrix generally extends into the bulk crystalline region and is not confined within the GB region.
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