J. Mater. Sci. Technol. ›› 2022, Vol. 102: 80-88.DOI: 10.1016/j.jmst.2021.06.035
• Research Article • Previous Articles Next Articles
Wenjun Lua,b,**(
), Jianjun Lic,*()
Received:2021-06-01
Revised:2021-06-15
Accepted:2021-06-17
Published:2021-08-27
Online:2021-08-27
Contact:
Wenjun Lu,Jianjun Li
About author:* mejjli@csu.edu.cn (J. Li).Wenjun Lu, Jianjun Li. Synergetic deformation mechanism in hierarchical twinned high-entropy alloys[J]. J. Mater. Sci. Technol., 2022, 102: 80-88.
Fig. 1. In-situ deformation set-up. (a) SEM image and corresponding EBSD micrographs (i.e., boundary and phase maps) of an FCC γ grain containing multiple Σ3 twins and FIB lift-out region. (b) Custom-designed Cu tensile dog-bone holder. (c) Enlarged SEM view of TEM window. (d) Enlarged LAADF-STEM view of SEM micrograph. Insets on right are corresponding SAED and stereographic projection figures for both matrix and twin. Key: Σ3 twins-red, FIB lift-out region-purple, coherent Σ3 boundary-red arrows, partial dislocations in matrix-MP, partial dislocations in twin-TP.
| Sample grain | Matrix | Twin | ||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Loading direction | [$\bar{5}5\bar{9}$] | [$\bar{4}8\bar{8}$] | ||||||||||||||
| Plane | Direction | m | Plane | Direction | m | |||||||||||
| Slip system | Symbol | h | k | l | u | v | w | Symbol | h | k | h | u | v | w | ||
| MF1 | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | 1 | 0 | 0.28 | TF1 | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | 1 | 0 | 0.14 | |
| MF2 | 1 | 0 | $\bar{1}$ | 0.11 | TF2 | 1 | 0 | $\bar{1}$ | 0.05 | |||||||
| MF3 | 0 | 1 | $\bar{1}$ | 0.39 | TF3 | 0 | 1 | $\bar{1}$ | 0.18 | |||||||
| MP4 | 1 | 1 | $\bar{2}$ | 0.29 | TP4 | 1 | 1 | $\bar{2}$ | 0.13 | |||||||
| MP5 | $\bar{1}$ | 2 | $\bar{1}$ | 0.39 | TP5 | $\bar{1}$ | 2 | $\bar{1}$ | 0.18 | |||||||
| MP6 | $\bar{2}$ | 1 | 1 | 0.10 | TP6 | $\bar{2}$ | 1 | 1 | 0.05 | |||||||
| MF7 | $\bar{1}$ | $\bar{1}$ | 1 | 1 | $\bar{1}$ | 0 | 0.28 | TF7 | $\bar{1}$ | $\bar{1}$ | 1 | 1 | $\bar{1}$ | 0 | 0.41 | |
| MF8 | 1 | 0 | 1 | 0.39 | TF8 | 1 | 0 | 1 | 0.41 | |||||||
| MF9 | 0 | 1 | 1 | 0.11 | TF9 | 0 | 1 | 1 | 0 | |||||||
| MP10 | 1 | 1 | 2 | 0.29 | TP10 | 1 | 1 | 2 | 0.24 | |||||||
| MP11 | 1 | $\bar{2}$ | $\bar{1}$ | 0.10 | TP11 | 1 | $\bar{2}$ | $\bar{1}$ | 0.24 | |||||||
| MP12 | 2 | $\bar{1}$ | 1 | 0.39 | TP12 | 2 | $\bar{1}$ | 1 | 0.47 | |||||||
| MF13 | $\bar{1}$ | 1 | $\bar{1}$ | 1 | 1 | 0 | 0 | TF13 | $\bar{1}$ | 1 | $\bar{1}$ | 1 | 1 | 0 | 0.23 | |
| MF14 | 1 | 0 | $\bar{1}$ | 0.24 | TF14 | 1 | 0 | $\bar{1}$ | 0.23 | |||||||
| MF15 | 0 | $\bar{1}$ | $\bar{1}$ | 0.24 | TF15 | 0 | $\bar{1}$ | $\bar{1}$ | 0 | |||||||
| MP16 | $\bar{1}$ | $\bar{2}$ | $\bar{1}$ | 0.14 | TP16 | 1 | 2 | 1 | 0.13 | |||||||
| MP17 | 1 | $\bar{1}$ | $\bar{2}$ | 0.27 | TP17 | 2 | 1 | $\bar{1}$ | 0.26 | |||||||
| MP18 | $\bar{2}$ | $\bar{1}$ | 1 | 0.14 | TP18 | 1 | $\bar{1}$ | $\bar{2}$ | 0.13 | |||||||
| MF19 | $\bar{1}$ | 1 | 1 | 1 | 1 | 0 | 0 | TF19 | $\bar{1}$ | 1 | 1 | 1 | 1 | 0 | 0.05 | |
| MF20 | $\bar{1}$ | 0 | $\bar{1}$ | 0.04 | TF20 | $\bar{1}$ | 0 | $\bar{1}$ | 0.14 | |||||||
| MF21 | 0 | $\bar{1}$ | 1 | 0.04 | TF21 | 0 | $\bar{1}$ | 1 | 0.18 | |||||||
| MP22 | 1 | 2 | $\bar{1}$ | 0.03 | TP22 | 1 | 2 | $\bar{1}$ | 0.13 | |||||||
| MP23 | $\bar{1}$ | 1 | $\bar{2}$ | 0.05 | TP23 | $\bar{1}$ | 1 | $\bar{2}$ | 0.18 | |||||||
| MP24 | 2 | 1 | 1 | 0.03 | TP24 | 2 | 1 | 1 | 0.05 | |||||||
Table. 1 The calculations of the Schmid factors for 24 possible slip systems in both matrix and twin. m refers to the Schmid factor.
| Sample grain | Matrix | Twin | ||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Loading direction | [$\bar{5}5\bar{9}$] | [$\bar{4}8\bar{8}$] | ||||||||||||||
| Plane | Direction | m | Plane | Direction | m | |||||||||||
| Slip system | Symbol | h | k | l | u | v | w | Symbol | h | k | h | u | v | w | ||
| MF1 | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | 1 | 0 | 0.28 | TF1 | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | $\bar{1}$ | 1 | 0 | 0.14 | |
| MF2 | 1 | 0 | $\bar{1}$ | 0.11 | TF2 | 1 | 0 | $\bar{1}$ | 0.05 | |||||||
| MF3 | 0 | 1 | $\bar{1}$ | 0.39 | TF3 | 0 | 1 | $\bar{1}$ | 0.18 | |||||||
| MP4 | 1 | 1 | $\bar{2}$ | 0.29 | TP4 | 1 | 1 | $\bar{2}$ | 0.13 | |||||||
| MP5 | $\bar{1}$ | 2 | $\bar{1}$ | 0.39 | TP5 | $\bar{1}$ | 2 | $\bar{1}$ | 0.18 | |||||||
| MP6 | $\bar{2}$ | 1 | 1 | 0.10 | TP6 | $\bar{2}$ | 1 | 1 | 0.05 | |||||||
| MF7 | $\bar{1}$ | $\bar{1}$ | 1 | 1 | $\bar{1}$ | 0 | 0.28 | TF7 | $\bar{1}$ | $\bar{1}$ | 1 | 1 | $\bar{1}$ | 0 | 0.41 | |
| MF8 | 1 | 0 | 1 | 0.39 | TF8 | 1 | 0 | 1 | 0.41 | |||||||
| MF9 | 0 | 1 | 1 | 0.11 | TF9 | 0 | 1 | 1 | 0 | |||||||
| MP10 | 1 | 1 | 2 | 0.29 | TP10 | 1 | 1 | 2 | 0.24 | |||||||
| MP11 | 1 | $\bar{2}$ | $\bar{1}$ | 0.10 | TP11 | 1 | $\bar{2}$ | $\bar{1}$ | 0.24 | |||||||
| MP12 | 2 | $\bar{1}$ | 1 | 0.39 | TP12 | 2 | $\bar{1}$ | 1 | 0.47 | |||||||
| MF13 | $\bar{1}$ | 1 | $\bar{1}$ | 1 | 1 | 0 | 0 | TF13 | $\bar{1}$ | 1 | $\bar{1}$ | 1 | 1 | 0 | 0.23 | |
| MF14 | 1 | 0 | $\bar{1}$ | 0.24 | TF14 | 1 | 0 | $\bar{1}$ | 0.23 | |||||||
| MF15 | 0 | $\bar{1}$ | $\bar{1}$ | 0.24 | TF15 | 0 | $\bar{1}$ | $\bar{1}$ | 0 | |||||||
| MP16 | $\bar{1}$ | $\bar{2}$ | $\bar{1}$ | 0.14 | TP16 | 1 | 2 | 1 | 0.13 | |||||||
| MP17 | 1 | $\bar{1}$ | $\bar{2}$ | 0.27 | TP17 | 2 | 1 | $\bar{1}$ | 0.26 | |||||||
| MP18 | $\bar{2}$ | $\bar{1}$ | 1 | 0.14 | TP18 | 1 | $\bar{1}$ | $\bar{2}$ | 0.13 | |||||||
| MF19 | $\bar{1}$ | 1 | 1 | 1 | 1 | 0 | 0 | TF19 | $\bar{1}$ | 1 | 1 | 1 | 1 | 0 | 0.05 | |
| MF20 | $\bar{1}$ | 0 | $\bar{1}$ | 0.04 | TF20 | $\bar{1}$ | 0 | $\bar{1}$ | 0.14 | |||||||
| MF21 | 0 | $\bar{1}$ | 1 | 0.04 | TF21 | 0 | $\bar{1}$ | 1 | 0.18 | |||||||
| MP22 | 1 | 2 | $\bar{1}$ | 0.03 | TP22 | 1 | 2 | $\bar{1}$ | 0.13 | |||||||
| MP23 | $\bar{1}$ | 1 | $\bar{2}$ | 0.05 | TP23 | $\bar{1}$ | 1 | $\bar{2}$ | 0.18 | |||||||
| MP24 | 2 | 1 | 1 | 0.03 | TP24 | 2 | 1 | 1 | 0.05 | |||||||
Fig. 2. Serial LAADF-STEM images for hierarchical twin boundaries during in-situ deformation. Rebound mechanisms for MP5 and MP12 slip systems during deformation from local strain of (a) 0%, (b) ~1.1%, (c) ~1.7%, and (d) ~4.4%. Nucleation and propagation of crack at triple junction between primary and secondary twins under strain of (e) ~8.9%, (f) ~13.9%, (g) ~15.6%, and (h) ~18.3%. Key: MP5-blue arrows, MP12-red arrows, position of the cleavage crack-black dashed area, tensile directions during deformation-vertical purple arrows.
Fig. 3. Strain-resolved LAADF-STEM images of response of coherent Σ3 boundary to twin-separation process, (a)-(h) under increasing strain of approximately 0-18.3%. In image (d), primary Σ3 boundary separates through formation of ITB into two distinct segments, Σ3-1 and Σ3-2. Key: tensile strain direction during in-situ deformation-light purple arrows, nucleation and propagation of SF bounded by partial dislocations-orange arrows, incoherent twin boundary-ITB Σ3.
Fig. 4. HRTEM analysis of twin-separation process at coherent Σ3 boundary under in-situ strain. (a) Low-magnification bright-field TEM image of hierarchical twin boundaries. (b-f) HRTEM images of positions marked in (a). Key: coherent ∑3 boundary-red, ITB ∑3-light blue, secondary ∑3 twin-green, HCP ɛ phase-dark blue, 9R structure-orange, and phase boundary of 9R-purple.
Fig. 5. TEM analysis of local grain rotation around hierarchical twin boundaries. Low-magnification bright-field TEM images of Σ9 boundary between matrix and secondary twin (a) before and (b) after strain. Inset in (b) shows corresponding LAADF-STEM image. (c) and (d) SAED images with beam direction parallel to <110> γ zone axis, corresponding to yellow dashed circles in (b). (e) Schematic of (c) and (d) showing local grain rotation before and after deformation. (f) HRTEM image of hierarchical twin boundaries with corresponding FFT patterns (Insets 1-3). Key: matrix before rotation-MO, matrix after rotation-MR, primary twin-T, secondary twin-ST.
Fig. 6. Macroscopic EBSD analysis of hierarchical twin boundaries in HEA. (a) EBSD image quality map showing twin boundaries and Σ9 boundary. (b) EBSD phase map of the same region. Misorientation profiles of (c) Σ9 and (d) Σ3 boundaries.
Fig. 7. Schematic of micro-deformation mechanisms of hierarchical twin boundaries under progressively increasing strain. (a) Matrix with SF prior to deformation. SF moves along MP5 slip system, with high Schmid factor (0.39). (b) Recombination of leading and trailing partial dislocations generates full dislocation (D1) at triple junction. (c) Twin-separation process initiates at triple junction via formation of ITB and forms a new full dislocation (D2) along MP12 slip system. (d) Movements of edge partial dislocations (b1) from ITB create 9R structure along one side of twin boundary (i.e., Σ3-1). Separation of newly formed full dislocation (D2) creates new SF along MP12 slip system. (e) Crack nucleated from triple junction point and HCP ε phases generates from phase boundary of 9R structure. HCP ε phase only forms along one side of coherent Σ3 boundary (i.e., Σ3-1). (f) Crack grows and propagates along MP12 slip system and eventually fractures. Key: full dislocation-D, stacking fault-SF, phase boundary of 9R structure-PB.
Fig. 8. (a-h) Serial LAADF-STEM images for cracking of twinned structure without hierarchical twin boundaries during progressively increasing in-situ deformation. The nucleation and propagation process of a crack inside a fully twinned HEA was revealed. Insets: (a) Enlarged LAADF-STEM view of coherent Σ3 boundaries; (b) SAEDs taken from orange and blue dashed circles; and (f) LAADF-STEM view of crack around coherent Σ3 boundaries and HCP ε phases. Key: coherent Σ3 boundaries-red dashed lines, slip direction of partial dislocations within the upper first grain-red arrows, slip trace of partial dislocations within the upper second grain-blue arrows.
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