Influence of V and Zn in FeCrCuMnTi High-Entropy Alloys on Microstructures and Uniaxial Compaction Behavior Prepared by Mechanical Alloying
Abstract
:1. Introduction
2. Materials and Methods
3. Results
3.1. Phase Evolutions and Structural Characterization Using XRD
3.2. Microstructural Examinations Using HRSEM and HRTEM
3.3. Examination of Powder Particle Size, Distribution, Apparent Density, Tap Density, and True Density
3.4. Densification Behavior of FeCrCuMnTi, FeCrCuMnTiV, and FeCrCuMnTiVZn HEAs
4. Discussion
5. Conclusions
- ❖
- Three nanostructured equiatomic FeCrCuMnTi, FeCrCuMnTiV, and FeCrCuMnTiVZn HEAs exhibited multiple solid solutions with major FCC phases, minor BCC, and HCP phases evidenced through XRD, HRSEM, and HRTEM.
- ❖
- XRD results revealed that FeCrCuMnTiVZn HEA produced more crystallite size reduction, more lattice strain, and a high value of lattice constants due to more structural refinements and high configurational entropy due to incorporation Zn.
- ❖
- A greater powder particle size reduction (24.56 ± 1.85 μm) occurred in FeCrCuMnTiV HEA due to the domination of fracturing mechanisms produced by the addition of V atoms.
- ❖
- The densification performance indicates that the FeCrCuMnTiV HEA produced a higher relative density of 0.7456 in the as-milled condition and 0.8284 in the stress-recovered conditions. The stress-relieved powder samples exhibited a higher relative density compared to the as-milled powders owing to the elimination of lattice strain.
- ❖
- Based on the applied linear and non-linear models, Balshin’s Equation (1) and Heckel’s Equation (2) linear models are well-fitted linear models. Whereas, Shapiro’s Equation (6), and Cooper and Eaton’s Equation (7) non-linear models have produced regression coefficients of more than 0.99 indicating the good accuracy of non-linear models compared to linear models.
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Alloy Code | Alloy Composition (Atomic Fraction of Each Element) | LECO CS 744 and ONH 836 Analyzers (wt.%) | Crystallite Size (t), nm | Lattice Strain, % | Lattice Constant, nm | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
O | C | H | N | S | BCC | FCC | HCP | BCC | FCC | HCP | BCC | FCC | HCP | |||
‘a’ | ‘a’ | ‘a’ | ‘c’ | |||||||||||||
HEA1 | FeCrCuMnTi (0.2) | 0.68 | 0.45 | 0.08 | 0.09 | 0.005 | 18 | 9 | 31 | 0.97 | 0.95 | 1.5 | 0.485 | 0.361 | 0.296 | 0.483 |
HEA2 | FeCrCuMnTiV (0.167) | 0.75 | 0.62 | 0.09 | 0.10 | 0.004 | 24 | 10 | 48 | 0.96 | 0.92 | 2.9 | 0.491 | 0.363 | 0.300 | 0.490 |
HEA3 | FeCrCuMnTiVZn (0.143) | 0.82 | 0.74 | 0.12 | 0.09 | 0.001 | 14 | 6 | 22 | 1.1 | 0.98 | 5.6 | 0.502 | 0.365 | 0.308 | 0.503 |
Alloy Code | Equiatomic Composition | Fe | Cr | Cu | Mn | Ti | V | Zn |
---|---|---|---|---|---|---|---|---|
HEA1 | FeCrCuMnTi | 20.75 ± 0.06 | 19.95 ± 0.22 | 19.61 ± 0.20 | 19.95 ± 0.05 | 19.79 ± 0.06 | - | - |
HEA2 | FeCrCuMnTiV | 20.47 ± 0.29 | 16.52 ± 0.41 | 16.23 ± 0.65 | 15.89 ± 0.04 | 14.94 ± 0.15 | 15.95 ± 0.42 | |
HEA3 | FeCrCuMnTiVZn | 14.27 ± 0.11 | 15.16 ± 0.39 | 13.02 ± 0.38 | 14.19 ± 0.01 | 14.59 ± 0.22 | 15.59 ± 0.50 | 13.16 ± 0.60 |
High Entropy Alloy Powders | Powder Particle Size | Surface Area | Apparent Density | Tap Density | True Density | Packing at Apparent Density | Packing at Tapped Density (150 No. of Taps) | |||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
D10 (μm) | D50 (μm) | D90 (μm) | Davg (μm) | m2/kg | g/cm3 | g/cm3 | g/cm3 | % | % | |||||
As-Milled | Stress Recovered | As-Milled | Stress Recovered | As-Milled | Stress Recovered | As-Milled | Stress Recovered | |||||||
FeCrCuMnTi | 24.5 | 37 | 53.9 | 40.79 ± 1.84 | 16.35 | 2.60 ± 0.045 | 2.73 ± 0.053 | 3.30 ± 0.032 | 3.47 ± 0.028 | 6.22 ± 0.011 | 41.69 ± 0.563 | 43.68 ± 0.489 | 52.88 ± 0.657 | 55.52 ± 0.258 |
FeCrCuMnTiV | 16 | 23.9 | 37.9 | 26.78 ± 2.89 | 24.75 | 2.62 ± 0.015 | 2.75 ± 0.023 | 3.40 ± 0.013 | 3.58 ± 0.031 | 6.52 ± 0.018 | 39.98 ± 0.687 | 41.92 ± 0.202 | 51.96 ± 0.326 | 54.57 ± 0.272 |
FeCrCuMnTiVZn | 24.6 | 37.7 | 54.7 | 41.39 ± 1.20 | 16.14 | 2.49 ± 0.017 | 2.62 ± 0.032 | 3.08 ± 0.012 | 3.24 ± 0.024 | 6.64 ± 0.014 | 37.47 ± 0.723 | 39.39 ± 0.277 | 46.40 ± 0.468 | 49.08 ± 0.240 |
Alloy Composition | Theoretical Density (g/cm3) | Green Density (g/cm3) | Relative Density (%) | ||
---|---|---|---|---|---|
No Stress Recovery | Stress Recovered | No Stress Recovery | Stress Recovered | ||
FeCrCuMnTi | 6.25 | 4.29 | 4.93 | 68.56 | 78.85 |
FeCrCuMnTiV | 6.56 | 4.89 | 5.43 | 74.56 | 82.84 |
FeCrCuMnTiVZn | 6.65 | 4.50 | 5.01 | 67.65 | 75.45 |
Compaction Equation | Parameter | FeCrCuMnTi (HEA1) | FeCrCuMnTiV (HEA2) | FeCrCuMnTiVZn (HEA3) | |||
---|---|---|---|---|---|---|---|
WOS | WS | WOS | WS | WOS | WS | ||
Balshin Equation (6) | A | 3.09845 | 3.06949 | 2.95709 | 2.99541 | 3.34952 | 3.27144 |
K | −0.22402 | −0.24659 | −0.22102 | −0.24461 | −0.25754 | −0.26668 | |
R2 | 0.97874 | 0.97134 | 0.97807 | 0.96946 | 0.98668 | 0.97168 | |
Heckel’s Equation (7) | A | 0.59261 | 0.61384 | 0.64873 | 0.64299 | 0.5524 | 0.57058 |
K | 0.00050 | 0.00081 | 0.00062 | 0.00095 | 0.00051 | 0.00073 | |
R2 | 0.98885 | 0.99439 | 0.98671 | 0.98705 | 0.98654 | 0.99573 | |
Ge’s Equation (8) | A | −0.54121 | −0.61291 | −0.54458 | −0.62799 | −0.59842 | −0.63899 |
K | 0.18382 | 0.24233 | 0.20618 | 0.26160 | 0.19908 | 0.23788 | |
R2 | 0.93834 | 0.90832 | 0.93080 | 0.89714 | 0.94849 | 0.91319 | |
Panelli and Ambrosio Filho Equation (9) | A | 0.4522 | 0.39226 | 0.45956 | 0.37035 | 0.40766 | 0.37123 |
K | 0.01950 | 0.03141 | 0.02485 | 0.03703 | 0.02003 | 0.02817 | |
R2 | 0.98261 | 0.95769 | 0.97648 | 0.94458 | 0.98531 | 0.96354 | |
Kawakita’s Equation (10) | A | 2.71834 | 2.4562 | 2.54322 | 2.40788 | 2.54003 | 2.48555 |
K | 135.8672 | 120.53758 | 107.0222 | 112.97297 | 185.8354 | 146.22189 | |
R2 | 0.90689 | 0.88789 | 0.88034 | 0.8753 | 0.96324 | 0.9095 | |
Shapiro Equation (11) | A | −0.81222 | −0.90605 | −0.89129 | −0.98031 | −0.74443 | −0.8176 |
B | −6.89 × 10−4 | −6.468 × 10−4 | −8.507 × 10−4 | −4.75 × 10−4 | −6.970 × 10−4 | −6.342 × 10−4 | |
C | −1.55 × 10−7 | −1.013 × 10−6 | −3.736 × 10−7 | −1.663 × 10−6 | −1.342 × 10−7 | −7.2824 × 10−7 | |
R2 | 0.99059 | 0.99532 | 0.99021 | 0.99386 | 0.99002 | 0.99608 | |
Cooper and Eaton’s Equation (12) | a1 | 0.32711 | 0.34005 | 0.4907 | 0.57359 | 0.49666 | 0.5512 |
a2 | 0.49837 | 0.55277 | 0.3198 | 0.34613 | 0.38257 | 0.34836 | |
k1 | 79.0513 | 72.8862 | 826.446 | 800.000 | 961.5384 | 787.4015 | |
k2 | 961.5384 | 793.6507 | 71.9424 | 74.96251 | 77.16049 | 76.2195 | |
R2 | 0.9992 | 0.9994 | 0.99806 | 0.99938 | 0.9993 | 0.99946 | |
Van Der Zwan and Sisken’s Equation (13) | a | 0.46183 | 0.71326 | 0.54438 | 0.79743 | 0.46777 | 0.67931 |
k | 384.6153 | 505.0505 | 401.6064 | 526.3157 | 348.4320 | 500.000 | |
R2 | 0.95966 | 0.96511 | 0.95371 | 0.96607 | 0.95918 | 0.96667 |
Equiatomic Alloy Composition | ΔHmix, kJ/mol | Δsmix, J/mol·k | Melting Temp, °C | Ω | Atomic Radius Difference (δ), % | , J/mol | VEC | Expected Phases | Actual Observed Phases | PED (Δx) |
---|---|---|---|---|---|---|---|---|---|---|
FeCrCuMnTi | −1.76 | 13.38 | 1488 | 13.3930 | 1.44% | −5747.50 | 7.20 | BCC, FCC | BCC, FCC, HCP | 0.15 |
FeCrCuMnTiV | −2.00 | 14.90 | 1588 | 13.6441 | 1.70 | −6439.21 | 6.83 | BCC, FCC | BCC, FCC, HCP | 0.14 |
FeCrCuMnTiVZn | −2.53 | 16.18 | 1396 | 10.6883 | 1.79 | −7353.93 | 7.57 | BCC, FCC | BCC, FCC, HCP | 0.13 |
Element (Atomic Size, nm) | Fe | Cr | Cu | Mn | Ti | V | Zn |
---|---|---|---|---|---|---|---|
Fe (0.14) | - | −1 | 13 | 0 | −17 | −7 | 4 |
Cr (0.14) | - | - | 12 | 2 | −7 | −2 | 5 |
Cu (0.135) | - | - | - | 4 | −9 | 5 | 1 |
Mn (0.14) | - | - | - | - | −8 | −1 | −6 |
Ti (0.14) | - | - | - | - | - | −2 | −15 |
V (0.135) | - | - | - | - | - | - | −2 |
Zn (0.135) | - | - | - | - | - | - | - |
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Sivasankaran, S.; Al-Mufadi, F.A.; Ammar, H.R. Influence of V and Zn in FeCrCuMnTi High-Entropy Alloys on Microstructures and Uniaxial Compaction Behavior Prepared by Mechanical Alloying. Crystals 2021, 11, 1413. https://doi.org/10.3390/cryst11111413
Sivasankaran S, Al-Mufadi FA, Ammar HR. Influence of V and Zn in FeCrCuMnTi High-Entropy Alloys on Microstructures and Uniaxial Compaction Behavior Prepared by Mechanical Alloying. Crystals. 2021; 11(11):1413. https://doi.org/10.3390/cryst11111413
Chicago/Turabian StyleSivasankaran, Subbarayan, Fahad A. Al-Mufadi, and Hany R. Ammar. 2021. "Influence of V and Zn in FeCrCuMnTi High-Entropy Alloys on Microstructures and Uniaxial Compaction Behavior Prepared by Mechanical Alloying" Crystals 11, no. 11: 1413. https://doi.org/10.3390/cryst11111413