The Effects of Severe Plastic Deformation and/or Thermal Treatment on the Mechanical Properties of Biodegradable Mg-Alloys
Abstract
:1. Introduction
Biodegradable Mg Alloys
2. Experimental Procedure
2.1. Materials, Samples and Preparations
2.2. HPT-Processing
2.3. Heat Treatments
2.4. Characterization of Microstructure
2.4.1. Microhardness Tests
2.4.2. Tensile Tests
2.4.3. Electron Microscopy
2.4.4. Differential Scanning Calorimetry
2.4.5. X-ray Diffraction Peak Profile Analysis (XPA)
2.4.6. Corrosion Tests
3. Results
3.1. Achieving the Supersaturated Solid-Solution Condition
3.2. The Effect of Severe Plastic Deformation
3.3. The Effects of Isothermal Heat Treatments
3.4. Total Hardness Increase after Processing
3.5. Tensile Strength and Ductility
3.6. Evolution of Young’s Modulus
3.7. Electron Microscopy Analysis of Precipitate Structure Evolution
- (1)
- IS (furnace-cooled) and additionally HPT-deformed at 4 GPa for 0.5 rotations at RT;
- (2)
- IS (furnace-cooled) and HPT-deformed at 4 GPa for 0.5 rotations at RT and heat treated at 100 °C for 24 h;
- (3)
- IS (furnace-cooled) and HPT-deformed at 4 GPa for 0.5 rotations at RT and heat treated at 125 °C for 24 h.
3.8. Determination of SPD-Induced Defect Densities by DSC and XPA
3.9. Corrosion Tests
4. Discussion
4.1. The Effect of Solid-Solution Treatment
4.2. The Effect of High-Pressure-Torsion
4.3. The Effect of Post-HPT Heat Treatments on Strength
4.4. The Effect of Precipitates on Strength
4.5. The Effect of Vacancy Agglomerates on Strength
4.6. The Effects of Processing Routes on Corrosion Behavior
4.7. The Effects of Processing Routes on the Evolutions of Texture and Young’s Modulus
4.8. Tensile tests
5. Summary and Conclusions
- (1)
- Microhardness increases of up to 250% after furnace cooling, further processing by HPT and/or heat treatment could be reached.
- (2)
- After those treatments, SEM and STEM investigations revealed complex precipitates, which contribute only ~16% to the hardness increase; this is the result of estimations applying the Orowan equation for precipitation hardening.
- (3)
- Trying for the first time quantitative analyses of HPT-induced defects, DSC and XPA measurements were undertaken which showed very large concentrations of vacancies (up to ~10−3;) in the furnace-cooled/HPT-processed/heat-treated samples. These started to migrate/agglomerate/anneal at the very temperature (70–100 °C) at which the largest microhardness appeared. Kissinger analyses confirmed that conclusion, as they exhibit a vacancy migration enthalpy between Q = 0.7–1.3 eV which agrees well with literature values for Mg and Mg alloys.
- (4)
- Theoretical calculations using Kirchner’s model indicated that about 1% of the HPT-induced vacancies formed vacancy agglomerates which could account for the significant thermally-induced hardness increases.
- (5)
- Tensile tests showed that the samples were rather brittle due to the high number of vacancies after HPT deformation and heat treatment. Elongations did not exceed 5%.
- (6)
- The Young’s modulus varied slightly during the processing history because of deformation, thermal treatment and second phase formation due to the evolutions of deformation textures and precipitates, but still remained too small to cause stress shielding; its maximum increase with regard to the homogenized state amounted to 15%.
- (7)
- Corrosion tests showed that neither the formation of vacancy agglomerates, dislocations and grain boundaries nor that of precipitates has a significant effect on corrosion rate. Mainly, the composition of biomedical binary or ternary Mg-alloys controls the corrosion rate.
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Alloy | Mg (at%) | Zn (at%) | Ca (at%) | Zr (at%) |
---|---|---|---|---|
Mg5Zn0.3Ca | 94.28 ± 0.03 | 5.44 ± 0.03 | 0.28 ± 0.03 | - |
Mg5Zn | 94.77 ± 0.03 | 5.23 ± 0.03 | - | - |
Mg0.3Ca | 99.73 ± 0.03 | - | 0.27 ± 0.03 | - |
Mg5Zn0.15Ca | 94.90 ± 0.03 | 5.1 ± 0.03 | 0.15 ± 0.03 | - |
Mg5Zn0.15Ca0.15Zr | 94.40 ± 0.03 | 5.6 ± 0.03 | 0.18 ± 0.03 | 0.18 ± 0.03 |
Alloy | Mg (at%) | Zn (at%) | Ca (at%) |
---|---|---|---|
Mg5Zn0.3Ca | 65 ± 5 | 31 ± 7 | 4 ± 1 |
Mg5Zn | 76 ± 4 | 24 ± 3 | - |
Mg0.3Ca | 90 ± 1 | - | 10 ± 1 |
Mg5Zn0.15Ca | 28 ± 6 | 70 ± 5 | 3 ± 1 |
Mg5Zn0.15Ca0.15Zr | 24 ± 5 | 72 ± 5 | 4 ± 1 |
Alloy | HV0.05 as-Cast | HV0.05 Furnace-Cooled | HV0.05 Quenched |
---|---|---|---|
Mg5Zn0.3Ca | 65 ± 6 | 58 ± 1 | 70 ± 2 |
Mg5Zn | 70 ± 9 | 55 ± 2 | 76 ± 4 |
Mg0.3Ca | 50 ± 3 | 47 ± 1 | 54 ± 3 |
Mg5Zn0.15Ca | 77 ± 2 | 78 ± 3 | 83 ± 5 |
Mg5Zn0.15Ca0.15Zr | 78 ± 4 | 74 ± 3 | 76 ± 3 |
Alloy | Condition | σyield (MPa) | UTS (MPa) | εtotal (%) |
---|---|---|---|---|
Mg5Zn0.3Ca | IS | 70 ± 10 | 153 ± 10 | 15 ± 1 |
IS + HT | 95 ± 15 | 175 ± 19 | 14 ± 2 | |
HPT (0.5) | 163 ± 36 | 221 ± 21 | 7 ± 2 | |
HPT (0.5) + HT | 303 ± 35 | 310 ± 55 | 5 ± 1 | |
HPT (2) | 55 ± 16 | 55 ± 16 | 1 ± 0.1 | |
HPT (2) + HT | 209 ± 45 | 209 ± 45 | 4 ± 1 | |
Mg5Zn | IS | 90 ± 10 | 174 ± 57 | 17 ± 3 |
IS + HT | 155 ± 15 | 180 ± 28 | 17 ± 3 | |
HPT (0.5) | 280 ± 10 | 303 ± 20 | 5 ± 1 | |
HPT (0.5) + HT | 310 ± 26 | 329 ± 36 | 5 ± 1 | |
HPT (2) | 280 ± 22 | 280 ± 22 | 6 ± 1 | |
HPT (2) + HT | 185 ± 51 | 185 ± 51 | 5 ± 1 | |
Mg0.3Ca | IS | 36 ± 20 | 92 ± 4 | 18 ± 6 |
IS + HT | 24 ± 9 | 57 ± 10 | 30 ± 10 | |
HPT (0.5) | 210 ± 26 | 222 ± 28 | 10 ± 2 | |
HPT (0.5) + HT | 245 ± 5 | 250 ± 2 | 5 ± 2 | |
HPT (2) | 202 ± 20 | 206 ± 17 | 14 ± 3 | |
HPT (2) + HT | 255 ± 42 | 258 ± 39 | 6 ± 1 | |
Mg5Zn0.15Ca | IS | 120 ± 5 | 339 ± 40 | 17 ± 4 |
IS + HT | 94 ± 12 | 180 ± 25 | 16 ± 2 | |
HPT (0.5) | 246 ± 15 | 285 ± 19 | 7 ± 2 | |
HPT (0.5) + HT | 265 ± 5 | 268 ± 22 | 6 ± 1 | |
HPT (2) | 306 ± 22 | 306 ± 22 | 6 ± 2 | |
HPT (2) + HT | 395 ± 25 | 418 ± 25 | 5 ± 1 | |
Mg5Zn0.15Ca0.15Zr | IS | 165 ± 15 | 266 ± 49 | 15 ± 2 |
IS + HT | 180 ± 40 | 204 ± 27 | 17 ± 4 | |
HPT (0.5) | 230 ± 10 | 224 ± 82 | 6 ± 1 | |
HPT (0.5) + HT | 280 ± 10 | 285 ± 20 | 5 ± 1 | |
HPT (2) | 303 ± 40 | 309 ± 24 | 5 ± 1 | |
HPT (2) + HT | 270 ± 10 | 292 ± 24 | 7 ± 2 |
Alloy | Condition | E (GPa) |
---|---|---|
Mg5Zn0.3Ca | IS | 43 ± 1 |
IS + HT | 42 ± 3 | |
HPT (0.5) | 44 ± 1 | |
HPT (0.5) + HT | 47 ± 2 | |
HPT (2) | 50 ± 5 | |
HPT (2) + HT | 37 ± 3 | |
Mg5Zn | IS | 44 ± 4 |
IS + HT | 46 ± 3 | |
HPT (0.5) | 50 ± 4 | |
HPT (0.5) + HT | 46 ± 2 | |
HPT (2) | 45 ± 3 | |
Mg0.3Ca | IS | 32 ± 1 |
IS + HT | 33 ± 2 | |
HPT (0.5) | 40 ± 2 | |
HPT (0.5) + HT | 43 ± 1 | |
HPT (2) + HT | 33 ± 4 | |
Mg5Zn0.15Ca | IS | 44 ± 2 |
IS + HT | 35 ± 5 | |
HPT (0.5) | 37 ± 3 | |
HPT (0.5) + HT | 32 ± 2 | |
HPT (2) | 45 ± 2 | |
HPT (2) + HT | 46 ± 3 | |
Mg5Zn0.15Ca0.15Zr | IS | 40 ± 3 |
IS + HT | 40 ± 2 | |
HPT (0.5) | 42 ± 2 | |
HPT (0.5) + HT | 37 ± 2 | |
HPT (2) | 44 ± 2 | |
HPT (2) + HT | 45 ± 3 |
Sample | Etotal (J/g) | ρ (m−2) | Edisl (J/g) | Evac (J/g) | cv |
---|---|---|---|---|---|
Mg5Zn0.3Ca | 9.7 ± 2 | 1.1 × 1014 ± 1013 | 0.06 ± 0.02 | 9.6 ± 2 | 2 × 103 ± 1 × 10−4 |
Mg5Zn | 5.1 ± 0.5 | 2.0 × 1014 ± 1013 | 0.10 ± 0.05 | 5.1 ± 0.5 | 1 × 10−3 ± 1 × 10−4 |
Mg5Zn0.15Ca | 8.2 ± 0.7 | 2.0 × 1014 ± 1013 | 0.05 ± 0.01 | 8.2 ± 0.8 | 2 × 10−3 ± 2 × 10−4 |
Mg5Zn0.15Ca0.15Zr | 5.4 ± 0.2 | 1.6 × 1014 ± 1013 | 0.02 ± 0.01 | 5.4 ± 0.3 | 1 × 10−3 ± 9 × 10−5 |
Mg0.3Ca | 1.7 ± 0.5 | 3.1 × 1014 ± 1013 | 0.05 ± 0.01 | 1.7 ± 0.5 | 5 × 10−4 ± 1 × 10−4 |
Sample | Etotal (J/g) | ρ (m−2) | Edisl (J/g) | Evac (J/g) | cv |
---|---|---|---|---|---|
Mg5Zn0.3Ca | 3.0 ± 0.5 | 4.1 × 1014 ± 1013 | 0.2 ± 0.1 | 2.7 ± 0.3 | 8 × 10−4 ± 1 × 10−4 |
Mg5Zn | 1.5 ± 0.2 | 4.4 × 1014 ± 1013 | 0.3 ± 0.1 | 1.0 ± 0.1 | 3 × 10−4 ± 1 × 10−4 |
Mg5Zn0.15Ca | 0.8 ± 0.1 | 3.6 × 1014 ± 1013 | 0.4 ± 0.1 | 0.4 ± 0.1 | 1 × 10−4 ± 9 × 10−5 |
Mg5Zn0.15Ca0.15Zr | 1.5 ± 0.01 | 3.5 × 1014 ± 1013 | 0.3 ± 0.1 | 1.1 ± 0.1 | 3 × 10−4 ± 2 × 10−5 |
Mg0.3Ca | 0.7 ± 0.1 | 2.2 × 1014 ± 1013 | 0.2 ± 0.01 | 0.5 ± 0.1 | 1 × 10−4 ± 1 × 10−5 |
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Ojdanic, A.; Horky, J.; Mingler, B.; Fanetti, M.; Gardonio, S.; Valant, M.; Sulkowski, B.; Schafler, E.; Orlov, D.; J. Zehetbauer, M. The Effects of Severe Plastic Deformation and/or Thermal Treatment on the Mechanical Properties of Biodegradable Mg-Alloys. Metals 2020, 10, 1064. https://doi.org/10.3390/met10081064
Ojdanic A, Horky J, Mingler B, Fanetti M, Gardonio S, Valant M, Sulkowski B, Schafler E, Orlov D, J. Zehetbauer M. The Effects of Severe Plastic Deformation and/or Thermal Treatment on the Mechanical Properties of Biodegradable Mg-Alloys. Metals. 2020; 10(8):1064. https://doi.org/10.3390/met10081064
Chicago/Turabian StyleOjdanic, Andrea, Jelena Horky, Bernhard Mingler, Mattia Fanetti, Sandra Gardonio, Matjaz Valant, Bartosz Sulkowski, Erhard Schafler, Dmytro Orlov, and Michael J. Zehetbauer. 2020. "The Effects of Severe Plastic Deformation and/or Thermal Treatment on the Mechanical Properties of Biodegradable Mg-Alloys" Metals 10, no. 8: 1064. https://doi.org/10.3390/met10081064