J. Mater. Sci. Technol. ›› 2022, Vol. 98: 219-232.DOI: 10.1016/j.jmst.2021.05.010
• Research Article • Previous Articles Next Articles
W. Wang X.a,b, W. Wanga,b,*(
), W. Chena,b, M. Chen D.a,b,*()
Received:2021-03-15
Revised:2021-04-26
Accepted:2021-05-20
Published:2022-01-30
Online:2022-01-25
Contact:
W. Wang,M. Chen D.
About author:demin.chen.1@imr.ac.cn (D.M. Chen).W. Wang X., W. Wang, W. Chen, M. Chen D.. Effect of Al addition and heat treatment on the microstructures and corrosion resistance of Mg-Cu alloys[J]. J. Mater. Sci. Technol., 2022, 98: 219-232.
| Alloy (wt.%) | Name | Solution treatment | Aging | |||
|---|---|---|---|---|---|---|
| Temperature (°C) | Time (h) | Temperature (°C) | Time (h) | |||
| Mg-3Cu | CA0 | S1 | 450 | 20 | - | - |
| A1 | 450 | 20 | 200 | 12 | ||
| Mg-3Cu-4Al | CA4 | S2 | 400 | 20 | - | - |
| A2 | 400 | 20 | 200 | 6 | ||
| Mg-3Cu-8Al | CA8 | S3 | 400 | 20 | - | - |
| A3 | 400 | 20 | 200 | 6 |
Table 1 Summary of nomenclature and heat treatment protocols of the investigated alloys.
| Alloy (wt.%) | Name | Solution treatment | Aging | |||
|---|---|---|---|---|---|---|
| Temperature (°C) | Time (h) | Temperature (°C) | Time (h) | |||
| Mg-3Cu | CA0 | S1 | 450 | 20 | - | - |
| A1 | 450 | 20 | 200 | 12 | ||
| Mg-3Cu-4Al | CA4 | S2 | 400 | 20 | - | - |
| A2 | 400 | 20 | 200 | 6 | ||
| Mg-3Cu-8Al | CA8 | S3 | 400 | 20 | - | - |
| A3 | 400 | 20 | 200 | 6 |
| Alloy | Cu | Al | Fe | Ni | Si | Mg |
|---|---|---|---|---|---|---|
| Mg-3Cu | 2.98 | - | 0.005 | 0.024 | 0.016 | Bal. |
| Mg-3Cu-4Al | 2.99 | 3.91 | 0.006 | 0.001 | 0.015 | Bal. |
| Mg-3Cu-8Al | 2.68 | 7.58 | 0.009 | 0.001 | 0.014 | Bal. |
Table 2 Actual chemical composition (wt.%) detected by ICP-AES of the investigated alloys.
| Alloy | Cu | Al | Fe | Ni | Si | Mg |
|---|---|---|---|---|---|---|
| Mg-3Cu | 2.98 | - | 0.005 | 0.024 | 0.016 | Bal. |
| Mg-3Cu-4Al | 2.99 | 3.91 | 0.006 | 0.001 | 0.015 | Bal. |
| Mg-3Cu-8Al | 2.68 | 7.58 | 0.009 | 0.001 | 0.014 | Bal. |
Fig. 1. XRD patterns of the cast and annealed CA0, CA4 and CA8 alloys.
Fig. 2. SEM images of the cast alloys: (a) CA0, (b) CA4, and (c) CA8; insets are their enlarged images; (d, e) SEM images and element distributions of CA4 and CA8 alloys, respectively.
| Sample | Spectrum | Element (at.%) | ||
|---|---|---|---|---|
| Mg | Al | Cu | ||
| CA0 | 1 | 83.6 | - | 16.4 |
| CA4 | 2 | 73.25 | 12.39 | 14.36 |
| 3 | 78.4 | 20.73 | 0.87 | |
| CA8 | 4 | 74.02 | 12.97 | 13.01 |
| 5 | 67.95 | 30.67 | 1.38 |
Table 3 Compositions of cast CA0, CA4 and CA8 alloys corresponding to Fig. 2 obtained by EDX.
| Sample | Spectrum | Element (at.%) | ||
|---|---|---|---|---|
| Mg | Al | Cu | ||
| CA0 | 1 | 83.6 | - | 16.4 |
| CA4 | 2 | 73.25 | 12.39 | 14.36 |
| 3 | 78.4 | 20.73 | 0.87 | |
| CA8 | 4 | 74.02 | 12.97 | 13.01 |
| 5 | 67.95 | 30.67 | 1.38 |
Fig. 3. (a, b) typical TEM images of cast CA4 alloy, (c) electron diffraction pattern of interfacial phase.
Fig. 4. SEM images of the annealed alloys: (a) S1, (b) A1, (c) S2, (d) A2, (e) S3, (f) A3.
Fig. 5. Cu and Al contents in α-Mg of the cast and annealed alloys: 1, cast; 2, T4 (350 °C, 10 h); 3, T4 (350 °C, 20 h); 4, T4 (400 °C, 20 h); 5, T4 (450 °C, 20 h); 6, T6: CA0 (450 °C, 20 h/200 °C, 12 h); CA4 and CA8 (400 °C, 20 h/200 °C, 6 h).
Fig. 6. Weight loss rates of (a) cast alloys at different temperatures, (b) annealed alloys at room temperature.
Fig. 7. SEM surface images of the cast alloys after immersion in 3.5 wt.% NaCl solution for different time: (a, d) CA0, 1 min; (b, e) CA4,1 min; (c, f) CA8, 1 min; (g) CA0, 1 h; (h) CA4, 1 h; (i) CA8, 1 h. (j), (k), and (l) are cross-section images of (g), (h), and (i), respectively. (m) XRD patterns and (n, o) XPS spectra of Al 2p (n) and Cu 2p (o) of corrosion products of the cast CA0, CA4 and CA8 alloys.
Fig. 8. Polarization curves of (a) CA0, CA4, S2 and A2 alloys and (b) CA8, S3 and A3 alloys in 3.5 wt.% NaCl solution at room temperature.
| Sample | Ecorr (VSCE) | -bc (mV/decade) | icorr (mA cm-2) |
|---|---|---|---|
| CA0 | -1.486±0.005 | 442.1 ± 18.4 | 2.69 ± 0.17 |
| CA4 | -1.481±0.005 | 279.6 ± 18.1 | 0.97 ± 0.19 |
| S2 | -1.424±0.004 | 232.2 ± 9.2 | 0.73 ± 0.02 |
| A2 | -1.452±0.01 | 224.9 ± 2.5 | 0.87 ± 0.007 |
| CA8 | -1.477±0.006 | 263.4 ± 9.1 | 0.64 ± 0.03 |
| S3 | -1.478±0.010 | 257.1 ± 2.9 | 0.65 ± 0.17 |
| A3 | -1.493±0.011 | 264.8 ± 13.3 | 0.83 ± 0.18 |
Table 4 Fitting results of polarization curves in 3.5 wt.% NaCl solution.
| Sample | Ecorr (VSCE) | -bc (mV/decade) | icorr (mA cm-2) |
|---|---|---|---|
| CA0 | -1.486±0.005 | 442.1 ± 18.4 | 2.69 ± 0.17 |
| CA4 | -1.481±0.005 | 279.6 ± 18.1 | 0.97 ± 0.19 |
| S2 | -1.424±0.004 | 232.2 ± 9.2 | 0.73 ± 0.02 |
| A2 | -1.452±0.01 | 224.9 ± 2.5 | 0.87 ± 0.007 |
| CA8 | -1.477±0.006 | 263.4 ± 9.1 | 0.64 ± 0.03 |
| S3 | -1.478±0.010 | 257.1 ± 2.9 | 0.65 ± 0.17 |
| A3 | -1.493±0.011 | 264.8 ± 13.3 | 0.83 ± 0.18 |
Fig. 9. EIS of alloys after immersion in 3.5 wt.% NaCl solution for different time at room temperature: (a, d, g) Nyquist plots; (b, e, h) Bode impedance magnitude plots; (c, f, i) Bode phase angle plots; (j) and (k) are enlarged images of (d) and (g), respectively.
Fig. 10. Equivalent circuits of the cast alloys after immersion in 3.5 wt.% NaCl solution for different time. (a) CA0, 30 min; (b-d) CA4, from 5 min to 4 h; (c, d) CA8, from 5 min to 4 h..
| Sample | Time | Rs (Ω cm2) | Rc (Ω cm2) | Qc (Ω-1 cm-2 s - n) | nc | Rf (Ω cm2) | Cf (F cm-2) | R1 (Ω cm2) | L1 (H cm2) | R2 (Ω cm2) | L2 (H cm2) | RL (Ω cm2) | CL (F cm-2) | nH |
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| CA0 | 30 min | 5.54 | 8.1 | 2.50 × 10-4 | 0.99 | 1.1 | 1.27 | - | - | - | - | a2.91 | a2.52 × 10-5 | 0.67 |
| CA4 | 5 min | 4.15 | 66.8 | 9.04 × 10-6 | 0.96 | 9.0 | 3 × 10-3 | 42.8 | 26.66 | - | - | - | - | - |
| 10 min | 5.44 | 43.7 | 9.26 × 10-6 | 0.94 | 4.0 | 1 × 10-2 | 39.8 | 14.74 | 31.8 | 183.2 | - | - | - | |
| 1 h | 3.14 | 15.7 | 2.90 × 10-5 | 1.00 | 1.8 | 1.34 × 10-2 | 23.4 | 7.29 | 14.5 | 50.7 | - | - | - | |
| 2 h | 3.01 | 4.8 | 5.18 × 10-5 | 0.99 | 0.6 | 4.78 × 10-2 | 17.2 | 1.81 | 22.7 | 13.4 | - | - | - | |
| 3 h | 3.39 | 3.0 | 5.62 × 10-5 | 0.95 | 0.9 | 6 × 10-2 | 8.7 | 0.67 | - | - | 0.22 | 16.36 | - | |
| 4 h | 4.20 | 2.7 | 5.41 × 10-5 | 0.93 | 0.5 | 8.4 × 10-2 | 10.4 | 0.81 | - | - | 0.27 | 15.55 | - | |
| CA8 | 5 min | 2.41 | 103.4 | 7.19 × 10-6 | 0.96 | 24.9 | 4.4 × 10-4 | 208.7 | 38.30 | 83.3 | 215.8 | - | - | - |
| 10 min | 4.04 | 108.3 | 4.55 × 10-6 | 0.94 | 31.4 | 3.6 × 10-4 | 323.7 | 53.49 | 210.1 | 359.7 | - | - | - | |
| 1 h | 4.05 | 43.3 | 5.43 × 10-6 | 0.93 | 7.8 | 1.6 × 10-3 | 126.6 | 17.90 | 92.1 | 174.1 | - | - | - | |
| 2 h | 4.25 | 16.3 | 7.64 × 10-6 | 0.87 | 2.5 | 7.2 × 10-3 | 45.6 | 6.42 | 38.5 | 64.9 | - | - | - | |
| 3 h | 4.30 | 8.1 | 1.37 × 10-5 | 0.84 | 1.4 | 1.6 × 10-2 | 24.4 | 2.99 | 37.0 | 33.9 | - | - | - | |
| 4 h | 4.53 | 5.8 | 2.72 × 10-5 | 0.86 | 0.6 | 2.8 × 10-2 | 18.8 | 3.48 | - | - | 0.59 | 24.74 | - | |
| 5 h | 4.63 | 5.7 | 3.06 × 10-5 | 0.85 | 0.6 | 3.9 × 10-2 | 24.7 | 3.99 | - | - | 0.69 | 17.86 | - |
Table 5 Fitting parameters of EIS obtained from equivalent circuits of the cast CA0, CA4 and CA8 alloys.
| Sample | Time | Rs (Ω cm2) | Rc (Ω cm2) | Qc (Ω-1 cm-2 s - n) | nc | Rf (Ω cm2) | Cf (F cm-2) | R1 (Ω cm2) | L1 (H cm2) | R2 (Ω cm2) | L2 (H cm2) | RL (Ω cm2) | CL (F cm-2) | nH |
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| CA0 | 30 min | 5.54 | 8.1 | 2.50 × 10-4 | 0.99 | 1.1 | 1.27 | - | - | - | - | a2.91 | a2.52 × 10-5 | 0.67 |
| CA4 | 5 min | 4.15 | 66.8 | 9.04 × 10-6 | 0.96 | 9.0 | 3 × 10-3 | 42.8 | 26.66 | - | - | - | - | - |
| 10 min | 5.44 | 43.7 | 9.26 × 10-6 | 0.94 | 4.0 | 1 × 10-2 | 39.8 | 14.74 | 31.8 | 183.2 | - | - | - | |
| 1 h | 3.14 | 15.7 | 2.90 × 10-5 | 1.00 | 1.8 | 1.34 × 10-2 | 23.4 | 7.29 | 14.5 | 50.7 | - | - | - | |
| 2 h | 3.01 | 4.8 | 5.18 × 10-5 | 0.99 | 0.6 | 4.78 × 10-2 | 17.2 | 1.81 | 22.7 | 13.4 | - | - | - | |
| 3 h | 3.39 | 3.0 | 5.62 × 10-5 | 0.95 | 0.9 | 6 × 10-2 | 8.7 | 0.67 | - | - | 0.22 | 16.36 | - | |
| 4 h | 4.20 | 2.7 | 5.41 × 10-5 | 0.93 | 0.5 | 8.4 × 10-2 | 10.4 | 0.81 | - | - | 0.27 | 15.55 | - | |
| CA8 | 5 min | 2.41 | 103.4 | 7.19 × 10-6 | 0.96 | 24.9 | 4.4 × 10-4 | 208.7 | 38.30 | 83.3 | 215.8 | - | - | - |
| 10 min | 4.04 | 108.3 | 4.55 × 10-6 | 0.94 | 31.4 | 3.6 × 10-4 | 323.7 | 53.49 | 210.1 | 359.7 | - | - | - | |
| 1 h | 4.05 | 43.3 | 5.43 × 10-6 | 0.93 | 7.8 | 1.6 × 10-3 | 126.6 | 17.90 | 92.1 | 174.1 | - | - | - | |
| 2 h | 4.25 | 16.3 | 7.64 × 10-6 | 0.87 | 2.5 | 7.2 × 10-3 | 45.6 | 6.42 | 38.5 | 64.9 | - | - | - | |
| 3 h | 4.30 | 8.1 | 1.37 × 10-5 | 0.84 | 1.4 | 1.6 × 10-2 | 24.4 | 2.99 | 37.0 | 33.9 | - | - | - | |
| 4 h | 4.53 | 5.8 | 2.72 × 10-5 | 0.86 | 0.6 | 2.8 × 10-2 | 18.8 | 3.48 | - | - | 0.59 | 24.74 | - | |
| 5 h | 4.63 | 5.7 | 3.06 × 10-5 | 0.85 | 0.6 | 3.9 × 10-2 | 24.7 | 3.99 | - | - | 0.69 | 17.86 | - |
Fig. 11. The relation of Rp with immersion time for CA4 and CA8 alloys.
Fig. 12. SEM images, surface potential maps, and potential profiles of cast alloys: (a-c) CA0; (d-f) CA4; (g-i) CA8.
| Sample | Mg2Cu | MgAlCu | Mg17Al12 |
|---|---|---|---|
| CA0 | +937 ± 44 | - | - |
| CA4 | - | +1034 ± 51 | - |
| CA8 | - | +877 ± 46 | +164 ± 46 |
Table 6 ΔVPD values (mV) of interfacial phases with respect to the Mg matrix of investigated alloys.
| Sample | Mg2Cu | MgAlCu | Mg17Al12 |
|---|---|---|---|
| CA0 | +937 ± 44 | - | - |
| CA4 | - | +1034 ± 51 | - |
| CA8 | - | +877 ± 46 | +164 ± 46 |
Fig. 13. Volume fraction of the second phases of alloys before and after heat treatment.
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