Acta Metallurgica Sinica (English Letters) ›› 2025, Vol. 38 ›› Issue (11): 2001-2023.DOI: 10.1007/s40195-025-01910-5
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Yonghua Chen1, Zhenzhen Tian1, Fubing Yu1, Mingyi Wu1, Wenhui Yao1,2, Yuantai He1, Yuan Yuan1,2, Zhihui Xie3, Guozhi Wu4, Jiahao Wu5, Fusheng Pan1,2, Liang Wu1,2(
)
Received:2025-03-19
Revised:2025-04-28
Accepted:2025-05-14
Online:2025-11-10
Published:2025-08-19
Contact:
Liang Wu, wuliang@cqu.edu.cnYonghua Chen, Zhenzhen Tian, Fubing Yu, Mingyi Wu, Wenhui Yao, Yuantai He, Yuan Yuan, Zhihui Xie, Guozhi Wu, Jiahao Wu, Fusheng Pan, Liang Wu. Evaluation of Corrosion Resistance for ZIF-67@Co-M (M = Fe, Al, Ni) LDHs Composite Coatings Based on AZ31 Magnesium Alloy[J]. Acta Metallurgica Sinica (English Letters), 2025, 38(11): 2001-2023.
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Fig. 1 Preparation process of ZCM composite coatings
| NaNO3 (mol·L-1) | Co(NO3)2·6H2O (mol·L-1) | Fe(NO3)3·9H2O (mol·L-1) | Al(NO3)3 (mol·L-1) | Ni(NO3)3·6H2O (mol·L-1) | PH | Time (min) | Tem. (°C) | |
|---|---|---|---|---|---|---|---|---|
| ZCF | 0.1 | 0.16 | 0.05 | - | - | 12 | 720 | 125 |
| ZCA | 0.1 | 0.15 | - | 0.05 | - | 8 | 720 | 135 |
| ZCN | 0.1 | 0.15 | - | - | 0.05 | 9 | 720 | 135 |
Table 1 Conditions for preparing Co-M LDHs
| NaNO3 (mol·L-1) | Co(NO3)2·6H2O (mol·L-1) | Fe(NO3)3·9H2O (mol·L-1) | Al(NO3)3 (mol·L-1) | Ni(NO3)3·6H2O (mol·L-1) | PH | Time (min) | Tem. (°C) | |
|---|---|---|---|---|---|---|---|---|
| ZCF | 0.1 | 0.16 | 0.05 | - | - | 12 | 720 | 125 |
| ZCA | 0.1 | 0.15 | - | 0.05 | - | 8 | 720 | 135 |
| ZCN | 0.1 | 0.15 | - | - | 0.05 | 9 | 720 | 135 |
Fig. 2 Surface morphologies of coating specimens and their corresponding EDS element mapping: a MAO, b ZIF-67, c ZCF, d ZCA, e ZCN
Fig. 3 XRD results of various coating specimens
Fig. 4 FT-IR spectra of different coating specimens
Fig. 5 Full XPS spectra of different coatings (left) and scanning spectra of universal elements (right): a Mg 1s, b Al 2p, c C 1s, d N 1s, e O 1s, f P 2p
Fig. 6 XPS spectra of characteristic metal elements in different coatings: a1-a4 Co 2p, b Fe 2p, c Ni 2p
Fig. 7 Cross-sectional and related EDS results: a MAO, b ZIF-67, c ZCF, d ZCA, e ZCN
Fig. 8 a Nyquist plot, b |Z| versus frequency, c phase angle versus frequency, d used equivalent circuit models of various coating specimens immersed for 30 min
Fig. 9 a Nyquist plot, b |Z| versus frequency, c phase angle versus frequency immersed for 5 days a1-c1, 10 days a2-c2 and 15 days a3-c3
| Specimen | CPEf (Ω-1·Sn·cm-2) | nf | Rf (Ω·cm2) | CPEdl (Ω-1·Sn·cm-2) | ndl | Rct (Ω·cm2) | χ2 |
|---|---|---|---|---|---|---|---|
| MAO | 4.9 × 10-7 | 1.0 | 4.7 × 104 | 1.1 × 10-5 | 0.9 | 6.4 × 103 | 9.45 × 10-3 |
| ZIF-67 | 7.2 × 10-7 | 1.0 | 6.4 × 105 | 2.8 × 10-5 | 0.8 | 5.2 × 104 | 5.97 × 10-3 |
| ZCF | 1.6 × 10-8 | 0.9 | 3.8 × 106 | 4.0 × 10-6 | 0.6 | 8.2 × 105 | 4.27 × 10-3 |
| ZCA | 5.3 × 10-8 | 0.8 | 5.6 × 106 | 7.3 × 10-6 | 0.8 | 7.8 × 105 | 1.57 × 10-3 |
| ZCN | 9.7 × 10-7 | 0.7 | 1.4 × 106 | 8.5 × 10-6 | 1.0 | 6.5 × 105 | 1.93 × 10-3 |
Table 2 Fitting parameters in circuit models in Fig. 8
| Specimen | CPEf (Ω-1·Sn·cm-2) | nf | Rf (Ω·cm2) | CPEdl (Ω-1·Sn·cm-2) | ndl | Rct (Ω·cm2) | χ2 |
|---|---|---|---|---|---|---|---|
| MAO | 4.9 × 10-7 | 1.0 | 4.7 × 104 | 1.1 × 10-5 | 0.9 | 6.4 × 103 | 9.45 × 10-3 |
| ZIF-67 | 7.2 × 10-7 | 1.0 | 6.4 × 105 | 2.8 × 10-5 | 0.8 | 5.2 × 104 | 5.97 × 10-3 |
| ZCF | 1.6 × 10-8 | 0.9 | 3.8 × 106 | 4.0 × 10-6 | 0.6 | 8.2 × 105 | 4.27 × 10-3 |
| ZCA | 5.3 × 10-8 | 0.8 | 5.6 × 106 | 7.3 × 10-6 | 0.8 | 7.8 × 105 | 1.57 × 10-3 |
| ZCN | 9.7 × 10-7 | 0.7 | 1.4 × 106 | 8.5 × 10-6 | 1.0 | 6.5 × 105 | 1.93 × 10-3 |
| Specimen | |Z|0.01 Hz value (Ω·cm2) | |||
|---|---|---|---|---|
| Immersion for 30 min | Immersion for 5 days | Immersion for 10 days | Immersion for 15 days | |
| MAO | 9.5 × 103 | 1.8 × 103 | 1.1 × 103 | 2.3 × 102 |
| ZIF-67 | 4.7 × 105 | 3.6 × 103 | 1.3 × 103 | 1.2 × 103 |
| ZCF | 1.4 × 106 | 2.7 × 104 | 1.0 × 104 | 4.6 × 103 |
| ZCA | 9.4 × 105 | 2.5 × 104 | 5.3 × 103 | 2.7 × 103 |
| ZCN | 6.0 × 105 | 4.2 × 103 | 1.9 × 103 | 1.5 × 103 |
Table 3 |Z|0.01 Hz values of different coating specimens immersed for different time
| Specimen | |Z|0.01 Hz value (Ω·cm2) | |||
|---|---|---|---|---|
| Immersion for 30 min | Immersion for 5 days | Immersion for 10 days | Immersion for 15 days | |
| MAO | 9.5 × 103 | 1.8 × 103 | 1.1 × 103 | 2.3 × 102 |
| ZIF-67 | 4.7 × 105 | 3.6 × 103 | 1.3 × 103 | 1.2 × 103 |
| ZCF | 1.4 × 106 | 2.7 × 104 | 1.0 × 104 | 4.6 × 103 |
| ZCA | 9.4 × 105 | 2.5 × 104 | 5.3 × 103 | 2.7 × 103 |
| ZCN | 6.0 × 105 | 4.2 × 103 | 1.9 × 103 | 1.5 × 103 |
Fig. 10 Equivalent circuit used for fitting the EIS data of various coating specimens
| Immersion time | Specimen | CPEout (Ω-1·Sn·cm-2) | nout | CPEin (Ω-1·Sn·cm-2) | nin | Rout (Ω·cm2) | Rin (Ω·cm2) | CPEdl (Ω-1·Sn·cm-2) | ndl | Rct (Ω·cm2) | χ2 |
|---|---|---|---|---|---|---|---|---|---|---|---|
| 5 days | MAO | 1.3 × 10-6 | 1.0 | 5.2 × 10-6 | 0.8 | 1.6 × 104 | 1.9 × 104 | 9.9 × 10-5 | 0.9 | 1.4 × 103 | 9.45 × 10-3 |
| ZIF-67 | 9.2 × 10-6 | 1.0 | 8.4 × 10-6 | 0.9 | 2.3 × 105 | 3.0 × 105 | 3.5 × 10-5 | 0.3 | 1.5 × 104 | 5.97 × 10-3 | |
| ZCF | 3.6 × 10-7 | 0.9 | 3.8 × 10-7 | 0.7 | 1.8 × 106 | 2.1 × 106 | 8.9 × 10-6 | 0.3 | 4.7 × 105 | 4.27 × 10-3 | |
| ZCA | 8.9 × 10-7 | 0.3 | 5.6 × 10-7 | 1.0 | 2.5 × 106 | 1.3 × 106 | 7.8 × 10-6 | 0.8 | 3.3 × 105 | 1.57 × 10-3 | |
| ZCN | 6.4 × 10-6 | 0.3 | 6.2 × 10-6 | 0.9 | 8.3 × 105 | 2.7 × 106 | 6.4 × 10-6 | 1.0 | 2.8 × 105 | 1.93 × 10-3 | |
| 10 days | MAO | 7.4 × 10-6 | 0.7 | 1.1 × 10-6 | 0.8 | 3.2 × 104 | 5.2 × 105 | 2.1 × 10-4 | 0.9 | 4.2 × 102 | 8.6 × 10-4 |
| ZIF-67 | 2.4 × 10-6 | 0.8 | 2.7 × 10-7 | 0.9 | 3.8 × 104 | 1.9 × 106 | 9.4 × 10-4 | 1.0 | 8.6 × 103 | 9.0 × 10-4 | |
| ZCF | 7.1 × 10-6 | 0.6 | 1.9 × 10-7 | 0.8 | 3.3 × 106 | 4.9 × 106 | 3.4 × 10-6 | 0.6 | 9.6 × 104 | 1.1 × 10-3 | |
| ZCA | 9.0 × 10-7 | 0.9 | 7.5 × 10-7 | 0.7 | 3.6 × 106 | 3.7 × 106 | 1.0 × 10-6 | 0.6 | 8.8 × 104 | 4.4 × 10-3 | |
| ZCN | 9.9 × 10-6 | 0.7 | 7.3 × 10-6 | 0.9 | 1.8 × 106 | 2.6 × 106 | 9.5 × 10-5 | 0.8 | 7.8 × 104 | 8.1 × 10-4 | |
| 15 days | MAO | 4.4 × 10-6 | 0.9 | 3.6 × 10-6 | 0.8 | 4.9 × 104 | 6.2 × 105 | 1.2 × 10-3 | 1.0 | 1.0 × 102 | 2.9 × 10-3 |
| ZIF-67 | 3.5 × 10-6 | 0.8 | 6.9 × 10-7 | 0.6 | 3.8 × 105 | 3.0 × 106 | 8.5 × 10-3 | 0.6 | 2.8 × 103 | 2.2 × 10-3 | |
| ZCF | 4.4 × 10-6 | 0.6 | 1.6 × 10-7 | 0.9 | 4.7 × 106 | 6.1 × 106 | 7.2 × 10-5 | 0.7 | 5.7 × 104 | 2.7 × 10-4 | |
| ZCA | 3.1 × 10-6 | 0.9 | 4.2 × 10-7 | 1.0 | 3.3 × 106 | 4.9 × 106 | 3.2 × 10-5 | 0.7 | 3.3 × 104 | 4.4 × 10-3 | |
| ZCN | 5.2 × 10-6 | 0.8 | 3.0 × 10-6 | 0.7 | 4.1 × 106 | 2.7 × 106 | 1.6 × 10-5 | 0.9 | 1.9 × 104 | 3.8 × 10-3 |
Table 4 Fitting results of EIS (in Fig. 9) for each coating specimen immersed for various durations
| Immersion time | Specimen | CPEout (Ω-1·Sn·cm-2) | nout | CPEin (Ω-1·Sn·cm-2) | nin | Rout (Ω·cm2) | Rin (Ω·cm2) | CPEdl (Ω-1·Sn·cm-2) | ndl | Rct (Ω·cm2) | χ2 |
|---|---|---|---|---|---|---|---|---|---|---|---|
| 5 days | MAO | 1.3 × 10-6 | 1.0 | 5.2 × 10-6 | 0.8 | 1.6 × 104 | 1.9 × 104 | 9.9 × 10-5 | 0.9 | 1.4 × 103 | 9.45 × 10-3 |
| ZIF-67 | 9.2 × 10-6 | 1.0 | 8.4 × 10-6 | 0.9 | 2.3 × 105 | 3.0 × 105 | 3.5 × 10-5 | 0.3 | 1.5 × 104 | 5.97 × 10-3 | |
| ZCF | 3.6 × 10-7 | 0.9 | 3.8 × 10-7 | 0.7 | 1.8 × 106 | 2.1 × 106 | 8.9 × 10-6 | 0.3 | 4.7 × 105 | 4.27 × 10-3 | |
| ZCA | 8.9 × 10-7 | 0.3 | 5.6 × 10-7 | 1.0 | 2.5 × 106 | 1.3 × 106 | 7.8 × 10-6 | 0.8 | 3.3 × 105 | 1.57 × 10-3 | |
| ZCN | 6.4 × 10-6 | 0.3 | 6.2 × 10-6 | 0.9 | 8.3 × 105 | 2.7 × 106 | 6.4 × 10-6 | 1.0 | 2.8 × 105 | 1.93 × 10-3 | |
| 10 days | MAO | 7.4 × 10-6 | 0.7 | 1.1 × 10-6 | 0.8 | 3.2 × 104 | 5.2 × 105 | 2.1 × 10-4 | 0.9 | 4.2 × 102 | 8.6 × 10-4 |
| ZIF-67 | 2.4 × 10-6 | 0.8 | 2.7 × 10-7 | 0.9 | 3.8 × 104 | 1.9 × 106 | 9.4 × 10-4 | 1.0 | 8.6 × 103 | 9.0 × 10-4 | |
| ZCF | 7.1 × 10-6 | 0.6 | 1.9 × 10-7 | 0.8 | 3.3 × 106 | 4.9 × 106 | 3.4 × 10-6 | 0.6 | 9.6 × 104 | 1.1 × 10-3 | |
| ZCA | 9.0 × 10-7 | 0.9 | 7.5 × 10-7 | 0.7 | 3.6 × 106 | 3.7 × 106 | 1.0 × 10-6 | 0.6 | 8.8 × 104 | 4.4 × 10-3 | |
| ZCN | 9.9 × 10-6 | 0.7 | 7.3 × 10-6 | 0.9 | 1.8 × 106 | 2.6 × 106 | 9.5 × 10-5 | 0.8 | 7.8 × 104 | 8.1 × 10-4 | |
| 15 days | MAO | 4.4 × 10-6 | 0.9 | 3.6 × 10-6 | 0.8 | 4.9 × 104 | 6.2 × 105 | 1.2 × 10-3 | 1.0 | 1.0 × 102 | 2.9 × 10-3 |
| ZIF-67 | 3.5 × 10-6 | 0.8 | 6.9 × 10-7 | 0.6 | 3.8 × 105 | 3.0 × 106 | 8.5 × 10-3 | 0.6 | 2.8 × 103 | 2.2 × 10-3 | |
| ZCF | 4.4 × 10-6 | 0.6 | 1.6 × 10-7 | 0.9 | 4.7 × 106 | 6.1 × 106 | 7.2 × 10-5 | 0.7 | 5.7 × 104 | 2.7 × 10-4 | |
| ZCA | 3.1 × 10-6 | 0.9 | 4.2 × 10-7 | 1.0 | 3.3 × 106 | 4.9 × 106 | 3.2 × 10-5 | 0.7 | 3.3 × 104 | 4.4 × 10-3 | |
| ZCN | 5.2 × 10-6 | 0.8 | 3.0 × 10-6 | 0.7 | 4.1 × 106 | 2.7 × 106 | 1.6 × 10-5 | 0.9 | 1.9 × 104 | 3.8 × 10-3 |
Fig. 11 Tafel curves of specimens after immersion of a 30 min, b 15 days
| Specimen | Ecorr (VSCE) | icorr (A·cm-2) | |
|---|---|---|---|
| Immersed for 30 min | MAO | − 1.53 ± 0.16 | (3.82 ± 0.23) × 10-6 |
| ZIF-67 | − 1.72 ± 0.13 | (5.15 ± 0.19) × 10-7 | |
| ZCF | − 1.58 ± 0.22 | (7.76 ± 0.24) × 10-8 | |
| ZCA | − 1.55 ± 0.21 | (8.77 ± 0.21) × 10-8 | |
| ZCN | − 1.51 ± 0.18 | (1.97 ± 0.27) × 10-7 | |
| Immersed for 15 days | MAO | − 1.45 ± 0.15 | (4.86 ± 0.23) × 10-5 |
| ZIF-67 | − 1.47 ± 0.19 | (1.23 ± 0.18) × 10-5 | |
| ZCF | − 1.37 ± 0.20 | (1.45 ± 0.25) × 10-6 | |
| ZCA | − 1.45 ± 0.19 | (4.71 ± 0.23) × 10-6 | |
| ZCN | − 1.44 ± 0.17 | (1.21 ± 0.25) × 10-5 |
Table 5 Fitting parameters of Tafel polarization curves
| Specimen | Ecorr (VSCE) | icorr (A·cm-2) | |
|---|---|---|---|
| Immersed for 30 min | MAO | − 1.53 ± 0.16 | (3.82 ± 0.23) × 10-6 |
| ZIF-67 | − 1.72 ± 0.13 | (5.15 ± 0.19) × 10-7 | |
| ZCF | − 1.58 ± 0.22 | (7.76 ± 0.24) × 10-8 | |
| ZCA | − 1.55 ± 0.21 | (8.77 ± 0.21) × 10-8 | |
| ZCN | − 1.51 ± 0.18 | (1.97 ± 0.27) × 10-7 | |
| Immersed for 15 days | MAO | − 1.45 ± 0.15 | (4.86 ± 0.23) × 10-5 |
| ZIF-67 | − 1.47 ± 0.19 | (1.23 ± 0.18) × 10-5 | |
| ZCF | − 1.37 ± 0.20 | (1.45 ± 0.25) × 10-6 | |
| ZCA | − 1.45 ± 0.19 | (4.71 ± 0.23) × 10-6 | |
| ZCN | − 1.44 ± 0.17 | (1.21 ± 0.25) × 10-5 |
Fig. 12 Changes in HEV of different specimens under different immersing time
Fig. 13 Optical images of different specimens at different immersing time: a MAO, b ZIF-67, c ZCF, d ZCA, e ZCN
Fig. 14 SVET results of scratched specimens at varying time
Fig. 15 (I) Comparison of artificial scratched specimens, (II) EDS point scanning results of scratched area and complete surface: a MAO, b ZIF-67, c ZCF, d ZCA, e ZCN
Fig. 16 Corrosion resistance mechanisms of ZCM (ZCF, ZCA, ZCN) composite coatings
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