J. Mater. Sci. Technol. ›› 2021, Vol. 92: 225-235.DOI: 10.1016/j.jmst.2021.03.021
• Research Article • Previous Articles
Ting Hua, Yuejun Ouyangb, Zhi-Hui Xiea,*(), Liang Wuc
Received:
2020-11-21
Revised:
2021-01-25
Accepted:
2021-03-07
Published:
2021-11-30
Online:
2021-05-08
Contact:
Zhi-Hui Xie
About author:
* E-mail address: zhxie@cwnu.edu.cn (Z.-H. Xie).Ting Hu, Yuejun Ouyang, Zhi-Hui Xie, Liang Wu. One-pot scalable in situ growth of highly corrosion-resistant MgAl-LDH/MBT composite coating on magnesium alloy under mild conditions[J]. J. Mater. Sci. Technol., 2021, 92: 225-235.
Fig. 1. Schematic diagram for preparation of blank, MBT, MgAl-LDH, and MgAl-LDH/MBT coatings using same process but different compositions of solutions.
Fig. 2. Digital photographs of (a) blank, (b) MBT, (c) MgAl-LDH, (d) MgAl-LDH/MBT coatings prepared with different reaction times at 95 °C and one atmospheric pressure.
Fig. 3. SEM images showing the microscopic morphologies of (a, b) blank, (c, d) MBT, (e, f, g) MgAl-LDH, and (h, i, j) MgAl-LDH/MBT coatings obtained at optimal reaction time. The insets in (f) and (i) are the corresponding TEM images of MgAl-LDH and MgAl-LDH/MBT coatings. The optimal reaction time is 8 h for blank and MBT samples, and 24 h for MgAl-LDH and MgAl-LDH/MBT samples.
Samples | Mg | Al | O | C | N | S |
---|---|---|---|---|---|---|
MgAl-LDH | 27.78 | 14.45 | 53.90 | 2.44 | 1.42 | \ |
MgAl-LDH/MBT | 18.36 | 16.16 | 58.18 | 5.67 | 1.02 | 0.59 |
Table 1 Elemental content (at.%) for freshly prepared MgAl-LDH and MgAl-LDH/MBT coatings.
Samples | Mg | Al | O | C | N | S |
---|---|---|---|---|---|---|
MgAl-LDH | 27.78 | 14.45 | 53.90 | 2.44 | 1.42 | \ |
MgAl-LDH/MBT | 18.36 | 16.16 | 58.18 | 5.67 | 1.02 | 0.59 |
Fig. 6. (a) XPS survey spectra of the MgAl-LDH and MgAl-LDH/MBT coatings. High resolution XPS spectra of (b) S 2p and (c) N 1s of MgAl-LDH and MgAl-LDH/MBT coatings. (d) High resolution XPS spectrum for C 1s of MgAl-LDH/MBT coating.
Fig. 7. (a) Cross-sectional SEM image and (b-e) corresponding EDS mapping images (white rectangle region in (a) for different elements (Mg, Al, S, and N) distributions in the MgAl-LDH/MBT coating.
Fig. 8. (a) Bode magnitude and (b) Bode phase diagrams of Mg alloy, blank, MBT, MgAl-LDH, and MgAl-LDH/MBT coatings in a 3.5 wt.% NaCl solution. EIS diagram of MgAl-LDH/MBT coating after exposing to NaCl solution for 15 d is also given for evaluation of the robustness. The scatter plots and solid lines are experimental and fitting results, respectively. Equivalent circuits for (c) Mg alloy substrate, (d) blank and MBT, (e) MgAl-LDH, and (f) MgAl-LDH/MBT coatings.
Samples | Bare Mg alloy | Blank | MBT | MgAl-LDH | MgAl-LDH/MBT before exposure | MgAl-LDH/MBT after exposure for 15 d |
---|---|---|---|---|---|---|
Rs (Ω cm2) | 2.5 ± 0.072 | 2.8 ± 0.041 | 2.9 ± 0.17 | 6.2 ± 0.57 | 7.80 ± 0.46 | 6.1 ± 0.36 |
YMBT (10-11 S sn cm-2) | N/A | N/A | N/A | N/A | 2.79 ± 0.18 | 2.92 ± 0.075 |
RMBT (MΩ cm2) | N/A | N/A | N/A | N/A | 0.38 ± 0.023 | 0.35 ± 0.013 |
YLDH (10-9 S sn cm-2) | N/A | N/A | N/A | 4.327 ± 0.39 | 0.237 ± 0.011 | 1.414 ± 0.11 |
RLDH (103 Ω cm2) | N/A | N/A | N/A | 18.73 ± 0.87 | 262.3 ± 14 | 256.2 ± 9.5 |
Ydl (10-9 S sn cm-2) | 6471 ± 1016 | 3000 ± 151.8 | 1214 ± 109.4 | 19.22 ± 1.440 | 0.001056 ± 0.00005600 | 0.001494 ± 0.00007200 |
Rct (103 Ω cm2) | 0.3748 ± 0.0108 | 0.9040 ± 0.0408 | 24.91 ± 2.26 | 482.3 ± 5.21 | 2336 ± 127 | 1979 ± 77.8 |
ZW (10-6 S s0.5 cm-2) | N/A | N/A | N/A | 0.8149 ± 0.0096 | 7.267 ± 0.15 | 1.634 ± 0.14 |
|Z|f = 0.1 Hz (103 Ω cm2) | 0.1822 | 1.795 | 31.42 | 476.6 | 1558 | 1256 |
χ2 (10-3) | 1.6 | 2.5 | 2.5 | 5.7 | 1.9 | 0.88 |
Table 2 Fitted EIS parameters for bare mg alloy, blank, MBT, MgAl-LDH, and MgAl-LDH/MBT coatings exposing to a 3.5 wt.% NaCl solution.
Samples | Bare Mg alloy | Blank | MBT | MgAl-LDH | MgAl-LDH/MBT before exposure | MgAl-LDH/MBT after exposure for 15 d |
---|---|---|---|---|---|---|
Rs (Ω cm2) | 2.5 ± 0.072 | 2.8 ± 0.041 | 2.9 ± 0.17 | 6.2 ± 0.57 | 7.80 ± 0.46 | 6.1 ± 0.36 |
YMBT (10-11 S sn cm-2) | N/A | N/A | N/A | N/A | 2.79 ± 0.18 | 2.92 ± 0.075 |
RMBT (MΩ cm2) | N/A | N/A | N/A | N/A | 0.38 ± 0.023 | 0.35 ± 0.013 |
YLDH (10-9 S sn cm-2) | N/A | N/A | N/A | 4.327 ± 0.39 | 0.237 ± 0.011 | 1.414 ± 0.11 |
RLDH (103 Ω cm2) | N/A | N/A | N/A | 18.73 ± 0.87 | 262.3 ± 14 | 256.2 ± 9.5 |
Ydl (10-9 S sn cm-2) | 6471 ± 1016 | 3000 ± 151.8 | 1214 ± 109.4 | 19.22 ± 1.440 | 0.001056 ± 0.00005600 | 0.001494 ± 0.00007200 |
Rct (103 Ω cm2) | 0.3748 ± 0.0108 | 0.9040 ± 0.0408 | 24.91 ± 2.26 | 482.3 ± 5.21 | 2336 ± 127 | 1979 ± 77.8 |
ZW (10-6 S s0.5 cm-2) | N/A | N/A | N/A | 0.8149 ± 0.0096 | 7.267 ± 0.15 | 1.634 ± 0.14 |
|Z|f = 0.1 Hz (103 Ω cm2) | 0.1822 | 1.795 | 31.42 | 476.6 | 1558 | 1256 |
χ2 (10-3) | 1.6 | 2.5 | 2.5 | 5.7 | 1.9 | 0.88 |
Samples | Ecorr (V) | jcorr (μA cm-2) | βa (V dec-1) | -βc (V dec-1) | Refs. |
---|---|---|---|---|---|
Bare Mg alloy | -1.407 ± 0. 23 | 139 ± 10.1 | 0.212 | 0.084 | This work |
Blank | -1.380 ± 0.035 | 11.5 ± 0.610 | 0.191 | 0.244 | This work |
MBT | -1.210 ± 0.052 | 0.345 ± 0.0307 | 0.259 | 0.202 | This work |
MgAl-LDH | -1.050 ± 0.070 | 0.0428 ± 0.000514 | 0.428 | 0.310 | This work |
MgAl-LDH/MBT before immersion | -0.162 ± 0.0057 | 0.0173 ± 0.000538 | 0.353 | 0.382 | This work |
MgAl-LDH/MBT after immersion | -0.268 ± 0.0075 | 0.0782 ± 0.00368 | 0.293 | 0.250 | This work |
MgAl-NO3- | -1.527 | 31.0 | 0.0443 | 0.402 | [ |
MgAl-NO3- | -1.340 | 0.118 | 0.330 | 0.160 | [ |
MgAl-WO43- | -1.260 | 7.44 | \ | \ | [ |
MgAl-NO3- | -1.300 | 0.558 | \ | \ | [ |
MgFe-NO3- | -1.440 | 1.09 | 0.450 | 0.160 | [ |
MgCr-NO3- | -1.470 | 2.16 | 0.360 | 0.160 | [ |
MgAl-CO32- | -1.456 | 1.03 | 0.388 | 0.174 | [ |
MgAl-CO32- | -1.450 | 1.78 | \ | 0.296 | [ |
MgAl-CO32- | -1.384 | 1.92 | 0.287 | 0.171 | [ |
Table 3 Electrochemical parameters extracted from Tafel plots of bare Mg alloy, different coatings, MgAl-LDH/MBT coating after 15 d of exposure to 3.5 wt.% NaCl solution, and different LDH coating on Mg alloy based on recent literature.
Samples | Ecorr (V) | jcorr (μA cm-2) | βa (V dec-1) | -βc (V dec-1) | Refs. |
---|---|---|---|---|---|
Bare Mg alloy | -1.407 ± 0. 23 | 139 ± 10.1 | 0.212 | 0.084 | This work |
Blank | -1.380 ± 0.035 | 11.5 ± 0.610 | 0.191 | 0.244 | This work |
MBT | -1.210 ± 0.052 | 0.345 ± 0.0307 | 0.259 | 0.202 | This work |
MgAl-LDH | -1.050 ± 0.070 | 0.0428 ± 0.000514 | 0.428 | 0.310 | This work |
MgAl-LDH/MBT before immersion | -0.162 ± 0.0057 | 0.0173 ± 0.000538 | 0.353 | 0.382 | This work |
MgAl-LDH/MBT after immersion | -0.268 ± 0.0075 | 0.0782 ± 0.00368 | 0.293 | 0.250 | This work |
MgAl-NO3- | -1.527 | 31.0 | 0.0443 | 0.402 | [ |
MgAl-NO3- | -1.340 | 0.118 | 0.330 | 0.160 | [ |
MgAl-WO43- | -1.260 | 7.44 | \ | \ | [ |
MgAl-NO3- | -1.300 | 0.558 | \ | \ | [ |
MgFe-NO3- | -1.440 | 1.09 | 0.450 | 0.160 | [ |
MgCr-NO3- | -1.470 | 2.16 | 0.360 | 0.160 | [ |
MgAl-CO32- | -1.456 | 1.03 | 0.388 | 0.174 | [ |
MgAl-CO32- | -1.450 | 1.78 | \ | 0.296 | [ |
MgAl-CO32- | -1.384 | 1.92 | 0.287 | 0.171 | [ |
Fig. 10. (a) Hydrogen evolution as a function of immersion time for bare Mg alloy, blank, MBT, MgAl-LDH, and MgAl-LDH/MBT coatings. (b) Enlarged diagram for observing the difference between MgAl-LDH and MgAl-LDH/MBT coatings.
Fig. 11. (a, b) SEM images of MgAl-LDH/MBT coating at different magnifications after 15 d of exposure to 3.5 wt.% NaCl solution. Inset in (a) is the corresponding digital picture of the sample. EDS spectra of (c) MgAl-LDH/MBT coating and (d) bare Mg alloy after exposure experiment. (e) Optical images of MgAl-LDH/MBT coating exposing to neutral salt fog at different times.
Samples | Mg | Al | O | C | N | S | Cl |
---|---|---|---|---|---|---|---|
Bare Mg alloy | 38.88 | 0.20 | 57.99 | 1.48 | 1.11 | \ | 0.34 |
MgAl-LDH/MBT | 21.74 | 12.7 | 59.57 | 2.86 | 1.23 | 0.40 | 1.50 |
Table 4 Elemental content (at.%) for bare Mg alloy and MgAl-LDH/MBT coating after 15 days of exposure to a 3.5 wt.% NaCl solution.
Samples | Mg | Al | O | C | N | S | Cl |
---|---|---|---|---|---|---|---|
Bare Mg alloy | 38.88 | 0.20 | 57.99 | 1.48 | 1.11 | \ | 0.34 |
MgAl-LDH/MBT | 21.74 | 12.7 | 59.57 | 2.86 | 1.23 | 0.40 | 1.50 |
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