J. Mater. Sci. Technol. ›› 2020, Vol. 49: 224-235.DOI: 10.1016/j.jmst.2020.01.046
• Research Article • Previous Articles Next Articles
Xiao-Li Fana, Chang-Yang Lia, Yu-Bo Wanga, Yuan-Fang Huoa, Shuo-Qi Lia, Rong-Chang Zenga,b,*()
Received:
2019-10-08
Revised:
2020-01-04
Accepted:
2020-01-13
Published:
2020-07-15
Online:
2020-07-17
Contact:
Rong-Chang Zeng
Xiao-Li Fan, Chang-Yang Li, Yu-Bo Wang, Yuan-Fang Huo, Shuo-Qi Li, Rong-Chang Zeng. Corrosion resistance of an amino acid-bioinspired calcium phosphate coating on magnesium alloy AZ31[J]. J. Mater. Sci. Technol., 2020, 49: 224-235.
Fig. 1. Illustration of the preparing of the Ca-P coating and Ca-PL-Cys coating on Mg alloy AZ31 and dissociation equilibrium diagram of l-cysteine in the solution.
Samples | Spectrum | O | P | Ca | C | Al | Mg | Cl | N | S | Ca/P |
---|---|---|---|---|---|---|---|---|---|---|---|
Ca-P coating | #1 | 49 | 20.77 | 13.1 | 10.24 | 3.86 | 2.84 | 0.19 | -- | -- | 0.63 |
#2 | 59.69 | 16.45 | 13.99 | 9.63 | 0.19 | 0.01 | 0.05 | -- | -- | 0.85 | |
#3 | 50.9 | 19.12 | 12.38 | 9.36 | 3.68 | 4.56 | 0 | -- | -- | 0.65 | |
Ca-PL-Cys coating | #4 | 63.73 | 16.94 | 13.52 | 4.14 | -- | -- | -- | 1.66 | -- | 0.80 |
#5 | 56.93 | 15.92 | 12.86 | 10.83 | -- | 0.39 | 0.03 | 2.99 | 0.06 | 0.81 | |
#6 | 70.91 | 13.25 | 10.89 | 4.2 | -- | -- | -- | 0.76 | -- | 0.81 |
Table 1 Chemical composition of Ca-P coating and Ca-PL-Cys coating (at.%).
Samples | Spectrum | O | P | Ca | C | Al | Mg | Cl | N | S | Ca/P |
---|---|---|---|---|---|---|---|---|---|---|---|
Ca-P coating | #1 | 49 | 20.77 | 13.1 | 10.24 | 3.86 | 2.84 | 0.19 | -- | -- | 0.63 |
#2 | 59.69 | 16.45 | 13.99 | 9.63 | 0.19 | 0.01 | 0.05 | -- | -- | 0.85 | |
#3 | 50.9 | 19.12 | 12.38 | 9.36 | 3.68 | 4.56 | 0 | -- | -- | 0.65 | |
Ca-PL-Cys coating | #4 | 63.73 | 16.94 | 13.52 | 4.14 | -- | -- | -- | 1.66 | -- | 0.80 |
#5 | 56.93 | 15.92 | 12.86 | 10.83 | -- | 0.39 | 0.03 | 2.99 | 0.06 | 0.81 | |
#6 | 70.91 | 13.25 | 10.89 | 4.2 | -- | -- | -- | 0.76 | -- | 0.81 |
Fig. 5. (I) FTIR spectra of (a) Ca-P coating and (b) Ca-PL-Cys coating and (II) XRD patterns of (a) Mg alloy AZ31, (b) Ca-P coating and (c) Ca-PL-Cys coating.
Fig. 7. (I, II, III) Nyquist curves and corresponding equivalent circuits, (IV) bode plots of (a) AZ31 Mg alloy, (b) Ca-P coating and (c) Ca-PL-Cys coating.
Samples | Rs (kΩ cm2) | CPE1 (Ω-1 sn cm-2) | n1 | R1 (kΩ cm2) | CPE2 (Ω-1 sn cm-2) | n2 | Rct (kΩ cm2) | L (102H cm2) | RL (kΩ cm2) |
---|---|---|---|---|---|---|---|---|---|
AZ31 substrate | 0.08 ± 0.01 | 1.58 × 10-5 ± 5.5 × 10-6 | 0.89 ± 0.02 | - | - | - | 0.55 ± 0.16 | 4.63 ± 0.83 | 7.21 ± 0.02 |
Ca-P coating | 0.12 ± 0.02 | 4.38 × 10-6 ± 4.47 × 10-7 | 0.68 ± 0.03 | 10.67 ± 0.55 | 8.13 × 10-6 ± 4.29 × 10-6 | 0.87 ± 0.04 | 2.98 ± 0.32 | 1.67 ± 0.82 | 2.95 ± 7.63 |
Ca-PL-Cys coating | 0.09 ± 0.01 | 1.15 × 10-5 ±7.28 × 10-6 | 0.65 ± 0.12 | 280.22 ± 152.57 | 1.3 × 10-5 ±1.27 × 10-5 | 0.80 ± 0.16 | 19.86 ± 2.93 | - | - |
Table 2 Fitting results of EIS spectra.
Samples | Rs (kΩ cm2) | CPE1 (Ω-1 sn cm-2) | n1 | R1 (kΩ cm2) | CPE2 (Ω-1 sn cm-2) | n2 | Rct (kΩ cm2) | L (102H cm2) | RL (kΩ cm2) |
---|---|---|---|---|---|---|---|---|---|
AZ31 substrate | 0.08 ± 0.01 | 1.58 × 10-5 ± 5.5 × 10-6 | 0.89 ± 0.02 | - | - | - | 0.55 ± 0.16 | 4.63 ± 0.83 | 7.21 ± 0.02 |
Ca-P coating | 0.12 ± 0.02 | 4.38 × 10-6 ± 4.47 × 10-7 | 0.68 ± 0.03 | 10.67 ± 0.55 | 8.13 × 10-6 ± 4.29 × 10-6 | 0.87 ± 0.04 | 2.98 ± 0.32 | 1.67 ± 0.82 | 2.95 ± 7.63 |
Ca-PL-Cys coating | 0.09 ± 0.01 | 1.15 × 10-5 ±7.28 × 10-6 | 0.65 ± 0.12 | 280.22 ± 152.57 | 1.3 × 10-5 ±1.27 × 10-5 | 0.80 ± 0.16 | 19.86 ± 2.93 | - | - |
Ecorr (V/SCE) | icorr (μA cm-2) | βa (102 mV/dec) | -βc (102 mV/dec) | Rp (kΩ cm2) | |
---|---|---|---|---|---|
AZ31 substrate | -1.48 ± 0.05 | 5.57 ± 2.49 | 1.51 ± 0.76 | 1.49 ± 0.04 | 2.53 ± 1.83 |
Ca-P coating | -1.51 ± 0.03 | 7.21 ± 2.96 | 1.70 ± 0.98 | 1.27 ± 0.21 | 4.30 ± 1.65 |
Ca-PL-Cys coating | -1.41 ± 0.03 | 0.42 ± 1.84 | 1.87 ± 0.57 | 1.55 ± 0.17 | 40.6 ± 2.09 |
Table 3 Electrochemical parameters of the polarization curves of the samples.
Ecorr (V/SCE) | icorr (μA cm-2) | βa (102 mV/dec) | -βc (102 mV/dec) | Rp (kΩ cm2) | |
---|---|---|---|---|---|
AZ31 substrate | -1.48 ± 0.05 | 5.57 ± 2.49 | 1.51 ± 0.76 | 1.49 ± 0.04 | 2.53 ± 1.83 |
Ca-P coating | -1.51 ± 0.03 | 7.21 ± 2.96 | 1.70 ± 0.98 | 1.27 ± 0.21 | 4.30 ± 1.65 |
Ca-PL-Cys coating | -1.41 ± 0.03 | 0.42 ± 1.84 | 1.87 ± 0.57 | 1.55 ± 0.17 | 40.6 ± 2.09 |
Fig. 10. Digital camera photographs and corrosion SEM morphologies after a 168 h immersion for (a, b, c) Mg alloy AZ31, (d, e, f) Ca-P coating and (g, h, i) Ca-PL-Cys coating.
Samples | Spectrum | O | C | P | Ca | Mg | Al | N | S |
---|---|---|---|---|---|---|---|---|---|
AZ31 | #1 | 51.49 | 13.68 | 15.06 | 8.56 | 6.38 | 4.83 | -- | -- |
#2 | 59.23 | -- | 18.24 | 12.36 | 6.73 | 3.43 | -- | -- | |
#3 | 56.5 | 20.2 | 9.98 | 7.88 | 3.9 | 1.54 | -- | -- | |
Ca-P coating | #4 | 41.62 | -- | 27.94 | 20.68 | 5.65 | 4.11 | -- | -- |
#5 | 35.84 | 27.87 | 8.99 | 14.47 | -- | -- | 10.15 | 2.68 | |
#6 | 34.67 | 37.68 | 7.29 | 5.56 | 0.69 | 0.74 | 12.75 | 0.62 | |
Ca-PL-Cys coating | #7 | 56.48 | 12.33 | 11.91 | 8.48 | 4.29 | 3.17 | 2.99 | 0.34 |
#8 | 34.4 | 2.69 | 26.84 | 20.76 | 5.2 | 4.73 | 5.24 | 0.14 | |
#9 | 45.73 | 9.2 | 17.8 | 12.75 | 5.58 | 2.1 | 6.71 | 0.14 |
Table 4 EDS analysis of the samples after immersion for 168 h (at.%).
Samples | Spectrum | O | C | P | Ca | Mg | Al | N | S |
---|---|---|---|---|---|---|---|---|---|
AZ31 | #1 | 51.49 | 13.68 | 15.06 | 8.56 | 6.38 | 4.83 | -- | -- |
#2 | 59.23 | -- | 18.24 | 12.36 | 6.73 | 3.43 | -- | -- | |
#3 | 56.5 | 20.2 | 9.98 | 7.88 | 3.9 | 1.54 | -- | -- | |
Ca-P coating | #4 | 41.62 | -- | 27.94 | 20.68 | 5.65 | 4.11 | -- | -- |
#5 | 35.84 | 27.87 | 8.99 | 14.47 | -- | -- | 10.15 | 2.68 | |
#6 | 34.67 | 37.68 | 7.29 | 5.56 | 0.69 | 0.74 | 12.75 | 0.62 | |
Ca-PL-Cys coating | #7 | 56.48 | 12.33 | 11.91 | 8.48 | 4.29 | 3.17 | 2.99 | 0.34 |
#8 | 34.4 | 2.69 | 26.84 | 20.76 | 5.2 | 4.73 | 5.24 | 0.14 | |
#9 | 45.73 | 9.2 | 17.8 | 12.75 | 5.58 | 2.1 | 6.71 | 0.14 |
Fig. 11. Digital camera photo and surface roughness of (a) Mg alloy AZ31, (b) Ca-P coating and (c) Ca-PL-Cys coating after immersion 168 h and removing corrosion products.
Samples | Spectrum | O | C | Mg | P | Ca | Al | N | S | Ca/P |
---|---|---|---|---|---|---|---|---|---|---|
Ca-P coating 10 s | #1 | 15.45 | -- | 76.9 | 4.26 | 1.4 | 2.00 | -- | -- | 0.33 |
#2 | 53.65 | -- | -- | 22.76 | 23.59 | -- | -- | -- | 1.04 | |
#3 | 12.39 | -- | 79.66 | 4.20 | 1.29 | 2.46 | -- | -- | 0.31 | |
Ca-P coating 30 s | #4 | 20.81 | 67.31 | 6.30 | 2.87 | 2.72 | 0.46 | |||
#5 | 77.79 | 12.45 | 9.75 | 0.78 | ||||||
#6 | 68.78 | 6.02 | 14.64 | 10.56 | 0.72 | |||||
Ca-P coating 60 s | #7 | 70.25 | 9.79 | 11.04 | 8.91 | 0.81 | ||||
#8 | 62.97 | 10.53 | 0.09 | 13.59 | 12.82 | 0.94 | ||||
#9 | 63.70 | 8.04 | 14.80 | 13.45 | 0.91 | |||||
Ca-PL-Cys coating 10 s | #10 | 60.68 | 20.94 | 3.03 | 7.35 | 6.01 | 1.53 | 0.46 | 0.82 | |
#11 | 50.92 | 13.48 | 13.99 | 10.41 | 8.18 | 3.03 | -- | 0.79 | ||
#12 | 50.53 | 20.17 | 4.11 | 11.52 | 9.77 | -- | 3.76 | 0.15 | 0.85 | |
Ca-PL-Cys coating 30 s | #13 | 66.32 | 13.06 | 8.80 | 6.59 | 5.00 | 0.23 | 0.75 | ||
#14 | 16.21 | 22.35 | 46.02 | 4.61 | 3.37 | 1.77 | 5.04 | 0.62 | 0.73 | |
#15 | 33.10 | 18.16 | 13.61 | 15.85 | 18.92 | 0.36 | 1.16 | |||
Ca-PL-Cys coating 60 s | #16 | 65.26 | 6.37 | 13.41 | 12.68 | 2.28 | 0.95 | |||
#17 | 19.64 | 20.07 | 49.88 | 4.67 | 2.14 | 1.41 | 1.94 | 0.27 | 0.46 | |
#18 | 67.14 | 11.86 | 9.06 | 6.93 | 4.92 | 0.09 | 0.77 |
Table 5 EDS analysis of corresponding microscopic topographies at different time during the formation of coatings (at.%).
Samples | Spectrum | O | C | Mg | P | Ca | Al | N | S | Ca/P |
---|---|---|---|---|---|---|---|---|---|---|
Ca-P coating 10 s | #1 | 15.45 | -- | 76.9 | 4.26 | 1.4 | 2.00 | -- | -- | 0.33 |
#2 | 53.65 | -- | -- | 22.76 | 23.59 | -- | -- | -- | 1.04 | |
#3 | 12.39 | -- | 79.66 | 4.20 | 1.29 | 2.46 | -- | -- | 0.31 | |
Ca-P coating 30 s | #4 | 20.81 | 67.31 | 6.30 | 2.87 | 2.72 | 0.46 | |||
#5 | 77.79 | 12.45 | 9.75 | 0.78 | ||||||
#6 | 68.78 | 6.02 | 14.64 | 10.56 | 0.72 | |||||
Ca-P coating 60 s | #7 | 70.25 | 9.79 | 11.04 | 8.91 | 0.81 | ||||
#8 | 62.97 | 10.53 | 0.09 | 13.59 | 12.82 | 0.94 | ||||
#9 | 63.70 | 8.04 | 14.80 | 13.45 | 0.91 | |||||
Ca-PL-Cys coating 10 s | #10 | 60.68 | 20.94 | 3.03 | 7.35 | 6.01 | 1.53 | 0.46 | 0.82 | |
#11 | 50.92 | 13.48 | 13.99 | 10.41 | 8.18 | 3.03 | -- | 0.79 | ||
#12 | 50.53 | 20.17 | 4.11 | 11.52 | 9.77 | -- | 3.76 | 0.15 | 0.85 | |
Ca-PL-Cys coating 30 s | #13 | 66.32 | 13.06 | 8.80 | 6.59 | 5.00 | 0.23 | 0.75 | ||
#14 | 16.21 | 22.35 | 46.02 | 4.61 | 3.37 | 1.77 | 5.04 | 0.62 | 0.73 | |
#15 | 33.10 | 18.16 | 13.61 | 15.85 | 18.92 | 0.36 | 1.16 | |||
Ca-PL-Cys coating 60 s | #16 | 65.26 | 6.37 | 13.41 | 12.68 | 2.28 | 0.95 | |||
#17 | 19.64 | 20.07 | 49.88 | 4.67 | 2.14 | 1.41 | 1.94 | 0.27 | 0.46 | |
#18 | 67.14 | 11.86 | 9.06 | 6.93 | 4.92 | 0.09 | 0.77 |
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