J. Mater. Sci. Technol. ›› 2018, Vol. 34 ›› Issue (12): 2271-2282.DOI: 10.1016/j.jmst.2018.05.005
Special Issue: Corrosion in 2018; Biomaterials 2018
• Orginal Article • Previous Articles Next Articles
Lijun Liua, Yao Menga, Chaofang Dongab, YuY anb, Alex A. Volinskyc, Lu-Ning Wanga*()
Received:
2018-01-12
Revised:
2018-02-25
Accepted:
2018-03-13
Online:
2018-12-20
Published:
2018-11-15
Contact:
Wang Lu-Ning
Lijun Liu, Yao Meng, Chaofang Dong, YuY an, Alex A. Volinsky, Lu-Ning Wang. Initial formation of corrosion products on pure zinc in simulated body fluid[J]. J. Mater. Sci. Technol., 2018, 34(12): 2271-2282.
Plasma [ | r-SBF [ | PBS [ | Ringer’s solution [ | Hank’s Solution [ | |
---|---|---|---|---|---|
Na+ (mmol/L) | 142.0 | 142.0 | 154.05 | 156.4 | 141.8 |
K+ (mmol/L) | 5.0 | 5.0 | 4.14 | 5.8 | 5.8 |
Ca2+ (mmol/L) | 2.5 | 2.5 | - | 2.2 | 2.5 |
Mg2+ (mmol/L) | 1.5 | 1.5 | - | - | 0.8 |
Cl- (mmol/L) | 103.0 | 103.0 | 140.6 | 164.2 | 147.4 |
HCO3- (mmol/L) | 27.0 | 27.0 | - | 2.4 | 4.2 |
HPO42- (mmol/L) | 1.0 | 1.0 | 8.06 | - | 0.3 |
H2PO4- (mmol/L) | - | - | 1.47 | - | 0.4 |
SO42- (mmol/L) | 0.5 | 0.5 | - | - | 0.8 |
Amino acids (mg/L) | nd | - | - | - | |
Glucose (g/L) | nd | - | - | - | 5.6 |
Proteins (g/L) | 63-80 | - | - | - |
Table 1 Comparison of the inorganic ion concentrations and some organic components among human blood plasma, r-SBF, PBS, Ringer’s solution and Hank’s solution.
Plasma [ | r-SBF [ | PBS [ | Ringer’s solution [ | Hank’s Solution [ | |
---|---|---|---|---|---|
Na+ (mmol/L) | 142.0 | 142.0 | 154.05 | 156.4 | 141.8 |
K+ (mmol/L) | 5.0 | 5.0 | 4.14 | 5.8 | 5.8 |
Ca2+ (mmol/L) | 2.5 | 2.5 | - | 2.2 | 2.5 |
Mg2+ (mmol/L) | 1.5 | 1.5 | - | - | 0.8 |
Cl- (mmol/L) | 103.0 | 103.0 | 140.6 | 164.2 | 147.4 |
HCO3- (mmol/L) | 27.0 | 27.0 | - | 2.4 | 4.2 |
HPO42- (mmol/L) | 1.0 | 1.0 | 8.06 | - | 0.3 |
H2PO4- (mmol/L) | - | - | 1.47 | - | 0.4 |
SO42- (mmol/L) | 0.5 | 0.5 | - | - | 0.8 |
Amino acids (mg/L) | nd | - | - | - | |
Glucose (g/L) | nd | - | - | - | 5.6 |
Proteins (g/L) | 63-80 | - | - | - |
Fig. 2. (a) Potentiodynamic curves of pure Zn at different immersion periods in r-SBF: 0?h, 6?h, 12?h, 24?h, 48?h, 120?h, 168?h, 240?h and 360?h; (b) The current density obtained from PDP curves.
Immersion time | Ecorr (V vs. SCE) | Icorr (μA?cm-2) | βc (V dec) |
---|---|---|---|
0?h | -1.12?±?0.09 | 5.72?±?6.77 | 0.13?±?0.07 |
6?h | -1.02?±?0.04 | 2.55?±?1.03 | 0.15?±?0.04 |
12?h | -0.99?±?0.01 | 4.25?±?1.67 | 0.15?±?0.21 |
24?h | -1.03?±?0.0002 | 6.03?±?2.35 | 0.17?±?0.05 |
48?h | -1.01?±?0.01 | 18.90?±?5.83 | 0.29?±?0.06 |
120?h | -1.04?±?0.03 | 11.30?±?3.52 | 0.28?±?0.10 |
168?h | -0.98?±?0.02 | 5.77?±?3.47 | 0.13?±?0.04 |
240?h | -0.99?±?0.02 | 18.00?±?2.07 | 0.19?±?0.09 |
336?h | -1.08?±?0.07 | 11.90?±?4.29 | 0.22?±?0.08 |
Table 2 The polarization data of the pure Zn at different immersion periods in r-SBF.
Immersion time | Ecorr (V vs. SCE) | Icorr (μA?cm-2) | βc (V dec) |
---|---|---|---|
0?h | -1.12?±?0.09 | 5.72?±?6.77 | 0.13?±?0.07 |
6?h | -1.02?±?0.04 | 2.55?±?1.03 | 0.15?±?0.04 |
12?h | -0.99?±?0.01 | 4.25?±?1.67 | 0.15?±?0.21 |
24?h | -1.03?±?0.0002 | 6.03?±?2.35 | 0.17?±?0.05 |
48?h | -1.01?±?0.01 | 18.90?±?5.83 | 0.29?±?0.06 |
120?h | -1.04?±?0.03 | 11.30?±?3.52 | 0.28?±?0.10 |
168?h | -0.98?±?0.02 | 5.77?±?3.47 | 0.13?±?0.04 |
240?h | -0.99?±?0.02 | 18.00?±?2.07 | 0.19?±?0.09 |
336?h | -1.08?±?0.07 | 11.90?±?4.29 | 0.22?±?0.08 |
Fig. 3. EIS results of pure Zn after immersion in r-SBF: (a) Bode plots of |Z| vs. frequency and phase angle vs. frequency; (b) the equivalent electrical circuit used to fit the EIS data and (c) the total resistance Rt calculated from EIS components. Different immersion periods: 0?h, 6?h, 12?h, 24?h, 48?h, 120?h, 168?h, 240?h and 336?h. Symbols represent experimental data and lines represent simulated spectra.
Immersion time | Rs (Ω cm2) | Qdl (μΩ-1?s-1?cm-2) | n | Rct (Ω cm2) | Cc (μF?cm-2) | Rc (Ω?cm2) |
---|---|---|---|---|---|---|
0?h | 12.17?±?1.99 | 4.87?±?2.00 | 0.79?±?0.04 | 1962.67?±?476.05 | 2530?±?2880 | 1144.43?±?297.76 |
6?h | 12.70?±?0.86 | 2.83?±?0.97 | 0.81?±?0.01 | 1765.33?±?462.59 | 6910?±?5480 | 977.03?±?293.65 |
12?h | 14.23?±?0.31 | 2.02?±?0.09 | 0.84?±?0.01 | 1181.87?±?338.15 | 2022?±?1966 | 398.67?±?108.17 |
24?h | 13.96?±?1.67 | 1.86?±?0.09 | 0.83?±?0.03 | 764.47?±?93.07 | 1930?±?1030 | 364.8?±?120.54 |
48?h | 13.08?±?1.25 | 1.32?±?0.37 | 0.83?±?0.005 | 1174.93?±?171.90 | 4250?±?3690 | 390.67?±?104.21 |
120?h | 15.03?±?2.07 | 1.32?±?0.20 | 0.85?±?0.006 | 2362.33?±?260.53 | 1780?±?1610 | 497.83?±?157.23 |
168?h | 14.00?±?0.86 | 1.87?±?0.19 | 0.84?±?0 | 3442.33?±?1087.38 | 820?±?330 | 746.13?±?169.88 |
240?h | 12.79?±?2.04 | 3.96?±?3.51 | 0.84?±?0.01 | 2733.67?±?619.95 | 1350?±?350 | 742.17?±?185.11 |
336?h | 13.58?±?1.66 | 1.90?±?1.14 | 0.82?±?0.05 | 1092.17?±?185.01 | 5240?±?2390 | 347.17?±?129.61 |
Table 3 Equivalent electrical circuit parameters of the pure Zn at different immersion periods in r-SBF at 37?°C.
Immersion time | Rs (Ω cm2) | Qdl (μΩ-1?s-1?cm-2) | n | Rct (Ω cm2) | Cc (μF?cm-2) | Rc (Ω?cm2) |
---|---|---|---|---|---|---|
0?h | 12.17?±?1.99 | 4.87?±?2.00 | 0.79?±?0.04 | 1962.67?±?476.05 | 2530?±?2880 | 1144.43?±?297.76 |
6?h | 12.70?±?0.86 | 2.83?±?0.97 | 0.81?±?0.01 | 1765.33?±?462.59 | 6910?±?5480 | 977.03?±?293.65 |
12?h | 14.23?±?0.31 | 2.02?±?0.09 | 0.84?±?0.01 | 1181.87?±?338.15 | 2022?±?1966 | 398.67?±?108.17 |
24?h | 13.96?±?1.67 | 1.86?±?0.09 | 0.83?±?0.03 | 764.47?±?93.07 | 1930?±?1030 | 364.8?±?120.54 |
48?h | 13.08?±?1.25 | 1.32?±?0.37 | 0.83?±?0.005 | 1174.93?±?171.90 | 4250?±?3690 | 390.67?±?104.21 |
120?h | 15.03?±?2.07 | 1.32?±?0.20 | 0.85?±?0.006 | 2362.33?±?260.53 | 1780?±?1610 | 497.83?±?157.23 |
168?h | 14.00?±?0.86 | 1.87?±?0.19 | 0.84?±?0 | 3442.33?±?1087.38 | 820?±?330 | 746.13?±?169.88 |
240?h | 12.79?±?2.04 | 3.96?±?3.51 | 0.84?±?0.01 | 2733.67?±?619.95 | 1350?±?350 | 742.17?±?185.11 |
336?h | 13.58?±?1.66 | 1.90?±?1.14 | 0.82?±?0.05 | 1092.17?±?185.01 | 5240?±?2390 | 347.17?±?129.61 |
Fig. 4. Optical images of pure Zn tested in r-SBF for different time: (a) 6?h, (b) 12?h, (c) 24?h, (d) 48?h, (e) 120?h, (f) 168?h, (g) 240?h and (h) 336?h.
Fig. 5. SEM images of pure Zn immersed in r-SBF for (a) 6?h, (b) 12?h, (c) 24?h, (d) 48?h, (e) 120?h, (f) 168?h, (g) 240?h and (h) 336?h. The insets show local high magnification area.
6?h | 12?h | 24?h | 48?h | 120?h | 168?h | 240?h | 336?h | |
---|---|---|---|---|---|---|---|---|
Zn | 65.8 | 64.9 | 63.4 | 62.8 | 46.3 | 47.8 | 41.4 | 17.4 |
C | 23.1 | 23.9 | 24.3 | 23.1 | 29.3 | 26.7 | 31.7 | 12.5 |
O | 9.6 | 9.8 | 10.9 | 12.2 | 19.3 | 21.3 | 21.8 | 58.4 |
P | 1.4 | 0.9 | 1.1 | 1.3 | 3.8 | 2.8 | 3.4 | 8.5 |
Ca | 0.1 | 0.5 | 0.4 | 0.6 | 1.3 | 1.4 | 1.7 | 3.2 |
P/Zn | 0.021 | 0.014 | 0.017 | 0.021 | 0.082 | 0.058 | 0.082 | 0.488 |
Table 4 EDS data of the surface of Zn samples after immersion in SBF for different time (at.%).
6?h | 12?h | 24?h | 48?h | 120?h | 168?h | 240?h | 336?h | |
---|---|---|---|---|---|---|---|---|
Zn | 65.8 | 64.9 | 63.4 | 62.8 | 46.3 | 47.8 | 41.4 | 17.4 |
C | 23.1 | 23.9 | 24.3 | 23.1 | 29.3 | 26.7 | 31.7 | 12.5 |
O | 9.6 | 9.8 | 10.9 | 12.2 | 19.3 | 21.3 | 21.8 | 58.4 |
P | 1.4 | 0.9 | 1.1 | 1.3 | 3.8 | 2.8 | 3.4 | 8.5 |
Ca | 0.1 | 0.5 | 0.4 | 0.6 | 1.3 | 1.4 | 1.7 | 3.2 |
P/Zn | 0.021 | 0.014 | 0.017 | 0.021 | 0.082 | 0.058 | 0.082 | 0.488 |
Fig. 8. XPS spectra of pure Zn: (a) The overview XPS spectrum, (b) P 2p and (c) Zn 2p3/2 spectra of pure Zn after immersion in r-SBF for 6?h, 12?h, 24?h, 48?h, 120?h, 168?h, 240?h and 336?h; Deconvoluted XPS spectra (d-g) of P 2p after immersion for 6?h, 48?h, 168?h and 336?h, and (h-l) of Zn 2p3/2 after immersion for 0?h, 6?h, 48?h, 168?h and 336?h.
Immersion time | Zn3(PO4)2 | Ca3(PO4)2 | CaHPO4·2H2O |
---|---|---|---|
6?h | 72.2 | 24.8 | 3.0 |
48?h | 62.5 | 32.3 | 5.2 |
168?h | 58.2 | 36.2 | 5.6 |
336?h | 49.0 | 44.2 | 6.8 |
Table 5 Proportion of different component in the corrosion products (%).
Immersion time | Zn3(PO4)2 | Ca3(PO4)2 | CaHPO4·2H2O |
---|---|---|---|
6?h | 72.2 | 24.8 | 3.0 |
48?h | 62.5 | 32.3 | 5.2 |
168?h | 58.2 | 36.2 | 5.6 |
336?h | 49.0 | 44.2 | 6.8 |
Fig. 9. GIXRD patterns of Zn after immersion in r-SBF solution for 6?h, 12?h, 24?h, 48?h, 120?h, 168?h, 240?h and 336?h. Inset shows the high magnification patterns from 10° to 38° 2θ angle for Zn immersed for 120?h, 168?h, 240?h and 336?h.
Immersion time | CRi (mm?y-1) | CRw (mm?y-1) |
---|---|---|
0?h | 0.08?±?0.10 | 0 |
12?h | 0.06?±?0.02 | 0.04?±?0.02 |
24?h | 0.09?±?0.03 | 0.06?±?0.01 |
48?h | 0.28?±?0.09 | 0.05?±?0.006 |
120?h | 0.17?±?0.05 | 0.04?±?0.006 |
168?h | 0.09?±?0.05 | 0.03?±?0.006 |
240?h | 0.27?±?0.03 | 0.03?±?0.001 |
336?h | 0.18?±?0.06 | 0.03?±?0.002 |
Table 6 Corrosion rates of pure Zn in the r-SBF obtained from the electrochemical measurements (CRi, mm y-1) and immersion tests (CRw, mm y-1).
Immersion time | CRi (mm?y-1) | CRw (mm?y-1) |
---|---|---|
0?h | 0.08?±?0.10 | 0 |
12?h | 0.06?±?0.02 | 0.04?±?0.02 |
24?h | 0.09?±?0.03 | 0.06?±?0.01 |
48?h | 0.28?±?0.09 | 0.05?±?0.006 |
120?h | 0.17?±?0.05 | 0.04?±?0.006 |
168?h | 0.09?±?0.05 | 0.03?±?0.006 |
240?h | 0.27?±?0.03 | 0.03?±?0.001 |
336?h | 0.18?±?0.06 | 0.03?±?0.002 |
Fig. 12. Schematic illustration of corrosion process of pure Zn immersed in r-SBF solution: (a) the dissolution of Zn and formation of ZnO/Zn(OH)2 at initial stage during immersion; (b) the nucleation of zinc phosphate and calcium phosphates by extending the immersion time; (c) the growth of phosphates and thickening of the corrosion products; (d) partially dissolution of the corrosion product.
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