J. Mater. Sci. Technol. ›› 2020, Vol. 49: 166-178.DOI: 10.1016/j.jmst.2020.01.016
• Research Article • Previous Articles Next Articles
Shidong Wang, Lyndon Lambornb, Karina Chevilc, Erwin Gamboac, Weixing Chena,*()
Received:
2019-06-09
Revised:
2019-09-17
Accepted:
2019-10-04
Published:
2020-07-15
Online:
2020-07-17
Contact:
Weixing Chen
Shidong Wang, Lyndon Lamborn, Karina Chevil, Erwin Gamboa, Weixing Chen. Near-neutral pH corrosion of mill-scaled X-65 pipeline steel with paint primer[J]. J. Mater. Sci. Technol., 2020, 49: 166-178.
Ingredient | Concentration | CAS number |
---|---|---|
Acetone | 24.23 | 67-64-1 |
Propane | 13.86 | 74-98-6 |
N-butane | 8.14 | 106-97-8 |
VM&P Naphtha | 5.58 | 64742-89-8 |
TiO2 | 5.13 | 13463-67-7 |
Toluene | 5.07 | 108-88-3 |
Talc (Mg3Si4O10(OH)2) | 4.49 | 14807-96-6 |
Xylene (mix) | 4.08 | 1330-20-7 |
Ethyl alcohol | 3.98 | 64-17-5 |
N-butyl acetate | 2.78 | 123-86-4 |
Mineral spirits | 2.55 | 64742-47-8 |
Isobutyl acetate | 1.62 | 110-19-0 |
Isopropyl alcohol | 1.02 | 67-63-0 |
Other additives | 17.47 | N/A |
Table 1 Chemical composition of the primer paint used in the current investigation (wt%).
Ingredient | Concentration | CAS number |
---|---|---|
Acetone | 24.23 | 67-64-1 |
Propane | 13.86 | 74-98-6 |
N-butane | 8.14 | 106-97-8 |
VM&P Naphtha | 5.58 | 64742-89-8 |
TiO2 | 5.13 | 13463-67-7 |
Toluene | 5.07 | 108-88-3 |
Talc (Mg3Si4O10(OH)2) | 4.49 | 14807-96-6 |
Xylene (mix) | 4.08 | 1330-20-7 |
Ethyl alcohol | 3.98 | 64-17-5 |
N-butyl acetate | 2.78 | 123-86-4 |
Mineral spirits | 2.55 | 64742-47-8 |
Isobutyl acetate | 1.62 | 110-19-0 |
Isopropyl alcohol | 1.02 | 67-63-0 |
Other additives | 17.47 | N/A |
KCl | NaHCO3 | CaCl2·2H2O | MgSO4·7H2O | CaCO3 |
---|---|---|---|---|
0.0035 | 0.0195 | 0.0255 | 0.0274 | 0.0606 |
Table 2 Chemical composition of the C2 solution used in the current investigation (g/l).
KCl | NaHCO3 | CaCl2·2H2O | MgSO4·7H2O | CaCO3 |
---|---|---|---|---|
0.0035 | 0.0195 | 0.0255 | 0.0274 | 0.0606 |
Fig. 2. Microstructural characterization of samples before test: (a, b) secondary electron imaging of the surfaces of mill-scaled and primer pre-coated samples, respectively; (c, d) backscattered electron imaging of the cross-sectional surfaces of mill-scaled and primer pre-coated samples, respectively; (e) Raman spectra of the outer and inner layers of mill scale.
Fig. 3. Mass loss of the mill-scaled and primer pre-coated samples immersed in C2 solution for up to 90 d. Standard deviation of the measured data was provided. The symbols and lines denote the experimental and fitted data, respectively.
Fig. 5. XRD patterns of samples after exposure to C2 solution for up to 90 d: (a) mill-scaled, (b) primer pre-coated and (c) polished samples. JCPDS standard cards are provided, and the strongest lines are marked correspondingly (Fe, No. 65-4899; γ-FeOOH, No. 74-1877; α-FeOOH, No. 08-0097; Fe3O4, No. 79-0419; FeCO3, No. 29-0696; TiO2, No. 87-0710; Mg3Si4O10(OH)2, No. 83-1768).
Fig. 6. Backscattered electron imaging to surfaces of mill-scaled samples exposed to C2 solution for (a) 0 d, (b) 5 d, (c) 30 d and (d) 90 d; (e) secondary electron observation of the image (d); (f) high-magnification imaging of the marked area “f” in image (e). The inset in image (f) is a Raman spectrum from the corresponding marked area in image (f).
Fig. 7. EDS analysis results obtained within the marked areas in Fig. 6. Images (a), (b), (c) and (d) are EDS results of the corresponding marked areas “a”, “b”, “c” and “d” in Fig. 6 (a, b), respectively. Note that C element was removed from EDS results, as it might come from the contamination.
Fig. 8. Backscattered electron imaging to surfaces of primer pre-coated samples exposed to C2 solution for (a) 0 d, (b) 5 d, (c) 30 d and (d) 90 d; (e) secondary electron observation of the image (d); (f) high-magnification imaging of marked area “f” in image (e). The inset in image (f) is the backscattered electron observation of the marked area “g” in image (f).
Fig. 9. Representative backscattered electron images of cross-sectional surfaces of samples after exposure to C2 solution for various time: (a, c) mill-scaled and primer pre-coated samples after 30 d of immersion, respectively; (b, d) mill-scaled and primer pre-coated samples after 90 d of immersion, respectively.
Fig. 10. Pit-depth distribution measured on 1 cm long cross-section of each sample after corrosion exposure for 90 d. Error bars show the standard deviation of the measured data.
Fig. 12. Electrochemical impedance spectra of mill-scaled samples with different immersion time: (a) Nyquist plots, (b) enlarged graph of (a), (c) Bode plots of log |Z| vs. log f and (d) Bode plots of phase angle (θ) vs. log f. The symbols and lines in images (a-d) denote the experimental and fitted data, respectively.
Fig. 13. Electrochemical impedance spectra of primer pre-coated samples with different immersion time: (a) Nyquist plots, (b) enlarged graph of (a), (c) Bode plots of log |Z| vs. log f and (d) Bode plots of phase angle (θ) vs. log f. The symbols and lines in images (a-d) denote the experimental and fitted data, respectively.
Fig. 14. Equivalent circuit models used for fitting the impedance spectra of samples: (a) mill-scaled samples and (b) primer pre-coated samples. (Rs: solution resistance; CPEo: CPE of the reduction process of oxides; Ro: resistance of the reduction process of oxides; CPEi: CPE of the dissolution of iron; Ri: resistance of the dissolution of iron; CPEc: CPE of the primer layer; Rc: resistance of the primer layer).
Time | Rs (Ω cm2) | Qo (μΩ-1 cm-2 sn) | no | Ro (Ω cm2) | Qi (μΩ-1 cm-2 sn) | ni | Ri (Ω cm2) | χ2×104 |
---|---|---|---|---|---|---|---|---|
5 d | 582 | 412 | 0.76 | 223 | 658 | 0.76 | 4535 | 1.01 |
30 d | 561 | 484 | 0.79 | 690 | 173 | 0.80 | 3078 | 0.54 |
60 d | 539 | 624 | 0.80 | 449 | 293 | 0.79 | 2278 | 0.43 |
90 d | 529 | 671 | 0.82 | 407 | 373 | 0.80 | 2268 | 0.39 |
Table 3 Fitting results of the EIS for mill-scaled samples with various immersion time.
Time | Rs (Ω cm2) | Qo (μΩ-1 cm-2 sn) | no | Ro (Ω cm2) | Qi (μΩ-1 cm-2 sn) | ni | Ri (Ω cm2) | χ2×104 |
---|---|---|---|---|---|---|---|---|
5 d | 582 | 412 | 0.76 | 223 | 658 | 0.76 | 4535 | 1.01 |
30 d | 561 | 484 | 0.79 | 690 | 173 | 0.80 | 3078 | 0.54 |
60 d | 539 | 624 | 0.80 | 449 | 293 | 0.79 | 2278 | 0.43 |
90 d | 529 | 671 | 0.82 | 407 | 373 | 0.80 | 2268 | 0.39 |
Time | Rs (Ω cm2) | Qc (μΩ-1 cm-2 sn) | nc | Rc (Ω cm2) | Qo (μΩ-1 cm-2 sn) | no | Ro (Ω cm2) | Qi (μΩ-1 cm-2 sn) | ni | Ri (Ω cm2) | χ2×104 |
---|---|---|---|---|---|---|---|---|---|---|---|
5 d | 588 | 0.5 | 0.67 | 923 | 170 | 0.59 | 1392 | 426 | 0.65 | 7875 | 1.49 |
30 d | 569 | 0.8 | 0.65 | 911 | 183 | 0.63 | 1131 | 354 | 0.77 | 8833 | 1.43 |
60 d | 541 | 1.2 | 0.61 | 631 | 189 | 0.77 | 808 | 357 | 0.81 | 6740 | 1.71 |
90 d | 512 | 1.4 | 0.60 | 555 | 191 | 0.77 | 405 | 380 | 0.82 | 5910 | 1.70 |
Table 4 Fitting results of the EIS for primer pre-coated samples with various immersion time.
Time | Rs (Ω cm2) | Qc (μΩ-1 cm-2 sn) | nc | Rc (Ω cm2) | Qo (μΩ-1 cm-2 sn) | no | Ro (Ω cm2) | Qi (μΩ-1 cm-2 sn) | ni | Ri (Ω cm2) | χ2×104 |
---|---|---|---|---|---|---|---|---|---|---|---|
5 d | 588 | 0.5 | 0.67 | 923 | 170 | 0.59 | 1392 | 426 | 0.65 | 7875 | 1.49 |
30 d | 569 | 0.8 | 0.65 | 911 | 183 | 0.63 | 1131 | 354 | 0.77 | 8833 | 1.43 |
60 d | 541 | 1.2 | 0.61 | 631 | 189 | 0.77 | 808 | 357 | 0.81 | 6740 | 1.71 |
90 d | 512 | 1.4 | 0.60 | 555 | 191 | 0.77 | 405 | 380 | 0.82 | 5910 | 1.70 |
Species | ΔG0 (kJ mol-1) | Ref. | Species | ΔG0 (kJ mol-1) | Ref. |
---|---|---|---|---|---|
H2 | 0 | [ | CO32- | -527.9 | [ |
H+ | 0 | [ | Fe2+ | -78.9 | [ |
Fe | 0 | [ | H2CO3 | -623.2 | [ |
FeCO3 | -666.67 | [ | HCO3- | -586.85 | [ |
Fe3O4 | -1015.4 | [ | H2O | -237.141 | [ |
α-FeOOH | -485.3 | [ | Fe2(OH)2CO3 | -1169.3 | [ |
γ-FeOOH | -480.1 | [ | Fe6(OH)12CO3 | -3650 | [ |
Table 5 Thermodynamic data of used species in E-pH calculations at 298.15 K.
Species | ΔG0 (kJ mol-1) | Ref. | Species | ΔG0 (kJ mol-1) | Ref. |
---|---|---|---|---|---|
H2 | 0 | [ | CO32- | -527.9 | [ |
H+ | 0 | [ | Fe2+ | -78.9 | [ |
Fe | 0 | [ | H2CO3 | -623.2 | [ |
FeCO3 | -666.67 | [ | HCO3- | -586.85 | [ |
Fe3O4 | -1015.4 | [ | H2O | -237.141 | [ |
α-FeOOH | -485.3 | [ | Fe2(OH)2CO3 | -1169.3 | [ |
γ-FeOOH | -480.1 | [ | Fe6(OH)12CO3 | -3650 | [ |
Fig. 15. E-pH diagrams for the Fe-H2O-CO2 system at 25 °C, pressure =1 bar: (a) [Fe2+] = 10-6, 10-5, 10-4 and 10-3 mol/l and the concentrations of the anions are assumed to be 10-2 mol/l, (b) [Fe2+] = 10-6 mol/l, [anions] = 10-3, 10-2 and 10-1 mol/l. The superposed red and blue triangles respectively represent OCP values of mill-scaled and primer pre-coated samples at various immersion time.
No. | Electrode reaction | Equilibrium potential equation | E (V/SCE) |
---|---|---|---|
(8) | Fe→Fe2++2e- | EFe2+/Fe=-0.6527+0.0296log[Fe2+] | -0.830 |
(9) | γFeOOH+3H++e-→Fe2++2H2O | EγFeOOH/ Fe2+=0.5136-0.0592log[Fe2+]-0.178pH | -0.251 |
(10) | αFeOOH+3H++e-→Fe2++2H2O | EαFeOOH/ Fe2+=0.4597-0.0592log[Fe2+]-0.178pH | -0.305 |
(11) | Fe3O4+8H++2e-→3Fe2++4H2O | EFe3O4/Fe2+=0.6364-0.0888log[Fe2+]-0.237pH | -0.322 |
(12) | 2H++2e-→H2 | EH+/H2=-0.2438-0.0592pH | -0.616 |
Table 6 Possible electrode reactions and corresponding expressions for their equilibrium potential used in the currently investigation (pH = 6.29, [Fe2+] = 10-6 mol/l).
No. | Electrode reaction | Equilibrium potential equation | E (V/SCE) |
---|---|---|---|
(8) | Fe→Fe2++2e- | EFe2+/Fe=-0.6527+0.0296log[Fe2+] | -0.830 |
(9) | γFeOOH+3H++e-→Fe2++2H2O | EγFeOOH/ Fe2+=0.5136-0.0592log[Fe2+]-0.178pH | -0.251 |
(10) | αFeOOH+3H++e-→Fe2++2H2O | EαFeOOH/ Fe2+=0.4597-0.0592log[Fe2+]-0.178pH | -0.305 |
(11) | Fe3O4+8H++2e-→3Fe2++4H2O | EFe3O4/Fe2+=0.6364-0.0888log[Fe2+]-0.237pH | -0.322 |
(12) | 2H++2e-→H2 | EH+/H2=-0.2438-0.0592pH | -0.616 |
Fig. 16. Schematic illustration for the corrosion process on cross-sections of (a, c, e, g) mill-scaled and (b, d, f, h) primer pre-coated samples in C2 solution.
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