Evaluation of Passive Films on 17-7PH and 410 Stainless Steel Exposed to NaCl Solution
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Passivation Treatment
- The samples were cleaned ultrasonically according to ASTM A380-17 [41]. This cleaning process involved immersing the samples in ethanol for a duration of 10 min; after that, they were rinsed with deionized water to remove any residual contaminants. Ultrasonic cleaning is a highly effective method for removing any impurities that could compromise subsequent treatments [42].
- Two passivation solutions were prepared for the treatment of the samples. The first solution consisted of citric acid (C6H8O7) at a concentration of 15 wt.% and a pH of 1.51. The second solution comprised nitric acid (HNO3) at a concentration of 20 v/v% and a pH of 0.41.
- After preconditioning the passivating solutions at 49 °C, the samples were carefully submerged. The immersion time was 90 min, ensuring adequate exposure to the passivation solution for effective treatment.
- Finally, rinsing in deionized water and air drying were carried out.
2.3. SEM Microstructural Characterization
2.4. Electrochemical Testing
2.5. X-ray Photoelectron Spectroscopy (XPS) Characterization
3. Results and Discussion
3.1. Scanning Electron Microscopy (SEM) and Microstructural Analysis
3.2. Pitting Resistance Equivalent Number (PREN)
3.3. XPS Characterization
3.4. Electrochemical Measurements
3.5. SEM Surface Characterization
4. Conclusions
- SEM characterization under the initial conditions and conducted on the samples in an as-received state indicated that the 17-7PH presented a microstructure with a martensitic (α′) phase, while 410 SS contained a microstructure consisting of austenite (γ), a delta (δ) ferrite phase, and chromium carbides.
- The PREN results indicate that 17-7PH (18.92) steel has better resistance to pitting corrosion than 410 SS (13.5).
- According to the cyclic potentiodynamic polarization results, 17-7PH steel passivated in citric acid exhibited lower corrosion rate values (in the order of ×10−3 mm/yr).
- The application of nitric acid passivation caused the surface to become susceptible to localized corrosion.
- Passivation of 410 SS in acid nitric showed a trend in the cyclic potentiodynamic polarization curves, although it was not fully defined.
- The passivated 17-7PH and 410 SS steels exhibited positive hysteresis, which indicates that they are susceptible to localized corrosion.
- The results obtained following SEM analysis of the electrochemically tested samples indicated the presence of localized corrosion (pitting), and for the 410 SS, a higher density of pits compared to that for 17-7PH stainless steel was found, showing 50 and 100 μm pit sizes, respectively.
- The XPS analysis indicated different chemical species on the surface films of the 17-7PH and 410 SSs, such as Cr2O3, Cr (OH)3, FeOOH, and Fe2O3. The passive films contained iron chromium oxide and hydroxide.
- The 17-7PH SS samples passivated at 49 °C for 90 min in citric and nitric baths exhibited the best performance.
- The application of the citric acid passivation process to passivated stainless steels could be an environmentally friendly alternative to the frequently used nitric acid passivation process.
- The potentiodynamic polarization results indicated that 17-7PH stainless steel passivated in citric and nitric acid showed lower corrosion rate values (in the order of ×10−3 mm/yr).
- XPS analysis allowed us to determine that the surface film of the 17-7PH and 410 SS samples analyzed in this work consisted of different chemical species, such as Cr2O3 and Fe (OH)O.
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Material | Elements (wt.%) | ||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
C | Cr | Ni | Mo | Mn | Cu | Ti | N | Nb | W | V | Al | Fe | |
17-7PH | 0.09 | 16.64 | 7.17 | 0.19 | 0.88 | 0.24 | 0.10 | 0.10 | 0.034 | 0.034 | 0.106 | 1.1 | Balance |
410 SS | 0.15 | 13.5 | 0.75 | -- | 0.5 | -- | -- | -- | -- | -- | -- | 0.5 | Balance |
Sample | Material | Temperature (°C) | Time (min) | Passivation Baths |
---|---|---|---|---|
A1 (Control) | 17-7PH | -- | -- | -- |
B1 (Control) | 410 SS | -- | -- | -- |
A2 | 17-7PH | 49 | 90 | Citric Acid C6H8O7 |
B2 | 410 SS | 49 | 90 | |
A3 | 17-7PH | 49 | 90 | Nitric Acid HNO3 |
B3 | 410 SS | 49 | 90 |
Sample | Cr | Mo | N | W | PREN |
---|---|---|---|---|---|
17-7PH | 16.64 | 0.190 | 0.10 | 0.034 | 18.92 |
410SS | 13.5 | - | - | - | 13.5 |
Samples: | 17-7 | 410 SS | ||||
---|---|---|---|---|---|---|
Element | Peak | Binding Energy (eV) | Citric | Nitric | Citric | Nitic |
Fe 2p3/2 | Fe metal | 706.6 | 0.296 | 0.345 | 0.071 | 0.395 |
FeO | 708.4 | 0.207 | 0.214 | 0.054 | 0.307 | |
Fe3O4 | 709.8 | 0.497 | 0.441 | 0.573 | 0.298 | |
FeOOH | 710.3 | - | - | 0.302 | - | |
Cr 2p3/2 | Cr metal | 574.2 | 0.154 | 0.096 | 0.094 | 0.107 |
Cr2O3 | 576.1 | 0.497 | 0.526 | 0.499 | 0.501 | |
Cr (OH)3 | 577.3 | 0.349 | 0.378 | 0.407 | 0.392 |
Sample | Ecorr (Volts) | Epit (Volts) | Erp (Volts) | icorr (A/cm2) | σicorr (A/cm2) | ipass (A/cm2) | Passive Range (Volts) | CR (mm/year) | Hysteresis |
---|---|---|---|---|---|---|---|---|---|
Control A1 | −0.364 | 0.062 | −0.238 | 1.146 × 10−6 | ±4.137 × 10−3 | 1.023 × 10−6 | 0.323 | 1.325 × 10−2 | Positive |
A2 | −0.341 | 0.311 | −0.276 | 1.8638 × 10−7 | ±4.292 × 10−3 | 4.4791 × 10−7 | 0.450 | 2.1345 × 10−3 | Positive |
A3 | −0.420 | 0.133 | −0.263 | 2.5118 × 10−7 | ±4.184 × 10−3 | 1.1230 × 10−6 | 0.427 | 2.9131 × 10−3 | Positive |
Control B1 | −0.380 | −0.170 | −0.440 | 1.113 × 10−6 | ±2.650 × 10−3 | 2.1682 × 10−6 | 0.492 | 1.2908 × 10−2 | Positive |
B2 | −0.687 | −0.154 | −0.531 | 1.1945 × 10−6 | ±2.361 × 10−3 | 5.7451 × 10−6 | 0.646 | 1.3854 × 10−2 | Positive |
B3 | −0.858 | −0.183 | −0.468 | 2.5971 × 10−6 | ±2.636 × 10−3 | 1.5502 × 10−5 | 0.857 | 3.0121 × 10−2 | Positive |
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Martínez-Aparicio, B.; Gaona-Tiburcio, C.; Almeraya-Calderon, F.; Goldsberry, R.; Castaneda, H. Evaluation of Passive Films on 17-7PH and 410 Stainless Steel Exposed to NaCl Solution. Materials 2024, 17, 4060. https://doi.org/10.3390/ma17164060
Martínez-Aparicio B, Gaona-Tiburcio C, Almeraya-Calderon F, Goldsberry R, Castaneda H. Evaluation of Passive Films on 17-7PH and 410 Stainless Steel Exposed to NaCl Solution. Materials. 2024; 17(16):4060. https://doi.org/10.3390/ma17164060
Chicago/Turabian StyleMartínez-Aparicio, Brisa, Citlalli Gaona-Tiburcio, Facundo Almeraya-Calderon, Reece Goldsberry, and Homero Castaneda. 2024. "Evaluation of Passive Films on 17-7PH and 410 Stainless Steel Exposed to NaCl Solution" Materials 17, no. 16: 4060. https://doi.org/10.3390/ma17164060