Data Mining Applied to the Electrochemical Noise Technique in the Time/Frequency Domain for Stress Corrosion Cracking Recognition
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials and Testing Conditions
2.2. Hilbert–Huang Transform Approach
- Executing the sifting process on the s(t), obtaining an IMF denominated as dn(t).
- Calculating the residual r(t) = sn−1(t) − dn(t) (then, this residual is considered a new s(t)).
- Extracting relative extremes, obtaining two functions: v1(t) is the interpolation of the maxima point, and v2(t) is the interpolation of the minima point
- Determining the m(t) function as m(t) = 1/2(v1(t) + v2(t))
- Extracting d(t) = s(t) − m(t)
3. Results and Discussion
3.1. Time Domain Analysis
3.2. Frequency Domain Analysis
3.3. Time-Frequency Domain Analysis
- At first, up to 1500 s, a low electrochemical activity region can be identified. As previously discussed, this stage could be related with the pre-activation corrosion phase. At very short times the electrochemical activity is not representative. However, with increasing time, the intensity of the IMF progressively increases. The first intensity and wide peak, point A in Figure 10, occurs at about 1000 s, in correspondence with the triggering of metastable pits [61]. Consequently, this phase can be associated with the superficial electrochemical activation of the specimen [62].
- The pre-activation stage continues to evolve during time, with the presence of several sub-peaks (point B in Figure 10), up to about 2000 s, in correspondence with the activation and propagation of superficial pits. Subsequently the IMF signal undergoes a sharp reduction in intensity, during which there are only occasional signal spikes (point B’ in Figure 10). During this time, in the time interval 2000–10,000 s, predominantly, the pit-to-crack transition takes place. The triggering of the SCC phenomenon obviously stimulates the defect evolution partly by mechanical contribution making therefore the electrochemical one less significant. The occasional secondary IMF peaks, identified by point B’, may be associated with the local formation and propagation of additional surface pits that evolve simultaneously during the stress corrosion triggering phase.
- After about 10,000 s a third stage was defined as short to long range crack propagation can be identified. During this stage several fluctuations in IMS signal can be highlighted. In particular After a long electrochemical quiescence step (point C in Figure 10) a significant peak can be identified at about 16,000–18,000 s (point C’ in Figure 10). This trend related to stabilization and abrupt increase steps in IMF noise current signal is periodically identifiable. This behaviour is caused by the crack evolution by SCC [36]. At this stage, the size of the crack can reach a length sufficient to assume that the stress concentration at the crack tip becomes significant, thus implying that there is a large area of plastic deformation, leading to a more extensive blunt at the crack tip. Due to the crack reshape, the mechanical crack evolution mechanism is inhibited, despite electrochemical dissolution [48]. Consequently, a phase of electrochemical stabilization associated with the mechanical evolution of SCC damage is complementary to a phase of metal dissolution at the crack tip, and, therefore, complementary to an electrochemical activity phase. Depending on various electrochemical dissolution factors, the current transient generated by the micro-crack opening and re-passivation can last for a few seconds [63]. These sub-steps alternate cyclically during this stage (points C* in Figure 10), where the sub-critical propagation of the medium and long-range crack takes place.
- After about 45,000 s, after a transient region (coded as pre-quiescence), a large electrochemical plateau in the IMF signal can be identified (above 48,000 s). During this step, no relevant electrochemical vents can be identified. This stage is the prelude for the critical failure of the sample that took place after about 58,000s.
- Stabilization: at first, in the rage 0–100 s (step I in Figure 11), the noise signal is not characterised by any significant fluctuations. EN transient related to this phenomenon is characterised by the absence of high-frequency events: only some events at about 10−3 Hz can be observed. In this phase, the interaction between the electrolyte and specimen surface takes place, with an unstable alternation of general corrosion and passivation phases. The aggressive ions locally destabilize the passive oxide layer of the sample, causing a local thinning of the oxide. This process has a short duration (approximately 100 s) due to the high aggressiveness of the environment conditions of the test.
- Electrochemical activation: in the range 100–1500 s (step II in Figure 11), in correspondence with depassivated surface regions, the electrochemical activity is enhanced and the pit initiation stage extends to micrometre-sized, large dissolved holes. In this phase, an increase in the cumulative charge trend was also identified. This sub-stage is identified by a high activity at medium and low frequencies. In particular, at increasing time (after about 500 s) and with a progressive increment in the number of pits on the surface, the signal activity evolves towards a higher frequency (from 2 × 10−2 to 5 × 10−1 Hz, defining two substep: IIa and Iib). This stage can be related with the electrochemical activation phase (Iia) and the subsequent triggering of metastable pits (Iib) on the sample surface [14].
- SCC Activation and Propagation: This region, ranging from 1500 to 10,000 s, can be related mainly with the SSC triggering by short range crack activation. At this stage, the electrochemical activity becomes significant. Some sub-clusters can be identified. At first, region IIIa, as shown in Figure 11, suggests that high-frequency contribution can be identified. At this stage, the aggressive ions locally destabilize the passive oxide layer of the sample, causing a local thinning of the oxide. In correspondence with depassivated surface regions, the electrochemical activity is enhanced and the pit initiation stage extends to micrometre-sized, large dissolved holes (see pit in Figure 12d). This process leads to the formation of preferential areas of localized attacks by pitting, identifiable by a high magnitude of the IMF. Progressively, the signal activity evolves towards a lower frequency (from 5 × 10−3 to 5 × 10−2 Hz) and magnitude (from 100.4 to 10−0.4 dB), as shown via region IIIb in Figure 11. In this low frequency phase, the mechanical contribution is more relevant than the electrochemical one, as evidenced by the low EN signal magnitude, indicating that SCC short-range activation of the cracks was triggered [14].
- SCC propagation. At about 10,000 s, a new step begins. During this step, the SCC damage evolution phase of the sample occurs (in Figure 12c, it is possible to note a secondary crack originating from a pit). The progressive crack growth (region III) leads to an increase in the region of plastic deformation at the crack tip [64]. This implies that a more severe anodic dissolution is needed by the crack to re-sharpen before inducing a further propagation. At this phase, in fact, the dissolution within the crack is still taking place. When increasing the crack length, an increase in stress concentration occurs, which induces a larger plastic zone ahead of the crack tips. As a result, the crack point becomes more blunted. A larger plastic zone suggests that it will take more time for the fracture to be re-sharpened via dissolving for future crack propagation. This phase was indeed indicated as a mechanical quiescence [53] and the driving force in crack propagation. This stage shows metal dissolution at the crack tip. This region could correspond to the high-frequency activity in the first IMF. The electrochemical dissolution (sub-steps IVa in Figure 11), identifiable via the step-wise increase in cumulative charge (Figure 5), stimulates the mechanical instability of the crack (sub-steps IVb in Figure 11), primed for future subsonic propagation. Consequently, this stage identifies the prelude to the catastrophic failure of the specimen. In the topological map, this region is identified by medium-low amplitude valleys alternating with high-frequency peaks (5 × 10−2–3 × 10−1 Hz). Afterwards, for times above 45,000 s, the Hilbert spectrum shows a low magnitude region where an electrochemical quiescence occurs. Finally, for catastrophic failure, the sample takes place after about 58,000s.
4. Conclusions
- Stabilization: at first, in the rage 0–100 s. The EN transient is characterised by the absence of high-frequency events. Only some events at about 10−3 Hz were observed.
- Electrochemical activation: in the range 100–1500 s. This stage was identified by a high activity at medium and low frequencies (from 2 × 10−2 to 5 × 10−1 Hz,). This stage can be related with electrochemical activation and the subsequent triggering of metastable pits on the sample surface.
- SCC Activation and Propagation: ranging from 1500 to 10,000 s. This is mainly related to the SSC triggering by short-range crack activation. At this stage, the electrochemical activity became significantly identifiable by a high magnitude of IMF. Then, progressively, the signal activity evolved towards a lower frequency (from 5 × 10−3 to 5 × 10−2 Hz) and magnitude (from 100.4 to 10−0.4 dB), because the mechanical contribution was more relevant than the electrochemical.
- SCC propagation. Above 10,000 s. This is related to progressive crack growth. This region was identified by medium–low amplitude valleys alternating with high-frequency peaks (5 × 10−2–3 × 10−1 Hz). For times above 45,000 s a low magnitude region, related to an electrochemical quiescence, was identified before catastrophic failure of the samples.
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
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Composition [wt %] | |||||||||
---|---|---|---|---|---|---|---|---|---|
C | Ni | Cr | S | P | Cu | Mn | Si | Nb | Fe |
0.042 | 4.43 | 15.10 | 0.005 | 0.02 | 3.31 | 0.44 | 0.50 | 0.22 | balance |
Mean Mechanical Properties | ||
---|---|---|
Yield stress fp 0.2k (MPa) | Ultimate tensile stress UTS fpk (MPa) | Elongation εuk (%) |
745 | 1010 | 24 |
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Calabrese, L.; Galeano, M.; Proverbio, E. Data Mining Applied to the Electrochemical Noise Technique in the Time/Frequency Domain for Stress Corrosion Cracking Recognition. Corros. Mater. Degrad. 2023, 4, 659-679. https://doi.org/10.3390/cmd4040034
Calabrese L, Galeano M, Proverbio E. Data Mining Applied to the Electrochemical Noise Technique in the Time/Frequency Domain for Stress Corrosion Cracking Recognition. Corrosion and Materials Degradation. 2023; 4(4):659-679. https://doi.org/10.3390/cmd4040034
Chicago/Turabian StyleCalabrese, Luigi, Massimiliano Galeano, and Edoardo Proverbio. 2023. "Data Mining Applied to the Electrochemical Noise Technique in the Time/Frequency Domain for Stress Corrosion Cracking Recognition" Corrosion and Materials Degradation 4, no. 4: 659-679. https://doi.org/10.3390/cmd4040034