CN210604325U - Stress corrosion cracking on-line monitoring device based on electrochemical noise - Google Patents
Stress corrosion cracking on-line monitoring device based on electrochemical noise Download PDFInfo
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Abstract
The utility model relates to the field of electrochemical corrosion monitoring, in particular to an electrochemical noise-based stress corrosion cracking online monitoring device, wherein a jacket electrolytic cell is arranged in a stress ring, and an SCC _ WE1 test electrode is positioned in the center of the jacket electrolytic cell; the test electrodes SCC _ WE2 are symmetrically distributed around the test electrode SCC _ WE1, the zero-resistance galvanometer is respectively connected with the test electrode SCC _ WE1 and the test electrode SCC _ WE2, and the potential follower is respectively connected with the test electrode SCC _ WE1 and the reference electrode RE. Distinguishing different stages of SCC crack propagation through different types of current/potential noise peak characteristics, and calculating the single crack propagation length and the average crack propagation rate according to the noise peak integral electric quantity and the occurrence frequency; and the sensitivity of the SCC is evaluated according to the amplitude of the current noise peak, so that the dynamic monitoring of the microcrack initiation and growth process is realized.
Description
Technical Field
The utility model relates to an electrochemical corrosion monitoring field specifically is a stress corrosion cracking on-line monitoring device based on electrochemical noise.
Background
During the production of oil and gas fields, CO2The tertiary oil recovery technologies such as flooding and the like can obviously improve the oil and gas recovery rate, and if the technology is adopted in the medium oil Jilin oil field, the oil and gas recovery rate is improved by 5-10 percent, so that a good demonstration effect is obtained. But CO2Dissolution in the downhole annular solution can lead to Stress Corrosion Cracking (SCC) of the oil casing under the combined effects of stress and corrosive environment. Research shows that P110 tubing steel contains CO2Can suffer toughness degradation in low temperature annular fluid environments, resulting in SCC. 316L stainless steel in H2S-CO2-Cl-In the environment, will follow H2S/CO2An increase in the partial pressure ratio leads to an increase in SCC sensitivity. The stress corrosion cracking has a propagation rate that is many orders of magnitude higher than other forms of corrosion without obvious symptoms, so that SCC failure of the tubing steel is often sudden and catastrophic, resulting in significant economic loss and casualties. Therefore, the early diagnosis of the SCC is realized through a nondestructive monitoring technology, the fault can be timely found, the accident can be prevented, and the method has important significance for the safety production of oil and gas fields.
Chinese utility model application CN 106568665a discloses a high strength pipeline soil SCC evaluation method, which calculates its residual strength mainly through the pipeline surface defect, and does not propose a corresponding SCC monitoring method. CN 106404554a discloses a test device for studying SCC of sulfate reducing bacteria, which studies the influence of sulfate reducing bacteria on metal SCC by regularly observing the conditions of crack nucleation and propagation on the surface of a test sample, but cannot realize in-situ nondestructive monitoring of SCC. CN 105675481a proposes an electrochemical experimental apparatus and a test method for corrosion of a sample loaded with tensile stress in a high-temperature and high-pressure fluid environment, which obtains the action mechanism of the tensile stress at high temperature and high pressure and the corrosion of the fluid on the metal material through electrochemical parameters, but does not propose an algorithm for SCC crack initiation or growth process.
The corrosion of the tubing steel in the underground annular solution belongs to electrochemical corrosion, and the uniform corrosion and the environmental corrosivity of the material can be monitored by adopting a hanging piece method, an electrochemical impedance method, a linear polarization method and the like. However, these conventional electrochemical methods have difficulty monitoring stress corrosion cracking caused by localized corrosion. The electrochemical noise monitoring technology can not only obtain the local corrosion information of the metal material, but also has no external interference to a test system, and can truly reflect the corrosion state of the material.
The electrochemical noise signal analysis method mainly comprises time domain statistical analysis, frequency domain analysis and wavelet analysis at present. The time domain analysis method is most widely applied, but the statistical analysis method based on the noise resistance cannot judge the occurrence time node and the severity of the local corrosion; the frequency domain analysis is easily influenced by background noise interference and signal drift, and the calculation error is large; the noise analysis algorithm based on wavelet transformation is complex, and real-time online analysis cannot be realized. The above problems have significantly limited the use of electrochemical noise techniques for in situ corrosion monitoring. In chinese patent CN107202755A, an electrochemical noise sensor is used to test the potential and current noise on the outer surface of the metal pipe, and the corrosion state of the metal pipe is evaluated according to the noise resistance calculated from the standard deviation of the current potential; in CN103983564A, corrosion of metal materials is monitored by an atmospheric corrosion electrochemical sensor, and a wavelet noise resistance close to 2Hz is used for reflecting the corrosion rate in the atmospheric corrosion process; in CN101017128A, a four-electrode probe electrochemical noise device is used to collect noise signals, and then statistical calculation and cluster analysis are performed on the data by software to determine the degree of local corrosion. However, no monitoring method for stress corrosion cracking has been reported.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the not enough of oil casing steel stress corrosion cracking monitoring technology, provide a stress corrosion cracking nondestructive monitoring method for evaluate the stress corrosion cracking of material and SCC sensitivity promptly. The purpose of the utility model is realized through the following technical scheme.
The device comprises a reference electrode RE, an SCC _ WE2 test electrode, an SCC _ WE1 test electrode, a rubber sealing ring, a jacket electrolytic cell, a stress ring, a tension meter, a zero-resistance ammeter, a potential follower and a signal acquisition and analysis unit;
the jacket electrolytic cell is arranged in the stress ring and is connected with the tension meter;
the test electrode SCC _ WE1 and the test electrode SCC _ WE2 are round rod-shaped metal samples made of the same material, the test electrode SCC _ WE1 is positioned in the center of the jacket electrolytic cell, two ends of the test electrode SCC _ WE1 are in tensile stress, four or six test electrodes SCC _ WE2 are symmetrically distributed around the test electrode SCC _ WE1, the surface of the test electrode SCC _ WE1 is ensured to be uniformly polarized, and the noise capture accuracy is improved; the bottom of the SCC _ WE1 test electrode and the SCC _ WE2 test electrode are sleeved with rubber sealing rings and then are installed in a jacketed electrolytic cell;
the zero-resistance galvanometer is respectively connected with the SCC _ WE1 test electrode and the SCC _ WE2 test electrode, and amplifies noise current from the SCC _ WE1 test electrode and the SCC _ WE2 test electrode through a precise current-voltage conversion circuit;
the potential follower is respectively connected with the SCC _ WE1 test electrode and the reference electrode RE, and the potential follower carries out impedance change on a noise voltage signal from the SCC _ WE1 test electrode relative to the reference electrode RE through a high-resistance voltage follower circuit;
the zero resistance current meter and the potential follower are connected with the signal acquisition and analysis unit, and all signals are sent to the signal acquisition and analysis unit.
The signal acquisition and analysis unit mainly comprises two multi-channel low-pass filters, two 24-bit A/D converters, a display/keyboard interface, a single chip microcomputer, a USB communication port and a Flash ROM nonvolatile memory;
the two multichannel low-pass filters are respectively connected with the zero-resistance galvanometer and the potential follower, each multichannel low-pass filter is respectively connected with an A/D converter, and the two 24-bit A/D converters are both connected with the single chip microcomputer; the singlechip is also connected with a USB communication port, a nonvolatile memory and a display/keyboard interface.
The current noise from the zero resistance current meter and the voltage noise signal from the potential follower pass through a 10 Hz-20 Hz LPF low pass filter to eliminate power frequency interference and aliasing noise, and then are sent to an A/D converter, the AD converter adopts the sigma-delta integral/differential principle to further eliminate power frequency and electromagnetic interference, all digital signals are sent to a single chip microcomputer to carry out data analysis, noise characteristic parameters in the SCC process are calculated, and a test result is stored in a nonvolatile memory or is uploaded to a PC computer through a USB communication port, and can also interact with a user through a display/keyboard interface.
The electrochemical noise analysis method of the utility model is carried out according to the following steps:
(1) collecting potential and current noise signals in the stress corrosion cracking process by using the electrochemical noise monitoring device, and calculating the service life (L) of a noise peak by using an analysis program compiled by matlabc) Amplitude (A)c) Integral electric quantity (q)c) A parameter;
(2) classifying electrochemical noise peaks with different parameter values, wherein different corrosion events are accompanied by different types of current/potential noise peaks, the noise peaks with short service life (3-5 s), low amplitude (0.01-1 muA) and small integrated electric quantity (0.1-1.0 muC) represent the occurrence of a metastable state pitting corrosion event, and SCC (continuous casting) crack events can cause strong current potential noise peaks with long service life (>30s), high amplitude (>1 muA) and large integrated electric quantity (>30 muC);
(3) carrying out statistical analysis on a metastable state pitting peak generated by a pitting event, judging the speed of a local corrosion rate according to the size of a nucleation rate lambda, and calculating a noise resistance R from a potential current standard deviation valuenBy comparison, the consistency of the results can be found; the growth time of a single crack can be obtained by analyzing the service life of a noise peak of a crack event, the growth length of the single crack can be obtained by an integral electric quantity value, and the stress corrosion cracking sensitivity of the single crack can be compared according to the length of the growth time and the length of the crackA perceptual property;
(4) taking fixed length time as a statistical window, and carrying out nucleation rate l and average integral electric quantity on electrochemical noise signals
Performing statistical analysis according to l and
the time points of the SCC crack initiation stage, crack propagation stage and rapid fracture stage can be judged according to the change curve along with time.
The utility model has the advantages that:
(1) a high-precision noise signal acquisition and analysis unit circuit is adopted, so that weak potential and current noise signals in the stress corrosion cracking process can be sensitively captured;
(2) according to the electrochemical noise statistical analysis result, the degree and the category of local corrosion can be judged, the germination and growth rate of the SCC crack can be calculated, and an online monitoring method is provided for early diagnosis of the SCC.
Drawings
FIG. 1 is a schematic view of the testing device of the present invention;
FIG. 2 is a circuit diagram of the electrochemical noise signal collection and analysis of the present invention;
FIG. 3 shows the steel of example P110 containing CO2Tensile curve and electrochemical noise in annular solution: i: elastic stage, II: yield stage, iii: hardening stage, IV: a necking stage;
FIG. 4 is an electrochemical noise signature of the crack initiation stage during an example SCC test;
FIG. 5 is an electrochemical noise signature of the crack growth process during the SCC test of the example;
FIG. 6 shows the nucleation rate (λ) and the average integrated electrical quantity (q) of electrochemical noise during the SCC test of examplec)；
FIG. 7 is a cross-sectional profile of the SCC test electrode after the end of the example test after fracture.
Detailed Description
The present invention and the technical solution thereof will be further explained with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, the SCC online monitoring device based on electrochemical noise includes a reference electrode RE1, an SCC _ WE2 test electrode 2, an SCC _ WE1 test electrode 3, a rubber seal ring 4, a jacketed electrolytic cell 5, a stress ring 6, a tension meter 7, a zero-resistance current meter 8, a potential follower 9, and a signal acquisition and analysis unit 10;
the jacket electrolytic cell 5 is placed in the stress ring 6 and is connected with the tension meter 7;
the test electrode 3 of SCC _ WE1 and the test electrode 2 of SCC _ WE2 are round bar-shaped metal samples made of the same material, the test electrode 3 of SCC _ WE1 is arranged in the positive of the jacket electrolytic cell 5, two ends of the test electrode are in tensile stress, four or six test electrodes 2 of SCC _ WESCC _ WE2 are symmetrically distributed around the test electrode 3 of SCC _ WE1, the surface of WE1 is ensured to be uniformly polarized, and the noise capture accuracy is improved; the reference electrode SCC _ WE1 test electrode 3 can be a saturated calomel electrode, an Ag/AgCl electrode or a mercurous sulfate electrode, the SCC _ WESCC _ WE1 test electrode 3 and the SCC _ WESCC _ WE2 test electrode 2 are made of P110 tubing steel, are processed into a round bar-shaped test sample according to the GB/T15970 once 2017 standard, and are mounted in the jacket electrolytic cell 5 after being sleeved with a rubber sealing ring 4 at the bottom. Four SCC _ WESCC _ WE2 test electrodes 2 were selected for this example.
The zero-resistance current meter 8 is respectively connected with the SCC _ WESCC _ WE1 test electrode 3 and the SCC _ WESCC _ WE2 test electrode 2, and the zero-resistance current meter 8 amplifies noise current from the SCC _ WESCC _ WE1 test electrode 3 and the SCC _ WESCC _ WE2 test electrode 2 through a precise current-voltage conversion circuit;
the potential follower 9 is respectively connected with the SCC _ WE1 test electrode 3 and the reference electrode RE1, and the potential follower 9 changes the impedance of a noise voltage signal from the SCC _ WE1 test electrode 3 relative to the reference electrode RE1 through a high-impedance voltage follower circuit;
the zero resistance current meter 8 and the potential follower 9 are both connected with the signal acquisition and analysis unit 10, and all signals are sent to the signal acquisition and analysis unit 10.
The temperature of the jacket electrolytic cell 5 is controlled to be 35-60 ℃ by a dieSimulating the temperature of the underground annular space solution, and filling the jacket electrolytic cell 5 with a simulated annular space protective solution with the composition of 0.2mol/L Na2CO3、0.5mol/L NaHCO30.5mol/L NaCl and 100mg/L Na2And S. Except that the surface of a round rod of which the middle is 5-10 mm long is exposed, the rest of the SCC _ WE1 test electrode 3 is protected by organic silicon resin on the contact surface with the solution, so that crevice corrosion is prevented. The SCC _ WE1 test electrode 3 is subjected to constant strain or slow strain stretching through a stress ring 6 or a slow tensile testing machine, 4 SCC _ WE2 test electrodes 2 are used as counter electrodes and distributed around WE13, the counter electrodes are not stressed, electrochemical potential and current noise are respectively connected to the input ends of a potential follower 9 and a zero-resistance ammeter 8, feedback resistance Rc of the zero-resistance ammeter 8 is subjected to self-adaptive control, and the resistance value of the switching Rc is automatically set according to the current.
As shown in fig. 2, the signal collecting and analyzing unit 10 mainly includes two multi-channel low-pass filters 11, two 24-bit a/D converters 12, a display/keyboard interface 13, a single chip 14, a USB communication port 15 and a Flash ROM nonvolatile memory 16;
the two multi-channel low-pass filters 11 are respectively connected with the zero-resistance ammeter 8 and the potential follower 9, each multi-channel low-pass filter 11 is respectively connected with an A/D converter 12, and the two A/D converters 12 are both connected with the single chip microcomputer 14; the single chip 14 is also connected with a USB communication port 15, a nonvolatile memory 16 and a display/keyboard interface 13.
Firstly, the potential and the current noise are subjected to anti-aliasing and denoising respectively through a 20Hz cut-off frequency multichannel low-pass filter 11 and then sent to two ADS1210 converters 12 for analog-to-digital conversion, and the sampling frequency is 5 Hz. The digitized potential and current noise signals are read into a memory by a 32-bit STM32F407 singlechip 14, statistical analysis is carried out on the noise by adopting a later algorithm, and the measurement result is stored in a 16M byte Flash ROM nonvolatile memory 16 or is uploaded to a PC computer from a USB communication port 15 by means of interaction of a display/keyboard interface 13 for further analysis.
The utility model provides a SCC monitoring adopts electrochemistry noise statistics analysis algorithm, calculates SCC _ WE1 test electrode 3's metastable state pitting and crackle emergence and growthLength and according to the lifetime (L) of the current and potential noise peaksc) Amplitude (A)c) And the integral electric quantity (q)c) To determine the stage and severity of SCC progression.
And (3) automatically counting the frequency, the service life, the amplitude, the integral electric quantity, the nucleation rate, the noise resistance and the average integral electric quantity of an electrochemical noise peak by adopting a Matlab 2012 programming program, wherein the integral electric quantity and the average integral electric quantity are calculated as formulas (1) and (3), and the crack length is calculated as formula (2).
Peak noise life (L)c) The difference between the start and end times of the noise peak, the peak amplitude (A)c) The difference between the current values at the highest and lowest noise peaks. Electrochemical noise peak integrated electrical quantity (q)c) The calculation formula of (2) is as follows:
in the formula (1), lambda is a nucleation rate and represents the number of noise peaks in unit time, and the unit is s-1(ii) a T is the duration of the measurement of the noise data, Tn、t'nRespectively the start and end times, i, of the nth noise peakn(t) is a function of current and time corresponding to the nth noise peak, ibThe baseline current for the noise peak.
According to the nucleation rate (λ), the SCC crack propagation speed can be determined, and the larger l is, the larger the number of cracks generated per unit time is, which indicates that the SCC process is faster. Integral electric quantity (q) according to single noise peakc) The value can be used for calculating the single crack growth length, and q can be calculated according to Faraday's lawcCorresponding metal dissolution volume, qcThe greater the degree of corrosion. If the shape of the crack front end is semicircular and the crack width w is 500nm, the crack width can be increased by qcEstimating the corresponding crack growth depth lcrackThe calculation formula is as follows:
m, rho and z in the formula (2)In terms of the molar mass (g/mol) and density (g/cm) of the metal, respectively3) And a valence number; f is a Faraday constant; q. q.scIs the integrated electric quantity.
FIG. 3 shows the potential and current noise data emitted from the simultaneous monitoring of SCC _ WE1 test electrode 3 and SCC _ WE2 test electrode 2 in a slow strain tensile test. According to the tensile curve form of the SCC _ WE1 test electrode, the tensile test process can be divided into four deformation stages, namely an elastic stage, a yield stage, a hardening stage and a necking stage, and the electrochemical noise characteristics of each stage are obviously different, so that the stage of the SCC test electrode can be judged according to the noise peak characteristics.
FIG. 4 is a plot of the electrochemical noise of the test electrode 3, SCC _ WE1, in simulated annular protection fluid, during the pre-crack initiation period (major metastable pitting events). The generation of pitting corrosion event is accompanied by a plurality of metastable pitting corrosion peaks with short service life, low amplitude and small integral electric quantity, and after the passivation film on the surface of the test electrode 3 of SCC _ WE1 is broken, the generation of metastable pitting corrosion makes the potential of the electrode move negatively, and then the repassivation of corrosion points makes the potential move positively again, and the continuous rapid dissolution-repassivation-dissolution processes form typical metastable pitting corrosion noise peaks on the electrochemical noise curve.
FIG. 5 shows the electrochemical noise peak corresponding to the crack growth on the surface of the SCC _ WE1 test electrode 3 during the slow tensile test, and the crack length l can be estimated from equation (2)crackAnd 164 μm. FIG. 7 shows a cross-sectional profile of the SCC _ WE1 test electrode 3 port, from which FIG. 7 the crack growth depth was measured to be about 123 μm, which is closer to the calculation of equation (2). Crack event noise peak qcThe larger, the single crack growth depth lcrackThe longer the metal, the higher the SCC sensitivity.
Then taking 1h as unit time, the nucleation rate lambda and the average integral electric quantity of the whole electrochemical noise spectrum
The statistical analysis is carried out and the analysis is carried out,
the calculation formula of (2) is as follows:
FIG. 6 shows λ and
curves as a function of SCC test time, lambda and
when the two are smaller, the surface of the metal sample has no obvious local corrosion, and the lambda is gradually increased
The slight increase indicates that the metal surface develops metastable pitting which promotes the microcracking into the initiation phase. When in use
And when the micro-crack is in an obvious increasing trend, the micro-crack is shown to form a steady-state crack under the action of tensile stress, the electrochemical noise peak is mainly a long crack event peak with longer service life and larger integral electric quantity, and the SCC electrode enters a crack steady-state growth stage. When in use
When the crack starts to descend, the crack expansion tends to be stable, the crack tip is in a high-activity dissolution state, the crack tip is not easy to passivate, the noise current does not descend any more, the noise peak nucleation frequency is reduced, and the SCC electrode enters a crack expansion stage. When λ and
when the trend gradually approached 0, indicating that the noise peak was completely gone, the SCC test electrode crack tip was in a fast anodic dissolution state and entered the fast tear stage.
Claims (2)
1. The device is characterized by comprising a reference electrode RE (1), an SCC _ WE2 test electrode (2), an SCC _ WE1 test electrode (3), a rubber sealing ring (4), a jacket electrolytic cell (5), a stress ring (6), a tension meter (7), a zero-resistance ammeter (8), a potential follower (9) and a signal acquisition and analysis unit (10);
the jacket electrolytic cell (5) is arranged in the stress ring (6) and is connected with the tension meter (7);
the test electrode (3) of SCC _ WE1 and the test electrode (2) of SCC _ WE2 are round bar-shaped metal samples made of the same material, the test electrode (3) of SCC _ WE1 is arranged in the center of the jacket electrolytic cell (5), the two ends of the test electrode are in tensile stress, and four or six test electrodes (2) of SCC _ WE2 are symmetrically distributed around the test electrode (3) of SCC _ WE 1; the bottoms of the SCC _ WE1 test electrode (3) and the SCC _ WE2 test electrode (2) are sleeved with a rubber sealing ring (4) and then are installed in a jacketed electrolytic cell (5);
the zero-resistance current meter (8) is respectively connected with the SCC _ WE1 test electrode (3) and the SCC _ WE2 test electrode (2), and the zero-resistance current meter (8) amplifies noise current from the SCC _ WE1 test electrode (3) and the SCC _ WE2 test electrode (2) through a precise current-voltage conversion circuit;
the potential follower (9) is respectively connected with the SCC _ WE1 test electrode (3) and the reference electrode RE (1), and the potential follower (9) changes the impedance of a noise voltage signal from the SCC _ WE1 test electrode (3) relative to the reference electrode RE (1) through a high-impedance voltage follower circuit;
the zero resistance ammeter (8) and the potential follower (9) are connected with the signal acquisition and analysis unit (10), and all signals are sent to the signal acquisition and analysis unit (10).
2. The electrochemical noise-based stress corrosion cracking online monitoring device according to claim 1, wherein the signal acquisition and analysis unit (10) mainly comprises two multi-channel low-pass filters (11), two A/D converters (12), a display/keyboard interface (13), a single chip microcomputer (14), a USB communication port (15) and a Flash ROM nonvolatile memory (16);
the two multi-channel low-pass filters (11) are respectively connected with the zero-resistance ammeter (8) and the potential follower (9), each multi-channel low-pass filter (11) is respectively connected with an A/D converter (12), and the two A/D converters (12) are both connected with the single chip microcomputer (14); the singlechip (14) is also connected with a USB communication port (15), a nonvolatile memory (16) and a display/keyboard interface (13).
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