CN114062006B - On-site sampling and electrochemical corrosion test method for concrete surface anti-corrosion material - Google Patents
On-site sampling and electrochemical corrosion test method for concrete surface anti-corrosion material Download PDFInfo
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- 238000005070 sampling Methods 0.000 title claims abstract description 68
- 238000005260 corrosion Methods 0.000 title claims abstract description 44
- 238000006056 electrooxidation reaction Methods 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000010998 test method Methods 0.000 title claims description 8
- 238000000576 coating method Methods 0.000 claims abstract description 65
- 238000012360 testing method Methods 0.000 claims abstract description 63
- 239000011248 coating agent Substances 0.000 claims abstract description 59
- 230000007797 corrosion Effects 0.000 claims abstract description 31
- 239000010865 sewage Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000005520 cutting process Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000000840 electrochemical analysis Methods 0.000 claims abstract description 10
- 238000005498 polishing Methods 0.000 claims abstract description 8
- 239000012085 test solution Substances 0.000 claims abstract description 8
- 230000010287 polarization Effects 0.000 claims abstract description 5
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- 229920002396 Polyurea Polymers 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 3
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000007517 polishing process Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000001238 wet grinding Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims 6
- 239000002351 wastewater Substances 0.000 claims 3
- 239000003112 inhibitor Substances 0.000 claims 2
- 239000002585 base Substances 0.000 claims 1
- 230000002401 inhibitory effect Effects 0.000 claims 1
- 239000010841 municipal wastewater Substances 0.000 claims 1
- 238000004065 wastewater treatment Methods 0.000 claims 1
- 239000003973 paint Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229920006334 epoxy coating Polymers 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
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- 238000002791 soaking Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
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- 150000003839 salts Chemical class 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/06—Devices for withdrawing samples in the solid state, e.g. by cutting providing a thin slice, e.g. microtome
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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Abstract
The invention provides a method for on-site sampling and electrochemical corrosion testing of a concrete surface anti-corrosion material, which comprises the following steps: 1. selecting a sampling point position: a. taking the side wall and the top of the sewage pool with serious corrosion as sampling positions to be tested, and sampling the side wall surface or the top of the sewage pool; b. the surface of the sampling part is in an attached state, is smooth and has no obvious holes or cracks; c. the sampling point is coated with at least 500 μm thick; 2. cutting the surface coating and ensuring the surface structure of the coating sample to be complete; 3. polishing the back of the cut surface coating, removing the attached concrete, and leaving a complete coating slice; coating slices are stuck to a metal backboard to prepare a tested electrode sample; 4. the test solution was configured as a test environment: 5. and carrying out electrochemical corrosion tests on the sample in different test solutions by using an electrochemical test platform, wherein the electrochemical corrosion tests at least comprise an open-circuit potential test, an alternating-current impedance test, an electrokinetic potential test and electrokinetic potential cyclic polarization.
Description
Technical Field
The invention relates to a method for on-site sampling and electrochemical corrosion test of a concrete surface anticorrosive paint.
Background
With the advancement of urban processes, new large-scale sewage treatment facilities become a necessary choice for coping with the increasing sewage treatment demands. Compared with the prior art, the novel large-scale sewage treatment plant has higher sewage flow rate, and the concentration of organic matters and the complexity of pollutants in the sewage are relatively higher, so that the concrete structure is corroded rapidly. However, the novel large sewage treatment plant is rotated to enter a full-load or overload running state after being built, and the time for stopping production, maintenance and overhaul are difficult to adjust.
It is therefore most common practice to extend the service life by painting the concrete surface with an anti-corrosive paint. However, most of the anticorrosive paint for concrete surfaces is damaged and fails in actual use under the expected service life. Therefore, in the early development and the model selection of the anti-corrosion coating, the corrosion resistance of the anti-corrosion coating is evaluated, and the method has important significance for the development of related products.
In the traditional anticorrosive coating evaluation means, salt spray tests and impressed current accelerated corrosion methods are mainly adopted, the two methods are carried out by brushing anticorrosive coatings on a metal substrate, deviation exists compared with the actual service environment, and most of anticorrosive coatings well-expressed in electrochemical corrosion tests have the phenomena of bubbling, chalking, water seepage, falling and the like when the service life of the anticorrosive coatings in the actual service environment is not reached. Therefore, in the selection and development of an anticorrosive paint, it is necessary to perform a corrosion resistance test for a concrete substrate. When the concrete substrate is used for corrosion resistance test, the concrete substrate is usually evaluated by means of surface roughness, water absorption, chromatic aberration, mass loss and the like, but the characteristics of different materials are different, so that quantitative evaluation is difficult to realize through the items.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art, and provides a field sampling and electrochemical corrosion test method for an organic anti-corrosion coating for concrete, which can accurately acquire the change of the corrosion resistance of a material in an actual service environment.
The technical problem to be solved can be implemented by the following means.
The on-site sampling and electrochemical corrosion test method for the concrete surface anticorrosive material is characterized by comprising the following steps of:
(1) Performing site investigation and selecting sampling points by combining with the actual service environment, wherein the selection rules are as follows:
1) Selecting a part with serious corrosion in actual service as a sampling position to be tested, wherein the sampling position to be tested at least comprises a group of side wall surfaces or tops of the sewage pool as the sampling position to be tested;
2) Normally, the corrosion damage amplitude of the side wall of the sewage pool is distributed longitudinally, and the point positions with different heights from the waterline can be selected for grouping sampling and measuring;
3) The method is applicable to organic inert coatings (epoxy, polyurea and the like) and is not applicable to permeable crystal coatings and concrete modifying admixtures; the surface of the sample is kept in an attached state and is approximately flat, and obvious holes and cracks are avoided;
4) The test method has certain requirements on thickness, and the sampling point is required to be coated with a film with the thickness of at least 500 mu m;
(2) The surface coating is cut by using a cutting tool, and the method is as follows:
1) Cutting the outline on the surface of the sampling coating by using a conventional cutter at the point position with relatively low adhesive force, and scraping a sampling article for sampling; sampling by using a handheld cutting machine at a point with relatively strong adhesive force;
2) The integrity of the surface structure of the coated sample should be ensured as much as possible during sampling, at least the area of 10mm by 10mm.
(3) Polishing the back of the cut coating, removing the concrete structure attached to the back of the coating, leaving only a complete coating slice, and pasting the coating slice on a metal backboard to prepare a tested electrode sample;
(4) Preparing at least one group of salt solution, one group of acid solution, one group of alkali solution and one group of reinforced sewage solution as test environments for performing subsequent electrochemical tests;
(5) Testing by using an electrochemical test platform, using a coating slice to paste a metal backboard as a working electrode, using a saturated calomel electrode/saturated KCl as a reference electrode, and using a platinum electrode as an auxiliary electrode to build a three-electrode system;
(6) The samples are subjected to electrochemical corrosion tests in different test solutions, wherein the tests comprise open circuit potential test (OPC), alternating current impedance test (EIS), electrokinetic potential Test (TAF), electrokinetic potential cyclic polarization and the like.
In the step (1), in the field sampling, the selected point is corroded to a certain extent and damaged and can keep complete adhesion, and for the coating which is obviously dropped and damaged, the anticorrosive material is considered to be invalid and does not have the conditions of sampling and electrochemical detection.
Preferably, in the on-site sampling in step (1), the sampling in the same sewage pool should at least comprise a group of side wall surfaces or tops of the sewage pool, and the sampling area of the single sewage pool should not be less than 3. The longitudinal distribution should be not less than 3 groups and at least one group of the covering waterline changing area when the side wall is sampled.
As a further improvement of the technology, in the sample preparation of the sampling coating in the step (3), the back surface of the coating needs to be polished, so that the surface of the coating is free from visible concrete adhesion to avoid the influence of the concrete on the test, the thickness of the coating part is ensured to be uniform as much as possible in the polishing process, and the acquired sample wafer is not less than 10mm multiplied by 10mm.
When polishing, equipment is used as much as possible for wet grinding, so that the influence of high temperature generated in the polishing process on the material performance is avoided.
After the coated sheet sample was obtained, the sheet was adhered to a stainless steel metal sheet of the same size using a conductive adhesive and sealed with an inert material as the working electrode in a three electrode system.
As a further improvement of the technology, the test solution prepared in the step (4) should be at least one type of salt solution, and acid solution, alkali solution and enhanced sewage solution can be selected according to the requirement.
Wherein, at least one type of salt solution is 3% NaCl solution according to the mass percentage concentration; at least one kind of acidic solution should be H with mass percent concentration of 2% 2 SO 4 A solution; at least one type of alkaline solution should be 0.1% NaOH+saturated Ca (OH) 2 Is a basic solution of (a) and (b).
As a further improvement of the technology, the reinforced sewage solution in the step (4) is an organic sewage solution, the urban sewage in a local sewage treatment system is used, and meanwhile, a certain amount of organic substances are added for culture, and the COD value is not lower than 1000mg/L.
As a further improvement of the technology, the electrochemical corrosion test is adjusted according to the actual test requirement, and the test at least comprises a group of test environments with the temperature of 23+/-5 ℃, and other temperatures can be selected for further evaluating the material performance.
As a further improvement of the technology, experimental parameter selection is optionally adjusted, wherein the open circuit potential test time is not less than 10min, the suggested range of alternating current impedance frequency is 100 kHz-10 mHz, the amplitude is 10mV, the suggested initial voltage of the electrokinetic potential/Tafil is-1V, the termination voltage is 2V, and the scanning rate is 0.01V/S.
The on-site sampling and electrochemical corrosion test method for the concrete surface anti-corrosion material can more accurately obtain the change condition of the corrosion resistance of the organic inert coating under the actual service condition, is beneficial to the model selection and development of the concrete anti-corrosion material under a sewage pool and similar working conditions, and can be used for laboratory early-stage research and on-site detection and evaluation. Compared with the traditional three-electrode electrochemical experiment method, the method can better reflect the performance of the corrosion-resistant material in the actual service environment, and the experimental result has better accuracy.
Drawings
FIG. 1 is a Tafel plot of electrochemical test results for polyurea coatings in accordance with embodiments of the present invention;
FIG. 2 is a Tafel plot of electrochemical test results for a solvent-free epoxy coating in an embodiment of the present invention;
Detailed Description
The following detailed description of specific embodiments of the invention is provided in further detail.
The invention provides a field sampling and electrochemical corrosion test method of a surface anti-corrosion coating for concrete, which can be used for laboratory and field sampling to evaluate the change condition of the corrosion resistance of an organic inert anti-corrosion coating in an actual service environment, and compared with the traditional electrochemical test method, the obtained test result has better accuracy.
The invention relates to a method for on-site sampling and electrochemical experiment of a concrete surface anti-corrosion material (mainly suitable for organic inert coating), which mainly comprises the following steps:
1. the method for cutting the anticorrosive paint sample on site comprises the following steps: selecting a position of the side wall or the pool wall, which is a certain height away from the water surface, for cutting the sample, wherein the samples cut at the same height position are taken as a group;
2. sampling point selection rules: the point positions are selected to have smooth surfaces and no obvious pore positions;
3. and (3) subsequent treatment of the anti-corrosion material and preparation of a test electrode: 1) Removing the concrete attached to the back surface of the paint by using an angle grinder; 2) Polishing the coating into a thin sheet with a certain thickness, adhering the thin sheet to a metal backboard, and sealing edges to prepare a test electrode;
4. electrochemical experimental environment and parameter selection: the more accurate result is obtained by adopting the sewage in the actual service environment or preparing the test solution similar to the sewage in composition.
The following are specific examples.
The method is used for sampling the anticorrosive paint for the urban sewage pool concrete on site, and the side wall of the biological reaction pool of a certain local sewage treatment plant is selected as a sampling position by combining early-stage on-site investigation, the position is subjected to surface anticorrosive treatment by using the epoxy paint, and the position has water level change and illumination effect. An epoxy paint coated on the same type of concrete surface was used as a control group.
The concrete test block coated with the anti-corrosion paint, which is used for acid resistance test in a laboratory, is selected for sampling, the test block is 100X 100mm, the surface is coated with a polyurea anticorrosive coating at 5%H 2 SO 4 Soaking in the solution for 120 days, and taking out. Test blocks immersed in water for 120 days in the same environment were selected as control groups.
And during sampling, selecting a side wall waterline change area, selecting the same horizontal plane height group point taking at the middle position of the waterline change area, and taking 3 points from the same horizontal plane for testing. The coating at the sampling position has relatively poor adhesive force effect, and can be directly scraped by a tool. When sampling, certain pulverization and light loss phenomena appear on the surface of the coating, but the surface of the coating is kept approximately intact, and the phenomena of leakage, breakage, falling and the like are avoided.
When sampling, a triangular crack is drawn along the edge of the coating by using an art designer knife, then the coating is embedded between the coating and the concrete substrate by using a strip knife, the whole coating is pried off, the taken sample is sealed by using a sealing bag, and the sample is brought back to a laboratory for later use.
For the coating with better adhesion, a triangular pyramid concrete test block with the coating is cut by using a handheld cutting machine at an inclined angle of 60 degrees, and a film can be adhered to the surface of a sample during cutting, so that the film is prevented from being brittle, and the surface is watered and cooled during cutting, so that the performance change of the coating caused by high temperature is avoided.
Before testing the sample, the sample is regulated for at least 24 hours at the temperature of 23+/-5 ℃ and the RH of 50+/-10%, so that the sample is ensured to be in a normal temperature state, and the influence on an experiment result is avoided. And (3) polishing the coated slice, so as to ensure that concrete particles are not adhered to the back surface of the coated slice, and polishing while maintaining water spraying, so that the coating is not influenced by heat generated in the polishing operation process. Meanwhile, the polished coating slice should be not less than 500 μm and have uniform thickness.
To ensure as uniform a thickness of the coating as possible, a hand-held angle grinder may be used for the sanding operation. Cutting the polished coating into slices with the thickness of 10 multiplied by 10mm, adhering the slices to the surface of a stainless steel metal backboard by using conductive adhesive, sealing edges by using epoxy paint, and adjusting the sample to be in a room temperature state after sample preparation is completed.
Preparing 3% NaCl solution as the solution for the electrochemical test, or selecting H with mass percent concentration of 2% according to the requirement of the test 2 SO 4 Solution, 0.1% NaOH+saturated Ca (OH) 2 The solution, the COD value should be not lower than 1000mg/L of the intensified sewage solution, is used as an experimental environment.
The coating slice is adhered with a metal backboard to serve as a working electrode, a saturated calomel electrode/saturated KCl is used as a reference electrode, and a platinum electrode is used as an auxiliary electrode to construct a three-electrode system.
The electrochemical experiment comprises an open circuit potential test (OPC), an alternating current impedance test (EIS) and a dynamic potential Test (TAF), wherein the open circuit potential test time is not less than 10min, the alternating current impedance frequency proposal range is 100 kHz-10 mHz, the amplitude is 10mV, the dynamic potential/Tafil proposal initial voltage is-1V, the termination voltage is 2V, and the scanning rate is 0.01V/S.
Compared with the solvent-free epoxy coating after corrosion soaking, the potential polarization curve moves to the right and upward, the corrosion current density JCorr is increased by one order of magnitude, which indicates that the polymer crosslinking structure is destroyed after corrosion, and the corrosion resistance is reduced. Compared with a polyurea coating, the change amplitude of the potential polarization curve is smaller, and meanwhile, the polyurea coating has the minimum corrosion current density JCorr and has relatively good corrosion resistance.
Claims (13)
1. The on-site sampling and electrochemical corrosion test method for the concrete surface anticorrosive material is characterized by comprising the following steps of:
(1) Selecting sampling points, wherein the requirements are as follows:
a. taking the side wall and the top of a sewage pool with serious corrosion in actual service as a sampling position to be tested, wherein the sampling position at least comprises a group of side wall surfaces or the top of the sewage pool;
b. selecting the surface coated with the organic inert coating as a sampling part, wherein the selected surface is in an attached state, and the surface is basically flat and has no obvious holes or cracks;
c. the selected sampling point is coated with an anticorrosive coating with the thickness of at least 500 mu m;
(2) Cutting the surface coating by using a cutting tool, and ensuring the integrity of the surface structure of the coating sample during sampling; the cutting area of the single sheet is not smaller than 10mm multiplied by 10mm;
(3) Polishing the back of the cut surface coating, removing the concrete structure attached to the back of the coating, and only leaving a complete coating slice; coating slices are stuck to a metal backboard to prepare a tested electrode sample;
(4) Preparing a test solution as a test environment for performing subsequent electrochemical tests:
(5) Electrochemical corrosion tests are carried out on samples in different test solutions by using an electrochemical test platform, and the electrochemical corrosion tests at least comprise an open circuit potential test (OPC), an alternating current impedance test (EIS), a potentiodynamic Test (TAF) and potentiodynamic cyclic polarization.
2. The method for in-situ sampling and electrochemical corrosion testing of a concrete surface corrosion resistant material according to claim 1, wherein the test solution comprises at least one set of salt solutions; alternatively, a set of salt solutions is included, and additionally a set of acid solutions, a set of base solutions, and/or a set of enhanced wastewater solutions is included.
3. The method for on-site sampling and electrochemical corrosion testing of a concrete surface corrosion preventing material according to claim 1, wherein when an electrochemical test platform is used for testing, a metal back plate adhered with a coating slice is used as a working electrode, a saturated calomel electrode/saturated KCl is used as a reference electrode, and a platinum electrode is used as an auxiliary electrode for building a three-electrode system.
4. The method for on-site sampling and electrochemical corrosion testing of a concrete surface corrosion inhibitor according to claim 1, wherein when the sampling site is a wall surface of a side wall of a sewage pool, the sampling site is selected to be sampled and measured in groups by points at different heights from a waterline.
5. The method for on-site sampling and electrochemical corrosion testing of a concrete surface corrosion protection material according to claim 1, wherein when the surface coating is cut, a conventional cutter is used for cutting the profile on the surface of the sampling coating for the point with relatively low adhesive force, and the sample is scraped for sampling; for the point with relatively strong adhesion, a hand-held cutter is used for sampling.
6. The method for in-situ sampling and electrochemical corrosion testing of a concrete surface corrosion protection material according to claim 1, wherein the organic inert coating is an epoxy organic inert coating or a polyurea organic inert coating.
7. The method for on-site sampling and electrochemical corrosion testing of a concrete surface corrosion protection material according to claim 1, wherein,
the on-site sampling in the step (1) is carried out, and when sampling is carried out in the same sewage pool, the method at least comprises a group of side wall surfaces or tops of the sewage pools, and the sampling area of a single sewage pool is not less than 3 parts; and selecting at least 3 groups of longitudinally distributed water line change areas and at least one group of longitudinally distributed water line change areas when sampling the side wall.
8. The method for in-situ sampling and electrochemical corrosion testing of a concrete surface corrosion protection material according to claim 1, wherein when preparing the electrode sample to be tested, a conductive adhesive is used to adhere the coated sheet to a stainless steel metal sheet of the same size and an inert material is used to seal the edges as a working electrode in a three-electrode system.
9. The method for on-site sampling and electrochemical corrosion testing of a concrete surface corrosion protection material according to claim 2, wherein the salt solution is 3% nacl solution according to mass percent concentration; the acid solution is 2% H 2 SO 4 A solution; the alkali solution is 0.1% NaOH+saturated Ca (OH) 2 An alkaline solution.
10. The method for on-site sampling and electrochemical corrosion testing of a concrete surface corrosion preventing material according to claim 2, wherein the enhanced wastewater solution is an organic wastewater solution selected from municipal wastewater in a local wastewater treatment system, and a certain amount of organic substances are added for cultivation, and the COD value is not lower than 1000mg/L.
11. The method for in-situ sampling and electrochemical corrosion testing of a concrete surface corrosion resistant material according to claim 1, wherein the back of the cut surface coating is polished by a wet grinding polishing process.
12. The method for in-situ sampling and electrochemical corrosion testing of a concrete surface corrosion inhibiting material according to claim 1, wherein the electrochemical corrosion test of step (5) comprises at least one set of corrosion tests in an experimental environment at 23±5 ℃.
13. The method for in-situ sampling and electrochemical corrosion testing of a concrete surface corrosion inhibitor according to claim 1, wherein in the electrochemical corrosion test of step (5), the experimental parameters are as follows: the open circuit potential test time is not less than 10min, the alternating current impedance frequency range is 100 kHz-10 mHz, the amplitude is 10mV, the initial voltage of the electrokinetic potential/Tafil is-1V, the termination voltage is 2V, and the scanning speed is 0.01V/S.
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